公开(公告)号：US5449701A

公开(公告)日：1995-09-12

申请号：US357619

申请日：1994-12-15

申请人： Ben Duh

发明人： Ben Duh

IPC分类号： C08G63/189 ,  C08G63/78 ,  C08G63/80 ,  C08J9/12 ,  C08J9/30 ,  C08G63/88

CPC分类号： C08J9/30 ,  C08G63/80 ,  C08J9/122 ,  C08J2367/02

摘要： This invention includes a process for preparing a solid state polymerized poly(ethylene naphthalate)or PEN polymer comprising: (1) preparing a molten PEN polymer with an intrinsic viscosity of from about 0.25 dl/g to about 0.55 dl/g, (2) dispersing an inert gas into the molten PEN polymer to form a foamed PEN polymer with a void fraction of from about 0.10 to about 0.50, (3) forming the foamed PEN polymer into granules, (4) devolatilizing the granular PEN polymer at a temperature of from about 80.degree. C. to about 140.degree. C., (5) crystallizing the devolatilized PEN polymer at a temperature of from about 150.degree. C. to about 260.degree. C., and (6) solid state polymerizing the crystallized PEN polymer at a temperature of from about 235.degree. C. to about 265.degree. C. to form a solid state polymerized PEN product.

摘要翻译： 本发明包括一种制备固态聚合的聚萘二甲酸乙二醇酯或PEN聚合物的方法，包括：（1）制备特性粘度为约0.25dl / g至约0.55dl / g的熔融PEN聚合物，（2） 将惰性气体分散到熔融PEN聚合物中以形成具有约0.10至约0.50的空隙率的泡沫PEN聚合物，（3）将泡沫PEN聚合物形成颗粒，（4）在颗粒状PEN聚合物的脱挥发分化温度 约80℃至约140℃，（5）在约150℃至约260℃的温度下使脱挥发份的PEN聚合物结晶，和（6）使结晶的PEN聚合物固态聚合 温度为约235℃至约265℃，以形成固态聚合的PEN产物。

公开(公告)号：US4374975A

公开(公告)日：1983-02-22

申请号：US345172

申请日：1982-02-02

申请人： Ben Duh

发明人： Ben Duh

IPC分类号： C08G63/00 ,  C08G63/78 ,  C08G63/80 ,  C08G63/70

CPC分类号： C08G63/80

摘要： A process for the continuous production of high molecular weight polyethylene terephthalate wherein the crystallized prepolymer having an intrinsic viscosity of at least 0.3 is dried, preheated and polymerized in a single moving bed reaction zone. The method is characterized by an inert gas atmosphere and a reaction zone with a temperature gradiant ranging from about 170.degree. C. at the uppermost portion and a higher temperature of about 225.degree. C. at the lowermost portion.

摘要翻译： 连续生产高分子量聚对苯二甲酸乙二醇酯的方法，其中特性粘度至少为0.3的结晶预聚物在单个移动床反应区中被干燥，预热和聚合。 该方法的特征在于惰性气体气氛和在最下部分具有约170℃的温度梯度和约225℃的较高温度的反应区。

公开(公告)号：US06461575B1

公开(公告)日：2002-10-08

申请号：US09309921

申请日：1999-05-11

申请人： Ben Duh ,  Ye-Mon Chen ,  Ann Marie Corey

发明人： Ben Duh ,  Ye-Mon Chen ,  Ann Marie Corey

IPC分类号： B01D900

CPC分类号： C08G63/88 ,  B29B9/16 ,  B29K2067/00 ,  B29K2995/0041

摘要： The pelletized product of melt condensation polymerization of 1,3-propanediol and terephthalic acid is crystallized in a vessel designed for continuous fluidized bed flow of the pellets in water at a temperature within the range of about 65 to about 100° C. Hot-water treatment in the vessel permits crystallization of the pellets in a continuous operation and results in an increase of the crystallinity of the polymer to greater than about 35% and an increase in pellet density.

摘要翻译： 1,3-丙二醇和对苯二甲酸的熔融缩聚的造粒产物在设计用于连续流化床流动的容器中在约65至约100℃范围内的水中在水中结晶。热水 在容器中的处理允许颗粒在连续操作中结晶，并导致聚合物的结晶度增加到大于约35％，并且颗粒密度增加。

公开(公告)号：US06403762B1

公开(公告)日：2002-06-11

申请号：US09891909

申请日：2001-06-26

申请人： Ben Duh

发明人： Ben Duh

IPC分类号： C08F600

CPC分类号： C08G63/80 ,  C08G63/183

摘要： The present invention is an improvement upon the process for producing poly(trimethylene terephthalate) (PTT) wherein 1,3-propanediol (PDO), and optionally other diols, and an aromatic diacid or diester thereof, and optionally other diacids or diesters, are esterified or transesterified and the esterification or transesterification product is polycondensed to produce a prepolymer which is solid state polymerized to produce a polymer with a desired intrinsic viscosity (IV). The prior art process includes the SSP prereaction steps of crystallization, drying/annealing, and preheating. The improvement in the present invention comprises crystallizing and preheating the PTT polymer in one step, without a drying/annealing step in between. Thus, the prepolymer still has a substantial moisture content when it is first exposed to the SSP reaction temperature inside the crystallizer/preheater.

摘要翻译： 本发明是对制备聚对苯二甲酸丙二醇酯（PTT）的方法的改进，其中1,3-丙二醇（PDO）和任选的其它二醇及其芳族二酸或二酯，以及任选的其它二酸或二酯是 酯化或酯交换，酯化或酯交换产物被缩聚以产生固态聚合以产生具有所需特性粘度（IV）的聚合物的预聚物。 现有技术的方法包括结晶，干燥/退火和预热的SSP预反应步骤。 本发明的改进包括在一个步骤中结晶和预热PTT聚合物，其间不进行干燥/退火步骤。 因此，当首次暴露于结晶器/预热器内的SSP反应温度时，预聚物仍然具有显着的水分含量。

公开(公告)号：US6124423A

公开(公告)日：2000-09-26

申请号：US339432

申请日：1999-06-24

申请人： Ben Duh ,  Edwin Andrew Sisson ,  Douglas David Callander

发明人： Ben Duh ,  Edwin Andrew Sisson ,  Douglas David Callander

IPC分类号： C08G63/189 ,  C08G63/80 ,  C08G63/88 ,  C08G63/02

CPC分类号： C08G63/88 ,  C08G63/189 ,  C08G63/80

摘要： A process for crystallizing a polyethylene naphthalate copolymer by:a) copolymerizing at least 60 mole % of 2,6-naphthalene dicarboxylic acid, based on the total moles of carboxylic acids, with polyols such as at least 80 mole % of ethylene glycol and from 2 mole % to 20 mole % of a polyol having three or more carbon atoms, each based on the total moles of polyols, to form PEN copolymer solids, andb) subsequently crystallizing the PEN copolymer solids by heating the solids to at least their sticking temperature at an average rate of at least 10.degree. C./min, to form agglomerate-free crystallized solids.The process may be performed under agitation. The pellets heated up in a during the crystallization step do not agglomerate or suddenly expand as the temperature rises to and through the sticking temperature of the PEN copolymers. The process allows one to rapidly heat up PEN during crystallization, and do so without conducting a prior drying step or a devolitilization step.

摘要翻译： 聚萘二甲酸乙二醇酯共聚物的结晶方法为：a）将至少60摩尔％的2,6-萘二羧酸与羧酸的总摩尔数与多元醇（例如至少80摩尔％的乙二醇）和 2摩尔％至20摩尔％的具有三个或更多个碳原子的多元醇，各自基于多元醇的总摩尔数，以形成PEN共聚物固体，和b）随后通过将固体加热至至少其粘附而结晶PEN共聚物固体 温度以至少10℃/分钟的平均速率，以形成无凝聚物的结晶固体。 该方法可以在搅拌下进行。 在结晶步骤中加热的颗粒在温度升高到并经过PEN共聚物的粘附温度时不会聚集或突然膨胀。 该方法允许在结晶期间快速加热PEN，并且不进行先前的干燥步骤或脱挥发步骤。

公开(公告)号：US5412063A

公开(公告)日：1995-05-02

申请号：US298702

申请日：1994-08-31

申请人： Ben Duh ,  William C. T. Tung

发明人： Ben Duh ,  William C. T. Tung

IPC分类号： C08J3/12 ,  B29B9/12 ,  B29K67/00 ,  C08G63/78 ,  C08G63/80 ,  C08G63/02 ,  C08F6/00 ,  C21B7/00

CPC分类号： C08G63/80

摘要： Polyester prepolymer granules with open-ended cavities provide greatly improved solid state polymerization rates by improving reaction by-product diffusion characteristics.

公开(公告)号：US5408035A

公开(公告)日：1995-04-18

申请号：US87446

申请日：1993-07-02

申请人： Ben Duh

发明人： Ben Duh

IPC分类号： C08G63/80 ,  C08F6/00 ,  C08G63/02

CPC分类号： C08G63/80

摘要： This invention is a process for solid state polymerization of polyester using multiple reactors in series to achieve molecular weight increases, as measured by intrinsic viscosity, in excess of 0.25 dl/g with low levels of undesirable by-products.

摘要翻译： 本发明是使用多个反应器串联的聚酯的固态聚合方法，以通过特性粘度测得的分子量增加超过0.25dl / g，并且具有低水平的不期望的副产物。

公开(公告)号：US06441129B2

公开(公告)日：2002-08-27

申请号：US09858171

申请日：2001-05-15

申请人： Ben Duh ,  Ann Marie Corey

发明人： Ben Duh ,  Ann Marie Corey

IPC分类号： C08F600

CPC分类号： C08G63/80 ,  C08G63/183

摘要： The present invention is a process for producing poly(trimethylene terephthalate) (PTT) at an increased solid state polymerization rate, wherein 1,3-propane diol and an aromatic acid or a dialkyl ester thereof are esterified or transesterified, the esterification or transesterification product is polycondensed, and the polycondensation product is pelletized and then subjected to continuous solid state polymerization at a temperature of 200 to 225° C., preferably 210 to 225° C. In one embodiment of the present invention, the temperature range is 200 to 220° C., and the pellet size of the polymer to be solid state polymerized is from 1.0 to 1.5 g/100. In another embodiment of the present invention, the solid state polymerization is carried out at 210 to 225° C. for from 1 to 20 hours and then the temperature is increased to above the initial melting point of the polymer to produce a PTT polymer with an intrinsic viscosity of 1.3 dl/g or greater.

摘要翻译： 本发明是以增加的固态聚合速率生产聚（对苯二甲酸丙二醇酯）（PTT）的方法，其中1,3-丙二醇和芳族酸或其二烷基酯被酯化或酯交换，酯化或酯交换产物 缩聚，缩聚产物造粒，然后在200〜225℃，优选210〜225℃的温度下进行连续固相聚合。在本发明的一个实施方案中，温度范围为200〜220 ℃，待固态聚合的聚合物的颗粒尺寸为1.0-1.5g / 100。 在本发明的另一个实施方案中，固态聚合在210-225℃下进行1至20小时，然后将温度升高到高于聚合物的初始熔点以产生具有 特性粘度为1.3dl / g以上。

公开(公告)号：US06297315B1

公开(公告)日：2001-10-02

申请号：US09309923

申请日：1999-05-11

申请人： Ben Duh ,  Ye-Mon Chen ,  Ann Marie Corey

发明人： Ben Duh ,  Ye-Mon Chen ,  Ann Marie Corey

IPC分类号： C08L6702

CPC分类号： B29B9/16 ,  B29K2067/00 ,  B29K2995/0041 ,  C08G63/88

摘要： The pelletized product of melt condensation polymerization of 1,3-propanediol and terephthalic acid (or alkyl ester thereof) is crystallized by immersion in water at a temperature within the range of 60 to about 100° C. Hot-water treatment increases the crystallinity of the polymer to at least about 35% and increases pellet density to about 1.33 g/cm3.

摘要翻译： 将1,3-丙二醇和对苯二甲酸（或其烷基酯）的熔融缩聚的造粒产物在60至100℃的温度范围内浸入水中结晶。热水处理使结晶度提高 该聚合物至少约35％，并将颗粒密度增加至约1.33g / cm 3。

公开(公告)号：US6113997A

公开(公告)日：2000-09-05

申请号：US316347

申请日：1999-05-21

申请人： Freddie Lee Massey ,  Deborah Ann Snell Tung ,  Millicent Louise Martin-Shultz ,  Ben Duh ,  Charles Louis Kern, Jr.

发明人： Freddie Lee Massey ,  Deborah Ann Snell Tung ,  Millicent Louise Martin-Shultz ,  Ben Duh ,  Charles Louis Kern, Jr.

IPC分类号： B29C49/00 ,  C08G63/181 ,  C08G63/183 ,  C08G63/78 ,  C08G63/80 ,  B29D22/00 ,  C08G63/16

CPC分类号： B29C49/0005 ,  C08G63/78 ,  C08G63/80 ,  C08G63/181 ,  C08G63/183 ,  Y10T428/1352 ,  Y10T428/1397

摘要： A process is disclosed to prepare a polyester resin having a predetermined acetaldehyde (AA) content whereby the IV of the melt phase resin is constrained to a certain range resulting in a longer SSP time to achieve a higher level of IV for the resin with an AA content of 1 PPM or less. The resultant resin can be transformed into a bottle preform, which, when blown, forms a bottle suitable for packaging of mineral water.

摘要翻译： 公开了一种制备具有预定乙醛（AA）含量的聚酯树脂的方法，其中熔融相树脂的IV被限制在一定范围，导致更长的SSP时间以获得具有AA的树脂的较高水平的IV 含量1 PPM以下。 所得到的树脂可以转化成瓶预成型件，当吹制时，其形成适于包装矿泉水的瓶子。