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Publication number | US6632390 B1 |
Publication type | Grant |
Application number | US 09/560,455 |
Publication date | Oct 14, 2003 |
Filing date | Apr 28, 2000 |
Priority date | Jun 15, 1999 |
Fee status | Lapsed |
Also published as | US6808805, US20030228479, WO2000077096A1 |
Publication number | 09560455, 560455, US 6632390 B1, US 6632390B1, US-B1-6632390, US6632390 B1, US6632390B1 |
Inventors | Marcus David Shelby, Julian Harold Scott Jensen, Daniel Christopher Cobb, Marc Alan Strand |
Original Assignee | Eastman Chemical Company |
Export Citation | BiBTeX, EndNote, RefMan |
Patent Citations (33), Referenced by (20), Classifications (11), Legal Events (7) | |
External Links: USPTO, USPTO Assignment, Espacenet | |
This application claims the benefit of U.S. Provisional Application Serial No. 60/139,285 filed Jun. 15, 1999 titled "Polyester Compositions for Profile Extrusion".
This invention relates to profile extrusion of thermoplastic polymers to form shaped articles commonly referred to as profiles. More particularly, this invention relates to processes of profile extrusion utilizing certain polyester compositions.
Thermoplastic polymers are commonly used to manufacture various shaped articles which may be utilized in applications such as automotive parts, food containers, signs, packaging materials and the like. Profile extrusion is a common, cost-effective method for producing these shaped articles. Polymers such as polyvinyl chloride (PVC), acrylics and polycarbonates are typically used in profile extrusion. Each of these polymers suffers from one or more disadvantages. PVC is undesirable from an environmental standpoint since PVC produces toxic gases during melt extrusion and is difficult to dispose of after use. Acrylic articles are brittle and shatter when dropped or struck against another object. Polycarbonate is difficult to work with from a processor's perspective and is too expensive for many applications. Polyesters, being notoriously difficult to process compared to many other polymers, have not been utilized as often in profile extrusion. As compared to polymers typically used in profile extrusion, polyesters have lower melt strengths and insufficient shear thinning resulting in a greater propensity for melt fracture if extruded at high output rates or low temperatures. Both melt strength and shear thinning are extremely important from the standpoint of profile extrusion.
Profiles are defined herein by a combination of two factors: shape and process of manufacture. The shape of a profile has a particular two-dimensional cross-section and an infinite length. The process of manufacture is known as profile extrusion. The cross-section lies in the x-y plane and the length lies along the z-axis. The x-y plane usually corresponds to the face of the die, whereas the z-axis corresponds to the extrusion or "take-off" direction. Profiles can take on a wide variety of cross-sections varying in size, shape and complexity. Common "simple" profile shapes include hollow tubes, solid round stock, square cross-section stock, etc. More complex shapes such as those used for pricing channels, corner guards, and house siding can also be made.
By this use of shape as part of the profile definition, fiber, film and sheet might also be considered as special classes of profiles. Fibers have very small circular cross-sections and are extruded continuously in one direction. Film and sheet have rectangular cross-sections and are extruded continuously. However, in the industry as a whole and as defined herein by the additional definition factor of process of manufacture, film, sheet and fiber are not profiles because of how they are manufactured. Film or sheet, while infinite in length, are manufactured by processes that include the use of calendering or chill rolls. Fiber processes involve very high drawdowns, along with spinning cabinets and godet rolls. Profiles, in the industrial vernacular, represent constant cross-section, axially extruded structures, which have axial rigidity and are not wound. Profiles are usually cut to length and bundled, stacked or otherwise bound for transport. This axial rigidity obviously has important implications for what kind of "haul-off" equipment is used to convey the extruded product. Furthermore, the issues of melt strength and melt fracture are not important factors in fiber, film and sheet due to the nature of the take-up/winding equipment and the fact that shape definition is already trivial. Thus, as defined in the industry and herein, "profile" shall not include fiber, film and sheet.
Profiles are fabricated by melt extrusion processes that begin by extruding a thermoplastic melt through an orifice of a die forming an extrudate capable of maintaining a desired shape. The extrudate is typically drawn into its final dimensions (along the z-axis) while maintaining the desired shape (in the x-y plane) and then quenched in air or a water bath to set the shape, thereby producing a profile. In the formation of simple profiles, the extrudate preferably maintains shape without any structural assistance. With extremely complex shapes, support means are often used to assist in shape retention. In either case, the type of thermoplastic resins utilized and its melt strength during formation is critical. Melt strength is defined as the ability of a polymer to support its weight in the molten state. For example, when extruded vertically from a die, a polymer with low melt strength will quickly sag and hit the floor; whereas, a polymer with high melt strength will maintain its shape for a much longer amount of time.
There are a number of quantitative and qualitative means for measuring melt strength. One standard test is disclosed in U.S. Pat. No. 4,398,022 wherein melt strengths for a polyester used in extrusion blow molding processes were measured at values between −10 and 10 percent. This same test is utilized herein and involves vertically extruding the polymer from a 0.1 inch (0.25 cm) diameter capillary die that is 0.25 inches (0.64 cm) long at a shear rate of 20 s−1 up to a total length of 19 inches (49 cm). At this point the strand is cut near the die face and allowed to cool at room temperature. The diameter 6 inches (15 cm) from the end of the extrudate is then measured and expressed as a percentage change relative to the capillary diameter to give the melt strength. For example, if the strand diameter at a point 6 inches (15 cm) from the bottom was 0.12 inches (30 cm), then the polymer melt strength at that given melt temperature would be 20 percent (i.e. MS=(0.12−0.1)/0.1*100 percent). Similarly, the "die swell" is obtained by measuring the diameter � inches (1.3 cm) from the bottom of the extrudate and expressing it as a percentage change relative to the capillary diameter.
Polyesters due to their poor melt strength may have a negative value for the melt strength since the 6 inches (15 cm) point diameter could be less than the nominal diameter. For example, linear poly(ethylene terephthalate) modified with 1,4-cyclohexanedimethanol (PETG) having an inherent viscosity (IV) of 0.76 dl/g has been observed to have a melt strength of −4 percent at 200� C. and −24 percent at 220� C. This means that the diameter of the extrudate measured 6 inches (15 cm) from the end of the strand was 4 percent smaller (200� C. sample) than the die opening. Typical melt strengths for PVC under standard processing conditions (160 to 200� C. processing temperature) are in the order of 20 to 30 percent. To achieve this melt strength with linear PETG would require an IV of around 0.95 dl/g. Thus, for applications in which melt strength is critical, polyesters will often not supplant these competitive polymers.
Another common melt strength test involves measuring the time period that an extrudate takes to reach a predetermined length below a die for a given flowrate/shear rate. While not standardized, this test provides an easy method for material comparison on a typical processing line and is used in some of the examples cited herein. Other non-standard melt strength tests such as measuring the degree of drooping in a horizontal profile extrusion line can also be applied giving a more application specific measure of melt strength.
Profile extrusions are usually run horizontally, and thus melt strength is important to minimize the amount of "drawdown" and gravity-induced sagging the polymer experiences upon exiting the die. Drawdown is defined in profile extrusion as the amount of thickness reduction between the die and the take-up system and is expressed as the nominal thickness or width dimension at the die divided by the same dimension in the final part). For example, a typical polyester drawdown is about two. This means that the width of the final part is � that of the width at the die exit. Similarly, the final thickness is � of the thickness at the die exit. The take-up force of the puller or winder causes drawdown as the melt exits the die. A higher melt strength reduces the amount of drawdown, since there is greater resistance to stretching and thinning. For example, the drawdown for higher melt strength PVC is more on the order of 1.25. Reduced drawdowns make designing the appropriate dies and maintaining critical final part dimensions much easier.
The inadequate melt strength of polyesters further results in severe processing problems when polyesters are processed at typical profile extrusion temperatures of 390-550� F. (200-290� C.) and line speeds. Processing line speeds vary considerably depending on the shape of the profile. Typical speeds for simple shapes like a corner guard may be from 50 to 70 feet (15 to 20 meters) per minute. More complicated shapes may have process line speeds as low as one foot (0.3 meters) per minute, whereas extremely simple shapes with certain types of processing technology may run at speeds as high as 100 feet (30 meters) per minute. At the higher speeds, which obviously would be preferred by profile manufacturers, inadequate melt strength produces an extrudate that does not maintain its shape prior to quenching, and thus deformation occurs. To increase the melt strength of the polyester, processing temperatures are often lowered. This, however, increases the likelihood of an undesirable phenomenon known as melt fracture, which can only be eliminated by lowering the extrusion speed. By decreasing speed, the economic attractiveness of using polyesters is also decreased. Thus, the profile extrusion processes are often operated at maximum speeds associated with the highest temperatures and minimal melt strengths for maintaining particular profile shapes. Any increase in speed or lowering of temperature may cause an increase in high shear viscosity in the die, which then may cause an undesirable melt fracture.
From a Theological standpoint, melt strength depends primarily on the viscosity and, to some degree, on the elasticity or relaxation time of the melt. A higher viscosity increases the resistance to drawdown/sagging. In contrast, melt elasticity causes an increase in die swell, which serves to offset some of the effects of drawdown. Even though the same amount of width/thickness reduction is occurring after the die, the highly elastic material starts with a much higher initial width/thickness due to the greater die swell. Thus, the final part dimensions remain closer to the die dimension and the effective drawdown seems lower (thereby making it easier to design the tooling needed).
A viscosity curve for a given polymer has two regions of interest, as shown in FIG. 1. At very low shear rates the viscosity is highest and this is referred to as the "zero shear viscosity", η0. The zero shear viscosity (along with the elasticity) defines the melt strength since the polymer is experiencing essentially a zero shear rate after exiting from the die. Thus, the higher the zero shear viscosity, the higher the melt strength. In the high shear rate region, the polymer is "processed" with shear rates in the die/extruder ranging anywhere from about 10 s−1 to 1000 s−1. As low of a viscosity as possible in this range is desired in order to minimize pumping pressure and melt fracture. Fortunately, most polymers exhibit at least some degree of viscosity reduction or "shear thinning" at higher shear rates, which aids in their "processability". Without the shear thinning, an extruder running a high melt viscosity polymer would require extremely high motor loads and/or very high melt temperatures, both of which can lead to polymer degradation and excessive energy consumption. In general, condensation polymers like polycarbonates and polyesters have a very low degree of shear thinning relative to addition type polymers like PVC and polyolefins. This is because the condensation polymers typically have narrower molecular weight distributions in addition to lacking the high molecular weight "tail" common in many addition polymers. This narrow molecular weight distribution makes polyesters more "Newtonian-like" (i.e. having a flat viscosity which does not depend much on shear rate) and characteristically harder to process.
Having a low viscosity at high shear rates (i.e. in the die) also serves to minimize the formation of melt fracture or "sharkskin" on the surface of the extruded part or article. Melt fracture is a flow instability phenomenon occurring during extrusion of thermoplastic polymers at the fabrication surface/polymer melt boundary. The occurrence of melt fracture produces severe surface irregularities in the extrudate as it emerges from the orifice. The naked eye detects this surface roughness in the melt-fractured sample as a frosty appearance or matte finish as opposed to an extrudate without melt fracture that appears clear.
Melt fracture occurs whenever the wall shear stress in the die exceeds a certain value (typically 0.1 to 0.2 MPa). In turn, shear stress is controlled by the volume throughput or line speed (which dictates the shear rate) and the viscosity of the polymer melt. By reducing either the line speed or the viscosity at high shear rates, the wall shear stress is reduced and the chance for melt fracture is lowered. Thus, by increasing the degree of shear thinning, the viscosity is reduced at high shear rates, which then allows higher line speeds before melt fracture occurs.
Coupling all of these desired properties together, the ideal polymer for profile extrusion clearly will have a high zero shear viscosity in conjunction with a high degree of shear thinning. This maximizes melt strength while at the same time minimizes melt fracture and die pressures. A representative "ideal" curve is illustrated in FIG. 1.
With respect to polyesters, either melt strength may be increased or melt fracture reduced without significantly affecting a change in the other. For example, by increasing the molecular weight or inherent viscosity of the polyester or by lowering the melt temperature, the zero shear viscosity will increase significantly along with the melt strength, but the degree of shear thinning will only change slightly. Thus, the melt strength will increase, but melt fracture will become even more of a problem since the high shear rate viscosity also increased significantly. This is in fact a problem for profile extrusions with polyesters and copolyesters. For example, in order to achieve an acceptable level of melt strength (i.e. greater than approximately 0 percent melt strength), PETG must be extruded at a melt temperature of 200� C. or lower. This is an extremely low processing temperature for a polymer normally designed to be run at 220� C. or higher. When run at this low temperature, PETG exhibits severe melt fracture even at low line speeds because the high shear rate viscosity is so high. This is due to the lack of significant shear thinning in PETG. Thus, with polyesters the process must be operated at either (1) hotter melt temperatures resulting in no melt fracture but too low melt strength or (2) low temperatures resulting in adequate melt strength but problems with melt fracture. Either scenario represents an economically unacceptable alternative for profile extrusion, so an improved processing polyester is needed that has both good melt strength and a high degree of shear thinning (i.e. melt fracture resistance).
Nevertheless, for some applications (e.g. flat film casting, extrusion blow molding, and foam extrusion) where the effective shear rates/stresses are already fairly low due to bigger die gaps and/or reduced extrusion rates, melt fracture may not be an issue. Thus, increasing just the melt strength alone may be acceptable. However, for profile extrusion, which typically has very high shear rates, both increased melt strength and resistance to melt fracture are important factors and should be improved simultaneously.
Chain branching is one of the most commonly used methods for improving the melt strength of a polymer, particularly polyesters. A tri-, tetra-, or higher functionality monomer is added to the polyester either during manufacture or in the processing step to create branches in the polymer. Typical branching agents for polyesters include trimellitic anhydride (TMA), pyromellitic dianhydride (PMDA), glycerol, sorbitol, hexane triol-1, 2, 6, pentaerythritol, trimethylolethane, and trimesic acid. Common applications for high melt strength polyesters include extrusion blow molding and foams.
U.S. Pat. No. 4,983,711 to Sublett describes high melt strength polyesters for extrusion blow molding applications. The polyester is poly(ethylene terephthalate) modified with 1,4-cyclohexanedimethanol (PETG) having from 0.05 to 1 mole percent of a tri-functional brancher, preferably trimellitic acid or anhydride. The 1,4-cyclohexanedimethanol (CHDM) levels are from 25 to 75 mole percent.
U.S. Pat. Nos. 5,523,382 and 5,442,036 to Beavers describe branched copolyesters suitable for extrusion blow molding. The branching agent is preferably trimellitic acid or anhydride. The copolyester contains an ethylene glycol component modified with 0.5 to 10 mole percent of CHDM and 3 to 10 mole percent of diethylene glycol. The acid component is terephthalic acid with up to 40 percent of isophthalic acid and naphthalenedicarboxylic acid.
U.S. Pat. No. 5,376,735 to Sublett describes high melt strength poly(ethylene terephthalate) (PET) for use in extrusion blow molding applications. The PET was blended with up to 3 mole percent isophthalic acid (IPA). A number of branching agents are mentioned including TMA.
Fukuda et. al. in U.S. Pat. No. 5,382,652 (reissued as RE35939) discloses a polyester resin branched with a range of tri- and tetra-functional materials including TMA and others. The resin composition is from 90 to 100 percent ethylene glycol and from 0 to 10 percent of one or more of the following: diethylene glycol, CHDM, propylene glycol, and butanediol. The application described is for improved processability around film extrusion, molding, and heat-sealability.
In U.S. Pat. No. 5,235,027, Thiele discloses a modified PET for extrusion blow molding. The PET contains from 0.5 to 5 wt. percent of isophthalic acid, 0.7 to 2.0 wt. percent of diethylene glycol, 300-2500 ppm tri- or tetra-hydroxyalkane, 80-150 ppm antimony, phosphorous of at least 25 percent by weight of the amount of antimony, red and blue toner (not exceeding 5 ppm), and various branching agents with pentaerythritol preferred. The resultant polyester has an IV between 0.8 and 1.5 dl/g.
Hauenstein in U.S. Pat. No. 4,182,841 describes a modified PET containing 12 mole percent neopentyl glycol terephthalate and 0.0062 mole percent of a polyfunctional modifying branching agent, including TMA.
Edelman et al, in U.S. Pat. Nos. 4,234,708, 4,219,527 and 4,161,579 disclose various high melt strength polyesters for extrusion blow molding. A variety of chain branching agents are utilized in amounts of from 0.025 to 1.5 mole percent with 0.25 to 10 equivalents of a chain terminator, which controls reaction conditions and prevents gelling. The importance of high zero shear viscosity coupled with shear sensitivity is also described.
Thus, there exists a need in art to have a polyester composition for use in profile extrusion which has both high melt strength to prevent sagging and excessive drawdown and a high degree of shear thinning to resist melt fracture at high processing speeds. Accordingly, it is to the provision of such that the present invention is primarily directed.
A process for producing a profile by profile extrusion comprises providing a melt of a polyester composition, which has a branching agent therein and an inherent viscosity of at least 0.65 dl/g, at a melt temperature and extruding the melt through a die to form a profile. The diacid component of the polyester composition comprises 100 to 98.0 mole percent of residues of a primary acid selected from the group consisting of terephthalic acid, naphthalenedicarboxylic acid, isophthalic acid and mixtures thereof. The glycol component of the polyester composition comprises 100 to 98.0 mole percent of residues of a primary glycol selected from the group consisting of ethylene glycol, 1,4-cyclohexanedimethanol, diethylene glycol, neopentyl glycol, and mixtures thereof. The polyester composition comprises from 0.05 to 2.0 mole percent of residues of the branching agent selected from an acidic branching agent with a tri-functional or greater monomer, an alcoholic branching agent with a tri-functional or greater monomer, and mixtures thereof. The branching agent is present as part of either the diacid component or glycol component depending on whether the functionality is acidic or alcoholic, respectively.
FIG. 1 is a typical viscosity versus shear rate curve for a standard polyester and an "ideal" resin having improved processability.
FIG. 2 is a photograph of actual profiles in their sagged state at constant throughput for PETG resins having different inherent viscosities and the same branching level.
FIG. 3 is a viscosity curve for branched PETG at 230� C. and 240� C. and neat PETG at 230� C.
FIG. 4. is a viscosity curve at 270� C. for copolyesters modified with either 24 mole percent or 35 mole percent isophthalic acid and containing no or 0.15 percent branching agent.
Polyester compositions as alternative materials for use in making profiles have heretofore been difficult to incorporate into profile extrusion processes. As discussed above, to obtain the requisite melt strength, polyesters are typically processed at lower temperatures and thus lower speeds to prevent melt fracture caused by the lack of shear thinning. The ideal polyester would thus have a high melt strength and a high degree of shear thinning so that the polyester could be run at the high speeds associated with profile extrusion without sagging and melt fracture.
The present invention addresses the problems of the prior art by providing a process for producing a profile by profile extrusion wherein a melt of a polyester composition, which has been modified by the addition of a tri-functional or greater branching agent, is extruded through a die to form a profile. Unexpectedly, this polyester provides both characteristics of high melt strength and a high degree of shear thinning making it suitable for use in profile extrusion processes. The branching agent imparts higher melt strength and a higher degree of shear thinning (i.e. resistance to melt fracture) to the polyester resulting in easier startup in the profile line, higher line speeds and better control of the final profile dimensions.
The polyester compositions of the present invention have an inherent viscosity (IV) of at least 0.65 dl/g, preferably at least 0.7 dl/g, providing the high melt strength necessary for profile extrusion. The polyester composition is based on 100 mole percent of a diacid component and 100 mole percent of a glycol component. A branching agent is present either as a portion of the mole percentage of the diacid component or the glycol component depending, respectively, on whether the branching agent has acid functionality or alcohol functionality as described below.
The polyester composition comprises a diacid component of from 100 to 98.0 mole percent, preferably 99.9 to 99.0 mole percent, of residues of a primary acid selected from terephthalic acid (TPA), isophthalic acid (IPA), naphthalenedicarboxylic acid (NDA) or mixtures thereof. Preferably, TPA is the predominant primary acid (at least 60 mole percent) with up to 40 mole percent of IPA therein. A more preferred embodiment has TPA as the sole primary acid.
The primary acid of the diacid component may optionally be modified by replacing one or more of TPA, IPA and NDA with up to 40 mole percent of one or more different diacids, such as saturated aliphatic dicarboxylic acids having 4 to 12 carbon atoms and cycloaliphatic dicarboxylic acids having 8 to 12 carbon atoms. Specific examples of diacids are: phthalic acid, cyclohexanedicarboxylic acid, cyclohexanediacetic acid, diphenyl-4,4′-dicarboxylic acid, succinic acid, glutaric acid, adipic acid, azelaic acid, sebacic acid, and the like. It should be understood that use of the corresponding acid anhydrides, esters, and acid chlorides of these acids is included in the term "diacid".
The polyester composition comprises a glycol component of from 100 to 98.0 mole percent, preferably 99.9 to 99.0 mole percent, of residues of a primary glycol selected from ethylene glycol (EG), 1,4-cyclohexanedimethanol (CHDM), diethylene glycol (DEG), neopentyl glycol (NPG), or mixtures thereof. A preferred level of EG and CHDM is from 0 to 100 mole percent, whereas a preferred level of NPG is from 0 to 40 mole percent. A small amount of DEG is usually also present as a side reaction in the manufacturing process, although it can be increased to higher levels if desired. A typical range for DEG is from 0 to 10 mole percent, with a preferable range from 0 to 3 mole percent. The most preferred embodiments have 57 to 90 mole percent EG with 10 to 40 mole percent of either CHDM or NPG and/or 0 to 3 mole percent of DEG.
In addition, the primary glycol of the glycol component can be modified with up to 40 mole percent of one or more different diols. Such additional diols include cycloaliphatic diols having 6 to 15 carbon atoms and aliphatic diols having 3 to 8 carbon atoms. Examples of such diols are: triethylene glycol, propane-1,3-diol, butane-1,4-diol, pentane-1,5-diol, hexane-1,6-diol, 3-methylpentanediol-(2,4), 2-methylpentanediol-(1,4), 2,2,4-trimethylpentane-diol-(1,3), 2-ethylhexanediol-(1,3), 2,2-diethylpropane-diol-(1,3), hexanediol-(1,3), 1,4-di-(hydroxyethoxy)-benzene, 2,2-bis-(4-hydroxycyclohexyl)-propane, 2,4-dihydroxy-1,1,3,3-tetramethyl-cyclobutane, 2,2-bis-(3-hydroxyethoxyphenyl)-propane, 2,2-bis-(4-hydroxypropoxyphenyl)-propane, and the like.
The polyester composition further comprises from 0.05 to 2.0 mole percent, preferably 0.1 to 1.0 mole percent, of residues of a branching agent selected from an acidic branching agent comprising a tri-functional or greater monomer, an alcoholic branching agent comprising a tri-functional or greater monomer, or mixtures thereof. The acidic branching agent refers to branching agents containing acid moieties that react within the polyester chain. The alcoholic branching agent refers to branching agents containing alcohol moieties that react within the polyester chain. The branching agents comprising a tri-functional or greater monomer have at least three functional groups that can react to create branches in the polyester chain. Preferred branching agents include trimellitic anhydride (TMA), pyromellitic dianhydride (PMDA), glycerol, sorbitol, hexane triol-1,2,6, pentaerythritol, trimethylolethane, and trimesic acid. When the acidic branching agent is used in the present invention, the mole percentage is part of the acid component. When the alcoholic branching agent is used, the mole percentage is part of the glycol component.
In a preferred embodiment of this invention, TMA is present from 0.1 to 2 mole percent, based on 100 mole percent of the diacid component. Because of the difficulties in processing the higher levels of branching due to high reactor viscosities, in addition to the problem of gel formation, the most preferred level of TMA is from 0.1 to 0.35 mole percent. Below 0.1 percent TMA, the degree of processability improvement does not warrant the added cost of introducing the branching agent; whereas, above about 0.3 mole percent the reaction rate in a production facility becomes more difficult to control unless chain terminators are added. Chain terminators suitable for use in the present invention are monfunctional with an acid or alcohol functionality. Examples include stearic acid and benzoic acid. If the branching agent is tri-functional, the chain terminator and branching agent are preferably present at a ratio of 3:1 and more preferably at a ratio of 1:1. If the branching agent is tetra-functional, the chain terminator and branching agent are preferably present at a ratio of 4:1 and more preferably at a ratio of 2:1.
The melt strength of the polyester composition used in the profile extrusion process is preferably greater than about 0 percent at a particular melt temperature utilized in the process. Typical processing temperatures of the polyesters of the present invention are about 220 to 230� C. A "standard" profile should be processed without too much difficulty at about 0 percent melt strength. More complicated shapes might require a melt strength greater than about 20 percent, whereas simpler parts could be run adequately at melt strengths below 20 percent. As mentioned previously, melt strength is a strong function of the melt temperature, IV and, as described in this invention, the degree of branching agent. The melt strength as used herein is determined by using the test described in U.S. Pat. No. 4,398,022.
The polyester compositions utilized in the process of the present invention are further characterized by their high degree of shear thinning, i.e. having a low high shear rate viscosity, resulting in a profile that does not suffer from the phenomenon known as melt fracture. The "power law index, n" can be used to quantify the shear thinning. With reference to FIGS. 1 and 3, the slope of the viscosity versus shear rate curve in the high shear rate region, on a log-log plot, is equal to "n−1". If n is equal to 1 as in a purely Newtonian case, then the slope is equal to 0 and there is no shear thinning. As n gets smaller and smaller, the slope, or degree of shear thinning gets greater and greater with n=0 being the ultimate limit. To determine the power law indices, the slope is measured for a given curve over the region from about ω=100 to ω=400 wherein ω is the effective shear rate or rheometer test frequency, which is approximately equivalent to the shear rate. In FIG. 3, neat PETG (IV of 0.76 dl/g) at 230� C. has a value of n equal to 0.64. Typical values for linear polyesters range from 0.6 to 0.7 depending on IV and error in the measurement. PETG with 0.15 mole percent TMA (IV of 0.76 dl/g) at 230� C. and 240� C., embodiments of the present invention, have values of n=0.56 and n=0.57, respectively. Thus, in a preferred embodiment, the polyesters used in the process of the present invention have a power law index less than 0.6, more preferably less than 0.575, and even more preferably less than 0.5. As a comparison, other typical polymers used in profile extrusion have even lower values of n. The exact value depends on the type of polymer and how the polymer is made. For example, low density polyethylene, linear low density polyethylene, and metallocene are all polyethylenes that vary in n due to differences in branching and molecular weight distribution. Similarly, all of the so-called "easy to process" resins such as PVC and polystyrene have low values as well, typically less than 0.5.
The occurrence of melt fracture in a profile, as previously discussed, is typically a visual determination. Cloudy appearance is an indication of melt fracture, and a smooth clear appearance is an indication of no melt fracture. To quantify this lack of melt fracture in the resulting profile of the present invention, a surface roughness measurement is utilized. Surface roughness measurements are made using a Dektak3 profilometer over a scan length of 0.39 inches (10 mm) along the axial direction of the profile. For comparison with the visual determination, the RMS surface roughness measurement of a profile made using linear PETG having visible melt fracture is approximately 17000 Angstroms. The surface roughness took the form of periodically spaced bumps on the surface having a "wavelength" of approximately 1000 microns. This periodicity is typical of melt fracture due to the stick-slip behavior. The surface roughness for a profile made using the polyester of the present invention having a smooth appearance, i.e. no melt fracture, is approximately 400 to 500 Angstroms. The actual surface roughness of a "smooth" profile will vary depending on the roughness of the die tooling, cooling rate, etc. even if no melt fracture is present. Thus, profiles produced according to the present invention preferably have a surface roughness measurement of 5000 Angstroms (RMS) or less. More preferably, the surface roughness is 1000 Angstroms or less and even more preferably is 500 Angstroms or less.
The polyesters can be made via direct esterification of the acid and glycol, or through ester exchange of the glycol with the corresponding dimethyl ester (e.g. dimethyl terephthalate (DMT) in place of TPA or dimethyl isophthalate (DMA) in place of IPA). When using TMA as the branching agent and EG as one of the glycol components, the TMA is preferably pre-reacted with ethylene glycol before adding to the reactor. This reduces the amount of residual TMA left in the final product and minimizes the amount of TMA related extractables.
The branching agent may be added in the form of a concentrate or masterbatch that could be dry blended with the neat polyester just before entering the extruder. Nevertheless, the level of branching agent would have to be much higher (>0.5 mole percent) with the exact level depending on the masterbatch letdown ratio. Because of the higher level of branching agent in the concentrate, reaction conditions would have to be carefully controlled. However, this approach may not achieve the same broad MW distribution (thus reducing its effectiveness) compared to a condensation reactor grade product.
Inherent Viscosity (IV) as used herein is measured at 25� C. in a solvent mixture consisting of 60 percent by weight phenol and 40 percent by weight tetrachloroethane.
This invention can be further illustrated by the following examples of preferred embodiments thereof, although it will be understood that these examples are included merely for purposes of illustration and are not intended to limit the scope of the invention unless otherwise specifically indicated.
There are a number of quantitative and qualitative means for measuring melt strength. The standard test used for this invention is that disclosed in U.S. Pat. No. 4,398,022 and set forth herein above. Another common melt strength test involves measuring the time for the extrudate to. reach a predetermined length at a given flowrate/shear rate. While not standardized, this test provides an easy method for material comparison on typical processing lines and is used in some of the examples. Other non-standard melt strength tests such as measuring the degree of drooping in a horizontal profile extrusion line can also be applied giving a more application specific measure of melt strength.
Melt fracture is more difficult to measure quantitatively and no standardized test has been developed. This is because a moderately melt-fractured part typically has a hazy, rough surface, which is immediately noticeable to the naked eye. Thus, visible melt fracture makes a profile extrusion unacceptable, particularly for polyesters, where it is usually desired that the profile be clear. Nevertheless, optical transmission and surface roughness measures, as already mentioned, can be applied effectively although visual observation is still the most common method.
Film Extrusion Comparison of PETG and 0.3 Mole Percent TMA Modified PETG
An unbranched PETG with 31 mole percent modification of CHDM and IV of 0.76 dl/g (Control 1) and a branched PETG with 31 mole percent modification CHDM, 0.30 mole percent TMA and an IV of 0.715 (Example 1) were extruded on a 1″ (2.54 cm) Killion extruder (24:1 UD, Maddock mixing section screw) using a 6″ (15.2 cm) film die, a 12 (0.3 mm) mil gap and a 60 RPM screw speed. Extrusion temperatures were the same for both polymers (feed zone temperature=21� C., all other zones at 230� C.). At a time denoted as "time zero", the die was scraped, and the polymer then allowed to flow until such a point that it contacted the floor (approximately a 4 foot (1.2 m) height). This time was denoted as the "sag time".
For the Control 1, the sag time was 20+/−2 seconds, whereas for Example 1, the sag time was 31+/−1 seconds. Thus the melt strength of Example 1 was about 50 percent higher than the Control 1 by this measure. The die pressures for the Control 1 and Example 1 were 1480 psi (10 MPa) and 1400 psi (9.6 MPa), respectively. Similarly the screw loads were 14 and 8.9 amps, respectively. The die pressures and screw loads are indicative of the shear thinning and ease of extrusion. Clearly, the TMA increases the melt strength while reducing the energy and pressure required to pump the material (a lower pressure indicates a lower probability for melt fracture since it relates to the wall shear stress).
Profile Extrusion Trials with PETG Samples
Different combinations of TMA vs. polyester resin IV samples were processed on a profile extrusion line and tested for melt strength. Since there was no known method for quantifying melt strength online, a method was devised (referred to herein as the "Sag Test") using a die and calibration tooling setup designed to make flat, thin (at die exit) profile shapes. The dimensions of the extrudate at the die exit was 3 inches (7.6 cm) by 0.080 inches (0.2 cm). Running at 30 ft/min (9.1 m/min) line speed, PETG with 31 mole percent modification of CHDM (Control 2) was extruded at conditions (temperature and screw speed, etc.) which were on the verge of melt fracture so as to establish a point (aesthetically) at which to set conditions for the test. After allowing the profile line to run for an hour in order to reach equilibrium conditions, the calibration tooling was gradually distanced from the die. This was done until 1) the face of the calibration tooling was exactly 20 inches (50.8 cm) from the face of the die or 2) the extrudate "sagged" to the point of not being able to run thus causing a system shutdown.
During this "Sag Test", the Control 2 extrudate often sagged to the floor causing system shutdown and thus failed the Sag Test. The polyester compositions of the present invention did not fall to the floor, but rather continued to run allowing for measurement of the amount of sag, and thus passed the Sag Test. A video camera was fixed 3 feet (92 cm) from the sagging extrudate for each sample. Pictures similar to that shown in FIG. 2 were taken. The point where the extrudate exits the die is 43.5 inches (110.5 cm) from the floor (referred to herein as the "Zero Sag" point). This is also the same height where the extrudate enters the water tank. Once each sample (while sagging) reached a state where maximum sag had been reached, the number of inches from the floor to the bottom of the sagging extrudate was recorded. This measurement was then subtracted from the Zero Sag point to give a Sag Value for each sample. Lower Sag Values indicate higher melt strength materials.
FIG. 2 is an image showing superimposition of actual extrudates in their sagging state. The samples in FIG. 2 were made using the composition of Control 2 and containing 0.15 mole percent TMA as the branching agent. Sample A (IV of 0.80 dl/g) had a Sag Value of 2.47 inches (6.27cm) a melt temperature of 229� C. Sample B (IV of 0.76 dl/g) had a Sag Value of 3.34 inches (8.48cm) at a melt temperature of 226� C. Sample C (IV of 0.74 dl/g) had a Sag Value of 5.91 inches (15.01cm) at a melt temperature of 224� C.
Table 1 below contains Sag Value data for other samples of polyester compositions with varying amounts of TMA and values of IV.
Sample: % TMA
and IV
Sag Value (in)
Sag Value (cm)
Melt Temp (� C.)
Rheological Data for Branched and Unbranched PETG Having a 0.76 IV
The melt strength test utilized in Example 2 was developed specifically for profile extrusion. The degree of drooping in a horizontal profile extrusion line between the die and the water bath for a given distance of separation is measured.
Samples of PETG having an IV of 0.76 dl/g were prepared both with and without TMA branching agent. The PETG has a 31 mole percent modification of CHDM. The viscosity curves for the branched PETG (0.15 mole percent TMA) at 230� C. and 240� C. and for the unbranched PETG at 230� C. are shown in FIG. 3. If the ratio of the viscosity at 1 rad/s over the viscosity at 400 rad/s is used as a "processability index", the unbranched resin has a processability index of 2.9 whereas the branched resin has an index of 7 measured at the same temperature. Thus, the branched resin will be much easier to process and have better melt strength than the unbranched resin. Additionally, by increasing the temperature of the branched resin by 10� C., both melt strength and shear thinning properties of the resin were enhanced.
Melt Strength Data for Branched and Unbranched PETG Having a 0.76 IV
Using the same samples as in Example 3, melt strength measurements were performed at a temperature of 220� C. using a capillary rheometer and the standard protocol outlined earlier. The unbranched PETG had a melt strength of −26 percent at 220� C., whereas the 0.15 mole percent TMA branched PETG had a melt strength of 4 percent. Clearly the branched PETG is much better suited for profile extrusions at this temperature because its melt strength is greater than 0 percent. The linear PETG would have to be run much colder to achieve the same melt strength, thereby increasing the likelihood of melt fracture.
Branched and Unbranched Copolyesters Containing Neopentyl Glycol
Samples of a copolyester of containing a glycol component of 37 mole percent of neopentyl glycol (NPG) and 63 mole percent of ethylene glycol and a diacid component of terephthalic acid were produced both with and without branching agent to an IV of 0.70 dl/g. Branching levels were 0, 0.15 or 0.30 mole percent of TMA. The measurements for viscosity were at 230� C. The zero shear viscosity was measured at a shear rate of 1 rad/s and the high shear viscosity was measured at a shear rate of 400 rad/s. As clearly indicated by the data in Table 2 below, the use of branching agents significantly improves the processability of NPG based copolyesters.
Sample %
zero shear
high shear
ability index
law index
Branched and Unbranched Copolyesters Containing Isophthalic Acid
Samples of a copolyester containing 100 mole percent CHDM as the glycol component and a diacid component of either 24 or 35 mole percent of isophthalic acid (IPA) and correspondingly 76 or 65 mole percent of terephthalic acid, respectively, were produced both with and without branching agent. The viscosity curves of the four samples are depicted in FIG. 4. As observed in FIG. 4, the degree of shear thinning is much greater in the branched samples making them more processable. The power law index for the four samples are set forth in Table 3. While these examples of branched IPA modified resins have a power law index of greater than 0.6, which is a preferred embodiment of the present invention, the data indicates that branch does improve processability of the resins making them more suitable for use in profiles. The data indicates that a higher level of branching agent would be required to lower the power law index.
Sample Description
Thus, the present invention provides polyester compositions that are suitable for use in making profiles by profile extrusion. These polyesters have higher melt strengths and higher shear thinning than linear polyesters making them extremely suitable for profile extrusion processes.
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Citing Patent | Filing date | Publication date | Applicant | Title |
US6808805 * | Jun 11, 2003 | Oct 26, 2004 | Eastman Chemical Company | Process for profile extrusion of a polyester |
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US7235623 | Nov 26, 2003 | Jun 26, 2007 | Eastman Chemical Company | Polyester compositions for calendering |
US7285587 | Nov 12, 2003 | Oct 23, 2007 | Eastman Chemical Company | Flame retardant polyester compositions for calendering |
US7354653 | Dec 6, 2004 | Apr 8, 2008 | Eastman Chemical Company | High clarity films with improved thermal properties |
US8071695 | Nov 10, 2005 | Dec 6, 2011 | Eastman Chemical Company | Polyeste blends with improved stress whitening for film and sheet applications |
US8604138 | Oct 21, 2008 | Dec 10, 2013 | Eastman Chemical Company | Extrusion blow molded articles |
US8604139 | Oct 21, 2008 | Dec 10, 2013 | Eastman Chemical Company | Extrusion profile articles |
US8980389 | Oct 21, 2008 | Mar 17, 2015 | Eastman Chemical Company | Copolyesters and blends with improved recyclability, processes for their manufacture, and articles prepared therefrom |
US20030060546 * | Feb 28, 2002 | Mar 27, 2003 | Moskala Eric Jon | Films prepared from plasticized polyesters |
US20030228479 * | Jun 11, 2003 | Dec 11, 2003 | Shelby Marcus David | Process for profile extrusion of a polyester |
US20040096874 * | Jul 10, 2003 | May 20, 2004 | Third Wave Technologies, Inc. | Characterization of CYP 2D6 genotypes |
US20040127609 * | Nov 12, 2003 | Jul 1, 2004 | Strand Marc Alan | Flame retardant polyester compositions for calendering |
US20050113556 * | Nov 26, 2003 | May 26, 2005 | Strand Marc A. | Polyester compositions for calendering |
US20050136271 * | Dec 6, 2004 | Jun 23, 2005 | Germroth Ted C. | High clarity films with improved thermal properties |
US20060111519 * | Nov 10, 2005 | May 25, 2006 | Strand Marc A | Polyester blends with improved stress whitening for film and sheet applications |
US20090181196 * | Oct 21, 2008 | Jul 16, 2009 | Eastman Chemical Company | Copolyesters and blends with improved recyclability, processes for their manufacture, and articles prepared therefrom |
US20090181201 * | Oct 21, 2008 | Jul 16, 2009 | Eastman Chemical Company | Extrusion blow molded articles |
US20090181202 * | Oct 21, 2008 | Jul 16, 2009 | Eastman Chemical Company | Extrusion profile articles |
US20120260436 * | Dec 3, 2010 | Oct 18, 2012 | Kuraray Co., Ltd. | Normal pressure dyeable polyester fiber and method for producing the same |
U.S. Classification | 264/176.1, 528/308.6, 528/272 |
International Classification | C08G63/20, C08L67/00 |
Cooperative Classification | Y10T428/31786, Y10T428/8305, C08L67/00, C08G63/20, Y10T428/2978 |
European Classification | C08L67/00 |
Date | Code | Event | Description |
Mar 2, 2004 | CC | Certificate of correction | |
Mar 27, 2007 | FPAY | Fee payment | Year of fee payment: 4 |
May 2, 2007 | REMI | Maintenance fee reminder mailed | |
Mar 23, 2011 | FPAY | Fee payment | Year of fee payment: 8 |
May 22, 2015 | REMI | Maintenance fee reminder mailed | |
Oct 14, 2015 | LAPS | Lapse for failure to pay maintenance fees | |
Dec 1, 2015 | FP | Expired due to failure to pay maintenance fee | Effective date: 20151014 |


text:
More in Theatre
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Concordia College – As Concordia's theater program kicks off November with the popular musical "Les Misérables," cooperation between the theater and music departments becomes the key to putting on the […]
Musical to be Story's Concordia Theatre directing debut
Among her numerous accolades as a runner, scuba diver, and certified barbecue judge, Professor Sally Story is also the director for Concordia's upcoming musical, "Les Misérables." Story, Concordia theatre department's […]
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Concordia 2012 alumnus Christopher Damlo has been named assistant director of the Tin Roof Theatre's upcoming production of Abby Man's "The Judgment at Nuremberg." The play is based upon the […]
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Seniors to experience last main stage performance with Concordia Theatre It is the Elizabethan era and the governor Leonata throws a masked ball. Noblemen, soldiers and friends of Lenoata mingle, […]
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Director explores new training methods for actors in upcoming play Marching in single line across the stage with knees bent and arms held out, nine students stay straight-faced and focused […]
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Theatre art professor Jen Thomas insists she did not come here planning to revitalize the theatre department; she has simply tried to do her part. Nonetheless, Thomas has made a […]
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/ Events, Music, Theatre, Variety
Using plungers to fight for their right to pee for free, the lower class of "Urinetown" raises important social questions in Concordia's upcoming musical production. "Urinetown," which opens Nov. 14 […]
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Improv has arrived at Concordia. Students of all majors can now join an on-campus, student-led improv group. Junior theatre major Anna Larranaga, founder of the group, led their first meeting […]
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This week a classic English play is taking the stage at Concordia. Oscar Wilde's "The Importance of Being Earnest" follows Englishmen Jack Worthing and Algernon Moncrieff, both of who lead […]

subset: commoncrawl


text:
Sounds like an interesting read! Hope your launch is very successful, Laura! :-)
Hello Mike, hi Laura, I wish you success in your book. Sounds interesting and I enjoyed the interview too.
Yay, Laura! I've joined her party, too. Good luck with your launch!!
Participating in the release blitz as well.
Yay for a great book blast! I have two YA books with Etopia and love all the new YA books coming out.
Laura is just amazing! I'm thrilled that today has finally arrived for her. Yay!
I really do love black panthers. And pretty girls. I might just have to pick this one up. ^_^
Congratulations Laura, sounds like a book I'd absolutely be into, going to add this one to my list right now. (:
Intrigued! And adding Laura's book to my TBR. :)
cool cover
EEEEP! Always so wild to see myself on video, LOL!Thanks for hosting me, Michael!Thanks, everyone, for being so supportive. Gotta say, Etopia Press knocked it out of the park with the cover! :)I hope you guys and gals enjoy reading it!
I love shapeshifters so this is cool news. Congrats on the release, Laura, and good luck!Jai
I just saw you over on Ciara Knight's blog, Laura, and of course I've signed up for a free copy here on Michael's. Good luck with your newest story!
So many great books, like this one. So little time.
Ditto what Stephen said. (Seriously, those were the very words I had in my head to comment with.)
grats, laura :)
You've been tagged.
Good on you for getting the word out, Michael. We writer folk need all the help we can get.
Sounds like an interesting story! :)


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08-11-2002 | |
Chip From Showcrash
 DRESS CHAIR A chair with the character of a chameleon, DRESS CHAIR can change to suit different environments. It is supplied in a silver or grey cover and you can easily customise it with your own fabric. DESIGN: Rane Vaskivuori, Timo Vierros, 1999. MATERIALS: 100% nylon upholstery, steel frame with lacquered white aluminium colour. COLOURS: Silver or anthracite upholstery. DIMENSIONS: 750w x 820h x 630d mm.  Cloud by Snowcrash http://www.designboom.com/snapshots/...snowcrash.html |
23-11-2002 | |
front row
OOPS, I mean the glow blo inflatable lamp.I also love the glow ball inflatable lamp.That is a Jasper Morrison design.
Trean, you should check out www.moooi.com Its a design house started by Marcel Wanders.He gained fame for his knot chair. He seems to have a limitless supply of crestive energy. He also has produced work for flos,cappelini & Droog design. Its always refreshing to see your design oriented postings. Im going to Houston nect week and they have a great design store called Sunset Settings.The women that owns it buys with her heart & always has very cool,Interesting adaptations in the way she presents each item and buys in very bizzare colorations. I always buy a slew of things when Im there. |
26-12-2002 | |
Astrid, if you like Rashid you should really check out Marc Newson's work (http://www.marcnewson.com ) they probably wouldn't appreciate the comparison but they often use similar shapes in their work: the curvilinear lines, organic shapes juxtaposed with use of synthetic materials. IMHO, Rashid is a better packaging designer than he is a furniture designer. He did some great packaging systems for Shiseido perfume and I believe his studio worked on the Prada cosmetics packaging. I must admit that some his lamps are cute, but his silly DJ table just gives me the jeebies.
Droog design is great, they do wonderfully clever stuff. I have one of their milk bottle lamps... makes me smile every time I look at it. One of my favorite pieces of furniture is the Eames walnut stool, or the Time Life stool. I love how sculptural it is and the wood grain is so damn pretty. I have the one labelled C (in the picture below) at home. That last picture you posted (of the Rashid chair) also looks like it was very much inspired by one of the classics that the Eames(es) did way back in the 50s. I'm posting a pic because the chair also happens to be one of my favorites. |


text:
A Tennessee woman became a bit of a news item recently when firefighters allowed her home to burn because she hadn't paid a subscription fee. Fees for emergency services are part of a growing national trend.
Family home burns because firefighter subscription fee was not paid
Part of the reason people pay taxes is that services need to be provided such as police, firefighters and so on. Unfortunately, taxes don't always cover all of the bills, and extra fees are required. During the past few years, a growing number of municipal governments have been imposing emergency service fees on residents. The type of fee depends on the city or county that imposes it.
For instance, according to the Daily Mail, the city of South Fulton, Tenn., charges a $75 annual fee for residents of nearby rural areas who want access to the services of the South Fulton Fire Department. The fee became the subject of national news when Vicky Bell's trailer went up in flames and firefighters stood by and did nothing because Bell hadn't paid up.
Other cities considering similar fees
Another rural South Fulton resident, Gene Cranick, had forgotten about the fee but told firefighters he'd pay on the spot when his house caught fire. They refused; he and his wife lost their home and pets in the blaze.
Other cities are considering or have enacted fire service subscription fees. The city of Lyndon, Ky., according to NBC affiliate WAVE3, recently began charging a tiered fee for every fire response ranging from $300 to $500. The upper range of the fee includes structure fires or hazardous waste disposal, though the charge is typically billed to insurance companies.
According to WFTV, an ABC affiliate in Orlando, Fla., the city of Lake Mary, Fla., started considering such a fee recently in the face of declining tax revenues. The city of College Station, Texas, is currently considering a fire response fee for traffic accidents, where the at-fault driver is billed for firefighters having to go to the scene, according to the Bryant-College Station Eagle.
It's a fee for all
Fees exist for almost every emergency service; even being able to call 911 can cost people. AT&T, according to the Tennessean, has been charging businesses in Tennessee $1.50 to $3 per phone line, per month for allowing them to call for help in an emergency. Various counties in Tennessee have been suing AT&T because they feel the company hasn't collected enough.
According to MSN, there are also "crash response fees" or "crash taxes," which means any non-resident of a municipality that's been involved in an accident gets charged for emergency service personnel showing up at the scene, needed or not. As of 2008, such fees existed in 24 states.
Daily Mail: http://www.dailymail.co.uk/news/article-2070834/Firefighters-watch-couples-home-burn-ground-hadnt-paid-75-subscription-fee.html
WAVE3: http://www.wave3.com/story/16025563/lyndon-fire-department-stepping-up-efforts-to-collect-of-fees-for-fire-runs-and-some-accident-runs
WFTV: http://www.wftv.com/news/news/local/lake-mary-considers-new-fire-protection-fee/nFrb7/
The Eagle: http://www.theeagle.com/local/CSFD-studies-rescue-fees–6784125
The Tennessean: http://www.tennessean.com/article/20111125/NEWS01/311250058/AT-T-settles-Davidson-County-over-911-phone-fees?odyssey=tab|topnews|text|FRONTPAGE
MSN: http://articles.moneycentral.msn.com/Insurance/InsureYourCar/crash-taxes-add-hefty-fees-for-aid.aspx?page=1
Do you have a fantastic idea related to this article, but just don't have the money you need to start your own company or side-business? Get the loans you need from https://personalmoneynetwork.com to help get your new company underway, from the small loan professionals at PersonalMoneyNetwork.


text:
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Utimaco attains Microsoft Gold Certified Partner Status
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Microsoft certifies Utimaco's security expertise
New status allows access to exclusive research resources
Partnership underlines strong relationship with ...
2006-06-14 08:03:15
Microsoft certifies Utimaco's security expertise
New status allows access to exclusive research resources
Partnership underlines strong relationship with Microsoft
Oberursel (Germany) and London (UK), June 14 2006, Utimaco - The Data Security Company, has earned Gold Certified Partner status in the Microsoft Partner Programme, indicating the highest degree of competence in working with Microsoft technologies. The status specifically recognises Utimaco's achievements as a security solutions provider and also for its Independent Software Vendor (ISV) solutions. This partner status is the result of Utimaco's success in working with Microsoft and delivering Microsoft compatible security solutions to enterprise customers. The award is another milestone in a series of initiatives Utimaco has undertaken with Microsoft.
The data security specialist gained the highest level within the Microsoft Certified Partners Programme by achieving the highest level of developer certification and providing numerous completed customer reference projects. The Gold Certified Partner status sends an important message to potential customers that Utimaco's products display excellence in operational functionality on Microsoft operating systems and that they can trust Utimaco's Microsoft Certified System Engineers.
The Gold Certified Partner Status is another milestone in the close relationship Utimaco shares with Microsoft for over 15 years. In February 2006, Utimaco became a founding member with Microsoft in the SecureIT Alliance, allowing Utimaco to access latest product and developer details on an exclusive level. An ongoing information flow is also guaranteed by Utimaco's "Microsoft Primary Support Contract". This contract incorporates a Microsoft staff member solely attending the needs of Utimaco developers, offering them close technical support.
In co-operation with Microsoft, Utimaco has already provided innovative security solutions, such as developing a certificate-based access to Microsoft Windows-based PCs using national electronic identity cards. With the implementation of Utimaco's SafeGuard software products to secure the Windows Mobile devices in use by the staff at the Microsoft subsidiary in Germany, Microsoft has recognised Utimaco for its reliable data security technology.
"Particularly in IT-security, customers need vendors they can trust who can assume the role as an advisor for their long-term strategic technology plans," said Allison Watson, vice president of the Worldwide Partner Sales and Marketing Group at Microsoft Corp. "We recognise Utimaco as a new Gold Certified Partner for demonstrating its expertise in providing security solutions on Microsoft products and technology."
Paul Yao, Utimaco's business alliance manager to Microsoft in Redmond, adds: "Microsoft's business is built on establishing partner relationships; but it reserves the Gold Certified Partner status for those companies which have fulfilled the promise of establishing the unique synergies which are necessary to help both companies do what they do best, and at the same time to help each other to be successful. Reaching Microsoft Gold Certified Partner status was a logical next step in the close relationship between Utimaco and Microsoft. Utimaco is committed to continuing to provide data security solutions that support and extend Microsoft's technologies in a way that provide our mutual customers with both cost efficient and secure environments."
About Utimaco Safeware AG
Utimaco is a world leading producer of professional solutions that secure data within companies and government agencies. The solutions, which have won multiple awards, protect data against unauthorized access and manipulation across a wide range of devices, including mobile PDAs, notebook computers, client PCs, server systems, or across networks. SafeGuard Easy, with nearly three million installations, is the best selling worldwide solution for protecting data on notebooks and PCs. Utimaco is also a leader in electronic transaction protections. In Germany, for example, Utimaco solutions secure over 90 percent of all card-based payment systems. Utimaco offers its customers comprehensive on site support via a worldwide network of partners and subsidiaries in Europe, the USA and Japan. Utimaco Safeware AG, with headquarters in Oberursel, near Frankfurt, Germany, is listed on the Frankfurt Stock Exchange (ISIN DE0007572406). For more information, visit our website at
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Decimal Degrees: Latitude: 36.7528009 Longitude: -103.4438372
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2016-17 Merrimack College Football News
March 21, 2017Football Hosts 2017 Pro Day Tuesday Current and former members of the football team performed in front of pro scouts Tuesday on campus
March 07, 2017Football Devotes Time to Participate in Bradford Elementary School Literacy Night Members of the football team were on hand for a special community service initiative last week
February 21, 2017Cortes Torres' Sports Excellence Award Highlights Six NE10 Fall Academic All-Conference Honorees Men's soccer senior adds additional academic accolade to resume; Merrimack has six academic all-league picks
February 02, 2017Merrimack Continues Head Coach Contract Extensions Dennehy (men's ice hockey), Morgan (men's lacrosse), Curran (football) receive multi-year contract extensions
January 13, 2017Hill Accepts Invite to 2017 Tropical Bowl, Named to Don Hansen Gazette Super Region Third Team Senior defensive lineman will join other top FBS DI players in special all-star game showcase
December 03, 2016Football Volunteers at Lazarus House on Thanksgiving Members of the football team spent part of their Thanksgiving giving back to local community
November 17, 2016Football Participates in Lawrence Literacy Night Warriors logged community service hours at local elementary school recently
November 16, 2016Hill Headlines Football's Four All-Conference Picks Senior defensive lineman earns all-conference first team recognition after leading league in sacks
November 15, 2016Merrimack College Boasts 89-Percent Graduation Clip in Latest NCAA Academic Success Rate (ASR) Report Athletic Department boasts fifth-highest ASR in Northeast-10 Conference for 2015-16 report
November 12, 2016Football Concludes 2016 on High Note, Triumphs over Pace, 28-18, on NE-10 Championship Weekend Warriors top Setters in final game of the fall
November 11, 2016Football Hosts Pace on NE-10 Championship Weekend Warriors welcome Setters in final game of 2016
November 05, 2016Football Honors Class of 2017 on Senior Day; #10 LIU Post Triumphs, 64-7, in Regular Season Finale Members of the Football Class of 2017 pose with Coach Curran after the game
November 04, 2016Football to Salute Seniors after Saturday Afternoon Clash with 10th-Ranked LIU Post Warriors welcome unbeaten Pioneers to campus in regular season finale Saturday
October 29, 2016Saint Anselm Trips up Football, 28-17 Redshirt sophomore Shamik Perry scored on an 85-yard rush on Saturday
October 28, 2016Football Heads to Saint Anselm for Final Road Game of Regular Season Saturday Afternoon Warriors look to bounce back against Hawks Saturday in Manchester
October 22, 2016Southern Connecticut State Spoils Football's Homecoming Afternoon Matchup Senior Matt Clifford returned an 85-yard kickoff return to the house in Saturday's game
October 19, 2016Football Hosts SCSU on Homecoming Saturday Warriors aim for second straight win in front of Homecoming crowd Saturday at home
October 15, 2016Offense Erupts in Football's 35-21 Victory at Pace Sophomore Brenton Martin (pictured) tossed for two touchdowns and rushed for another on Saturday
October 14, 2016Football Travels to Pace for Noon Saturday Kickoff Warriors look to get back on track with Saturday conference clash in Pleasantville
October 08, 2016New Haven Downs Football, 45-14 The 2006 NE-10 champion team was honored at halftime on Saturday
October 06, 2016Football Celebrates 10-Year Anniversary of NE-10 Championship Team Saturday vs. New Haven Merrimack welcomes New Haven to campus, will celebrate 2006 NE-10 champs at halftime
October 01, 2016Football Falls at Stonehill, 31-6, Saturday Senior Josh Hill (pictured) had two sacks against the Skyhawks Saturday
September 29, 2016Football Aims to Bounce Back, Opens October Slate at Stonehill Saturday in Easton Warriors looking to snap four-game skid against Skyhawks Saturday in Easton
September 24, 2016#17 Assumption Pulls Away in Second Half; Football Falls, 55-23, Saturday Senior corner back Matt Clifford had two interceptions on Saturday
September 23, 2016Football Welcomes #17 Assumption to Campus Saturday in NE-10 Clash (1 p.m.) Warriors face first ranked opponent in four years, look to upset Greyhounds at home
September 23, 2016Athletic Department to Honor 2006 NE-10 Champion Football Team Oct. 8 vs. New Haven Join fellow football alumni from the 2006 season in honoring the first NE-10 champions in school history!
September 16, 2016Football Falls at Bentley, 41-22, Friday Night Junior running back Derrick Villard rushed for a career-high 104 yards on Friday night
September 15, 2016Football Faces Bentley in Waltham Friday Night Warriors aiming for 2-0 start in conference play with Friday night bout against Falcons
September 12, 2016Hill Named NE-10 Defensive Player of the Week Senior defensive lineman posted three sacks and seven tackles in Saturday's win
September 10, 2016Football Roars Back to Defeat AIC in Home, NE-10 Opener, 16-13, Saturday Night Senior defensive lineman Josh Hill recorded three sacks in Saturday's victory
September 09, 2016Football Hosts AIC in 2016 Home Opener Saturday Warriors open conference play against Yellow Jackets tomorrow night (6 p.m.)
September 03, 2016Football Topped by Bryant, 41-20, in Season Opener Junior Devin O'Reilly hauled in a 40-yard touchdown catch on Saturday
September 01, 2016Football Starts 2016 in Smithfield, Visits Former NE-10 Mate Bryant on Saturday (3 p.m.) Warriors kick off the season against Bulldogs for second time in three years
August 28, 2016FROM THE E-T: Safety Brian Carroll Looks to Build on Big Sophomore Season The Eagle-Tribune featured captain Brian Carroll and previews the upcoming football season!
August 26, 20162016 Football Season Preview The football team's 2016 campaign begins in eight days at Bryant!
August 19, 2016Football Slotted Fourth in NE-10 Coaches' Poll Merrimack slotted fourth in the 10-team field
August 12, 2016Football Kicks Off 2016 with Preseason Camp The start of the 2016-17 athletic year begins today!
August 10, 2016Football 2016 Single-Game Tickets NOW ON SALE! Purchase your single-game tickets for the 2016 season today!
June 06, 2016Football Volunteers at Special Olympic Summer Games Student-athletes and members of the coaching staff were on hand to volunteer over the weekend


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Categories > Celebrities > My Chemical Romance
Two weeks in hell for seven minutes in heaven.
2 reviewsWaycest. Gerard and Mikey are stuck on holiday in the middle of nowhere with only each other for company, for two weeks. *Rated R for future chapters.. which will also probably be NC-17*
Two weeks in hell for seven minutes in heaven
9 reviewsWaycest. Gerard and Mikey are stuck on holiday in the middle of nowhere with only each other for company, for two weeks. *Rated R for future chapters.. which will also probably be NC-17*
5OriginalGet me out of my 'fucked up' mind
5 reviews5ExcitingToo weak-minded to sleep.
7 reviews"Uhh.. Mmmhhh.." he moaned again. I bit my lip, enduring the noises like torture.
5ExcitingIt'll be funner just the two of us anyway...
7 reviews"Y'know Mikes, if you really don't want to go on this walk, we can go on our own walk..." Gerard purred, his words poured out like smooth cream from his mouth.
5ExcitingCan't even take a little seduction?
5 reviews"Oh Mikey stop acting so angry like that," he interruped, sliding his hand back into mine and grasping it. Our bodies were close, only precious inches from touching. "It's so fucking cute."
5HotI wish you'd finish your god damn sentence.
7 reviewsNo! Not this time! Last time I'd let my nerves get the better of me I had passed out.
5ExcitingDoe eye'd demon
9 reviews"If you're really that scared..." he began, finishing his sentence by holding out his open palm.
5HotJust a little Brotherly love...
Each second we became more passionate, aching for each other's touch.
?BlockedJust because society says so, it doesn't mean it's true
5 reviews"What're you smiling about?" he asked me, noticing the huge grin that had developed accross my face. I couldn't control it any more, but it was okay because I didn't want to.
5MovingHe didn't even bring the coffee...
5 reviews"It's okay, just start slowly, don't worry before you know it we'll be at the camp and ready to..." "Wait, WHAT!?" Gerard blurted out, his eyes widening in horror, "D-did you just say camp?"
5ExcitingThe light cast from the crescent moon
11 reviewsGerard's lips tore from mine like velcro from felt, desperately wanting to hold on.


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Sometimes I think I have a problem. It's a good thing that where I work has the solutions.
Did you know that if you put a DT Swiss singlespeed freehub body onto a regular mountain shell after lopping off 15mm off of the drive side of the axle you get a 120mm ss hub and a dishless build? Yeah, my cross bike is going to be pretty sweet here shortly. Not any faster, but definitely sweeter. The only thing more awesomer was that I actually had the required spokes in my drawer 'o' shit.
Monday, March 30, 2009
240, 120, whatever it takes
2 comments:
- rfresh said...
i have no idea what any of that is, does or means. sounds awesome though :)
- Beerorkid said...
I love my DT's
had the TMCO guys etch them up - 5:30 PM
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text: Pet Photographer Says Better Photos Save Shelter Dogs' LivesMargaret Hartmann9/19/11 10:20amFiled to: PetsPet photographyShelter dogAnimalsDogs192EditPromoteShare to KinjaToggle Conversation toolsGo to permalinkTeresa Berg of Dallas, Texas is a professional pet photographer who specializes in glamour shots for shelter dogs. She believes that thousands of dogs are euthanized every year simply because the photos posted on adoption sites show them in a cage, looking like they're thinking about biting your three-year-old. Several years ago, she started volunteering to retake dogs' photos for a dachshund rescue group, and now she encourages other professional photographers to donate their services and teaches shelter employees to take more appealing pet photos.Reply192 repliesLeave a reply


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OK. Let's try this again. Let's play a game where you post something related to the Stern Show universe in alphabetical order. The first poster uses "A" and the next "B" and so on...When the alphabet is complete, you may start again with "A". I'll start: A. Amaaaaazing Arm Warmers
Hey thanks, Peach! I had fun thinking up answers. We had that thing passed 50 pages...too bad Mike had to shut down!


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Project photo archive Sept. 22, 2012 Pre-lift photos All is quiet on the existing bridge. Project leaders closed down Hwy 61 as a safety precaution while the new Main Span was being lifted into place. Spectators watched throughout the day as crews worked nonstop to lift the bridge into place. Looking eastward, crews are working hard to get the span aligned with the skid system so it can get moved into place. A closer look at the skid system that will be used to move the span between the piers. One of the strand jacks up close. There were four used to lift the bridge. Each jack has 54 strands, which are made of high-strength steel and are about 18 millimeters in diameter. The strand jack sits at the top of Pier 5, waiting to connect with the Main Span. Looking down at the Main Span before it is lifted into place. In the background is Jaycee Park where many spectators gathered throughout the move and lift.
Sept. 22, 2012 Main Span move Looking at the Main Span after it had been floated down the river from where it had been moored for a few days. Crews have the Main Span on the skid system and move it into place. It takes patience to move a 545-foot Main Span. A member of the lifting team works to help move the Main Span eastward between Piers 5 and 6. Another look at the skid system used to move the Main Span in place. MnDOT Project Manager Steve Korodosky (left) keeps a close eye on the entire process. Other members from the MnDOT team watch and assist with the move. As nightfall approaches, crews are getting closer to actually lifting the bridge. Work continues after dusk. The Main Span is connected to the strand system and can now be lifted. The project site is lit up as crews continue work into the night. Great precision is needed when moving such a large and heavy structure. By the morning of September 24, the new Main Span is in place next to the existing bridge. Traffic is reopened at noon – ahead of schedule. Looking southward at the new Main Span next to the existing bridge. The North Approach lanes were poured before the Main Span was lifted into place. A look at the new Main Span with the existing bridge sitting behind it. The new span will allow for the same wide navigation channel needed for river traffic.
Sept. 7, 2012 - Main Span move Early on Friday, September 7, the Main Span starts to make its way down to the river. The Main Span is 104 feet wide. The Main Span sits upon the Self Propelled Motorized Transports that are used to inch it down to barges in the river. Taking a look under the Main Span as it moves towards the shoreline. Crews started moving the Main Span early on a Friday, September 7. By early afternoon, the Main Span is making its way down a platform connecting the staging area and the barges in the river. Butch Ames of Ames Construction looks on as crews move the Main Span. Carefully measuring movement is important in a large move such as this. By afternoon, the Main Span is getting close to the barges in the river. Looking upstream as the Main Span moves onto the barges. By evening, the Main Span is fully on the barges. In between the flotilla of barges, there's an open area. Work continues to secure the bridge on the barges. Work continues to secure the bridge on the barges. One of the boats that will be used to move the Main Span sits in the foreground. Looking downstream from Lock and Dam No. 2. The tugboat Gracie M sits ready to help move the Main Span.
Project photo archive August 2012 Another perspective of the Main Span in the staging area. The existing bridge can be seen on the far left. A view of the deck of the southbound lanes for the new South Approach The 545 feet that the new Main Span will fit between. A view of where the Main Span will connect to the South Approach. A look at the Main Span down to the staging area where it was under construction to where it will connect to the South Approach. The Main Span sits upon the Self Propelled Motorized Transporters (SPMTs) that were used to move it from land to barges. A closer look at the SPMTs and what's below the Main Span as it moves. Before crews start to take apart the falsework – or temporary supports – for the Main Span The moon glows high in the sky next to one of the arch ribs Another view of the area where the Main Span will sit, with the existing bridge in the background A view from underneath the deck. The pre-cast concrete girders supporting the deck were put in place earlier in the year and are the longest of their kind in Minnesota. Looking up at one of the arch ribs A view from underneath the deck. The pre-cast concrete girders supporting the deck were put in place earlier in the year and are the longest of their kind in Minnesota. An inspection crew takes a closer look at the deck work Crews gathering sections of the lifting system that will be used to move the Main Span the 50 feet up into place. The railings next to the roadway match the color of the arches. A side view of the North Approach from nearby Jaycee Park Crews do finishing work on the deck of the new North Approach Crews doing preliminary work for what will eventually be the divider between the roadway and the 12-foot-wide bike and pedestrian path A member of the construction crew takes a closer look at the work Crews do finishing working on the deck. A view of the new bridge next to the old bridge. Welding a piece of falsework A look underneath the deck. This falsework, or temporary supports, was in place until crews successfully tensioned the approach. Looking down at the Main Span assembly site from across the Mississippi River A view of the site where the Main Span – with its two arch ribs – will be lifted into place soon; the existing bridge stands in the background. Looking at the arches from another perspective A closer look at the Main Span. The arch ribs are temporarily supported by "shoring towers." These will be removed before the Main Span is lifted up and moved out to barges by transporters. Underneath the floor system of the Main Span; the deck for the span will be poured after it is moved into place.
April 2012 Another perspective of the Main Span in the staging area. The existing bridge can be seen on the far left. A view of the deck of the southbound lanes for the new South Approach Girders spanning between Piers 7 and 8 Forms and rebar in place for the North Approach in the foreground, with the existing bridge in the background Looking at the arches from another perspective Looking between two girders before they are moved into place. The pier at the other side of the river is Pier 5. It's helpful to have a number of cranes on site for complex projects like moving 115-ton concrete girders
March 2012 There is very little wiggle room when placing one of these girders. There are little "nubs" on the pier that need to line up with holes on the bottom of the girders. Another massive concrete girder arrives on site. The girder and truck with specialized trailer make the descent down to the staging area. A spotter (on the left) walks alongside. It takes a pretty heavy duty crane to lift 116 tons. With three girders in place, a fourth is slowly brought in. Girder length: 174 feet. Crews secure a temporary support before hoisting it into place. As the girder arrives at the staging area, crews help maneuver things into place prior to the lift.
February 2012 A close up view of the post-tensioning ducts located on the cap of Pier 6. Crews will run cables through these ducts and then use machinery to add tension to the cables so they provide the proper support for the bridge. Another view of the post-tensioning ducts as they run through the pier cap of Pier 6. Eventually, crews will pour concrete around these ducts. A close up view of the giant concrete "knuckle" underway at Pier 5. Gracie the tugboat is used to move things on the river. Another view of the post-tensioning ducts on Pier 6. An inspector takes a close look at the post-tensioning ducts. Crews secure a temporary support before hoisting it into place. One of the project's many cranes lifts one of the many large components used to build temporary support structures.
December 2011 After a wet spring and summer created challenges for the project, excellent fall weather resulted in a flurry of construction and produced this late fall sunset over the Mississippi River. A night time view of the construction site with the existing bridge in the background (colors are enhanced). A close up look at Pier 5 after pier cap work begins. A November snow falls upon the construction site. At the north approach, concrete girders are in place between Pier 10 and the north abutment. Pier 9, complete with pier cap. The top of Pier 10's pier cap and the massive beams that rest upon it can be seen through the center of Pier 9. Crews work on the upper reaches of Pier 5 near downtown Hastings. Even if it's cold, the work needs to be done. Two crew members pump concrete in winter at Pier 5. Warm concrete gets delivered to the construction site, then trucked over the causeway and onto a barge before being pumped into the forms.
South Approach (Fall 2011) Falsework – or temporary support structures – holds up the forms for the southbound lanes of the new south approach. Forms in place for the southbound lanes of the new south approach. A close up look at Pier 5 after pier cap work begins. A partial view of Pier 5 (left) and the existing bridge (right). A close up look at Pier 5 after pier cap work begins.
North Approach Crews work on Pier 8. A close up view of a rebar structure used inside one of the piers. Looking down at Piers 6 (left) and 7 (right) during pile driving and prior to cofferdam dewatering. A view of the new bridge construction with the existing bridge in the background. Looking southeast at a closed 2nd Street. Although this section of road is closed, Historic Downtown Hastings remains easily accessible. From closest to furthest – Pier 2 Southbound, Pier 3 Southbound, Pier 4 Southbound. Filling the east access ramp back in after weekend utility work. Downtown Hastings is in the background. . Filling in the east access ramp back in after utility work. Another view of Pier 4 Southbound under construction. A completed Southbound Pier 3 A look at the insides of a pier before the forms go up. This is the base of the stem (column) for Pier 4 northbound. A worker readies the form for the Southbound Pier 2. A completed pier (Southbound Pier 3) and a pier under construction (Southbound Pier 4). Southbound Pier 4 from another angle. Putting the form into place for Pier 2 Southbound. Two piers under construction-Northbound Pier 4 on the left; Southbound Pier 4 on the right. Putting the form into place for Pier 2 Southbound. Welding a pier form for Pier 2 Southbound. Putting up the forms for the Southbound Pier 1 stem. View underneath the existing bridge. Looking south from the project's northern staging area near Hub's Landing Marina. In the background, forms are in place for Pier 10. On the right, forms and rebar are placed prior to pouring concrete for the north approach retaining wall. A close up look at some of the rebar that will be inside the north retaining wall. Looking south from the project's northern staging area near Hub's Landing Marina. Part of the north approach's retaining wall emerges from the forms. A mallard checks out the north side construction staging area In the foreground, completed pile caps. Crews ready pile cap forms in the ground improvement area northwest of the existing bridge. The pile caps will become part of the support structure for the new bridge's north approach. Crews place a concrete bucket prior to pouring. Crews release the bottom of the bucket and let the concrete flow into the pile cap form. Finishing touches on the pile cap. A worker places reinforcing steel to help steady the pier stem template. A worker places reinforcing steel to help steady the pier stem template (2nd shot) Crews work on the pier stem for Pier 2 (southbound lanes). Pier 5's foundation girder rebar is formed and ready to be placed before concrete is poured. Digging the trench for new sewer and water lines between the river and 2nd Street. Starting to move Pier 5 foundation girder rebar into place. Water overflowing the banks along the north side staging area creates a mirror image of the existing bridge. Pier 9, looking north across the river near Historic Downtown Hastings. Pier 9's foundation with rebar for pier stems (or columns).


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You can check out the original version of the Jet Car and the printing process in my earlier post.
Had to get creative to clean this one. |
Had to get creative to clean this one. |
Was that the true color of the jet car? What you only need is to color the jet car to give a lively look to it.
ReplyDeleteHi Harold, you can see what the original Jet Car looks like in my earlier post: http://opus5.complex88.com/2012/01/jet-car-my-first-3d-print.html
I would love to paint both the Jet Car and Octopod to make them look even better. It's on a long list of things to do! Just haven't had the time yet.
Thanks for the comments!
I just do wonder if where you got this cleaning material. Does this thing also work for car parts?
ReplyDeleteThe machine I'm using is an ultrasonic cleaner, just Google it for buying options. The sodium hydroxide (lye) is used in water to make the cleaning solution. You can get lye from photo places (I got mine from B&H Photo but it's pick-up only) not sure where else to get it. The ultrasonic cleaner would work for cleaning car parts but with a different solution than lye. You'd have to research what would work.