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1. 发明申请

WO1997021757A1 IMPROVED METHOD FOR RECOVERING DIACETATE ESTERS OF POLYTETRAMETHYLENE ETHERS 审中-公开
标题翻译：改进聚对苯二甲酸乙二醇酯酯的方法
公开(公告)号：WO1997021757A1
公开(公告)日：1997-06-19
申请号：PCT/US1996019355
申请日：1996-12-05
申请人： E.I. DU PONT DE NEMOURS AND COMPANY
发明人： E.I. DU PONT DE NEMOURS AND COMPANY , DORAI, Suriyanarayan
IPC分类号： C08G65/30
CPC分类号： C08G65/30 , C08G65/20
摘要： An improved method for recovering purified diesters of polytetramethylene ethers involving the polymerization of tetrahydrofuran (THF) optionally with one or more comonomers (e.g., 3-methyl THF, ethylene oxide, propylene oxide, or the like) utilizing a solid acid catalyst (e.g., Nafion3) and a carboxylic acid with carboxylic acid anhydride (e.g., acetic acid with acetic anhydride) as molecular weight control agents wherein after polymerization product recovery involves bulk flashing of unreacted THF and stripping of remaining THF, carboxylic acid and carboxylic acid anhydride (e.g., acetic acid and acetic anhydride) by use of superheated THF. Such a process is useful in producing high purity commercial grade PTMEA that advantageously avoids problems associated with the presence of high boilers when converting to PTMEG.
摘要翻译：一种改进的用于回收纯化的二聚四亚甲基二酯的方法，该方法涉及使用固体酸催化剂（例如，一种或多种）将任选地与一种或多种共聚单体（例如3-甲基THF，环氧乙烷，环氧丙烷等）聚合的四氢呋喃（THF） Nafion3）和羧酸与羧酸酐（例如，乙酸与乙酸酐）作为分子量控制剂，其中聚合后产物回收涉及未反应的THF的大量闪蒸和其余的THF，羧酸和羧酸酐的洗脱（例如，乙酸和乙酸酐），使用过热THF。这种方法可用于生产高纯度商业级PTMEA，其有利地避免了当转化为PTMEG时与高锅炉的存在相关的问题。

2. 发明申请

WO1997023559A2 ALKANOLYSIS OF POLYETHER POLYOL ESTERS BY REACTIVE DISTILLATION 审中-公开
标题翻译：通过反应性蒸馏分离聚醚多糖酯
公开(公告)号：WO1997023559A2
公开(公告)日：1997-07-03
申请号：PCT/US1996019464
申请日：1996-12-05
申请人： E.I. DU PONT DE NEMOURS AND COMPANY
发明人： E.I. DU PONT DE NEMOURS AND COMPANY , DORAI, Suriyanarayan
IPC分类号： C08L00/00
CPC分类号： C08G65/20 , C08G65/3312 , Y02P20/127
摘要： A method for converting the diester of a polyether polyol (e.g., the diacetate ester of polytetramethylene ether, PTMEA) to a corresponding dihydroxy polyether polyol (e.g., polytetramethylene ether glycol, PTMEG) involving reactive distillation wherein a diester of polyether polyol is fed to the top portion of the column along with an effective amount of at least one alkali metal oxide or alkaline earth metal oxide, hydroxide or alkoxide catalyst (e.g., sodium methoxide) and with a C1 to C4 alkanol (e.g., methanol) while simultaneously adding to the bottom of the reactive distillation column hot alkanol vapor to sweep any alkanol ester formed by alkanolysis of the diester of polyether polyol upwardly. Such a process is useful for achieving high levels of conversion PTMEA to PTMEG on a commercial scale with the overhead from the column being amenable to azeotropic separation of the methyl acetate and recycle of the methanol.
摘要翻译：将聚醚多元醇（例如，聚四亚甲基醚的二乙酸酯，PTMEA）的二酯转化为涉及反应性蒸馏的相应的二羟基聚醚多元醇（例如聚四亚甲基醚二醇，PTMEG）的方法，其中将聚醚多元醇的二酯加入到塔的顶部以及有效量的至少一种碱金属氧化物或碱土金属氧化物，氢氧化物或醇盐催化剂（例如甲醇钠）和C1-C4链烷醇（例如甲醇），同时加入到底部的反应蒸馏塔热链烷醇蒸气洗涤通过向上聚醚多元醇的二酯的链烷分解形成的任何链烷醇酯。这种方法对于实现高水平的商业规模的PTMEA到PTMEG的转化是有用的，其中塔的塔顶馏分适于乙酸甲酯的共沸分离和甲醇的再循环。

3. 发明申请

WO1993018084A1 REDUCTION OF MOLECULAR WEIGHT OF POLY(TETRAMETHYLENE ETHER) GLYCOL 审中-公开
标题翻译：降低分子量的聚（四乙烯醚）甘油
公开(公告)号：WO1993018084A1
公开(公告)日：1993-09-16
申请号：PCT/US1993002212
申请日：1993-03-10
申请人： E.I. DU PONT DE NEMOURS AND COMPANY
发明人： E.I. DU PONT DE NEMOURS AND COMPANY , DORAI, Suriyanarayan
IPC分类号： C08G65/32
CPC分类号： C08G65/3322 , C07C43/135 , C08G2650/12
摘要： A process for reducing the molecular weight of polytetramethylene ether glycol without significant conversion of polytetramethylene ether glycol to tetrahydrofuran monomer is disclosed. The process involves a two-step procedure. The first step comprises reacting polytetramethylene ether glycol with a perfluoroalkyl carboxylic acid to form a perfluoroalkyl ester of polytetramethylene ether glycol. That ester is, in the second step, converted back to polytetramethylene ether glycol of reduced molecular weight by hydrolysis or alcoholysis.

4. 发明申请

WO1993018083A1 REDUCING MOLECULAR WEIGHT DISTRIBUTION OF POLYETHER GLYCOLS BY SHORT-PATH DISTILLATION 审中-公开
标题翻译：通过短程蒸馏降低聚乙二醇的分子量分布
公开(公告)号：WO1993018083A1
公开(公告)日：1993-09-16
申请号：PCT/US1993001525
申请日：1993-02-26
申请人： E.I. DU PONT DE NEMOURS AND COMPANY
发明人： E.I. DU PONT DE NEMOURS AND COMPANY , DORAI, Suriyanarayan , RAWLINGS, Frank, Leslie, Jr. , SCHULTZ, James, A.
IPC分类号： C08G65/30
CPC分类号： B01D3/12 , C08G18/4854 , C08G65/20 , C08G65/30 , Y10S159/16
摘要： Polyether glycols, especiallly poly(tetramethylene ether) glycol (PTMEG) having a narrow molecular weight distribution of about 1.25 to 1.80, or dispersity of 1.05 to 1.90, are made by a process which consists of distilling the low molecular weight fraction in unit operations comprising at least one short-path distillation evaporator. Two short-path distillation evaporators, in series, are desirable if significant narrowing of the PTMEG is required. In these units, PTMEG is subjected to temperatures in the range of 150 DEG -400 DEG C with the hold-up time varying between 10-200 seconds. The required vacuum to force the separation of the low molecular weight PTMEG varies between 0.001 mm and 1.0 mbar. PTMEG residue from the distillation unit is also characterized by its low water content and low concentration of oligomeric cyclic ethers.
摘要翻译：聚醚二醇，特别是具有约1.25至1.80的窄分子量分布或1.05至1.90的分散性的聚（四亚甲基醚）二醇（PTMEG）通过以下步骤制备，该方法包括在单元操作中蒸馏低分子量级分，包括至少一个短路蒸馏蒸发器。如果需要PTMEG的显着变窄，则需要两个串联的短路蒸馏蒸发器。在这些单元中，PTMEG的温度范围为150°-400℃，保持时间在10-200秒之间变化。强制分离低分子量PTMEG所需的真空度在0.001毫米至1.0毫巴之间变化。来自蒸馏单元的PTMEG残余物的特征还在于其低含水量和低浓度的低聚环醚。

5. 发明申请

WO1997021756A1 IMPROVED METHOD FOR MANUFACTURING DIACETATE ESTERS OF POLYTETRAMETHYLENE ETHERS 审中-公开
标题翻译：制备聚对苯二甲酸乙二醇酯的改进方法
公开(公告)号：WO1997021756A1
公开(公告)日：1997-06-19
申请号：PCT/US1996019356
申请日：1996-12-05
申请人： E.I. DU PONT DE NEMOURS AND COMPANY
发明人： E.I. DU PONT DE NEMOURS AND COMPANY , DORAI, Suriyanarayan , TRUSZKOWSKI, Donald
IPC分类号： C08G65/20
CPC分类号： C08G65/2696 , C08G65/20
摘要： An improved method for manufacturing diesters of polytetramethylene ethers involving the polymerization of tetrahydrofuran (THF) optionally with one or more comonomers (e.g., 3-methyl THF, ethylene oxide, propylene oxide, or the like) utilizing a solid acid catalyst (e.g., Nafion3) and a carboxylic acid with carboxylic acid anhydride (e.g., acetic acid with acetic anhydride) as molecular weight control agents wherein setting the pressure of the reactor while simultaneously achieving removal of the heat of reaction by operating under solvent/monomer evaporative reaction conditions effectively controls the reaction temperature. Such a process is useful in producing high purity commercial grade PTMEA that advantageously avoids problems caused by the high heat of reaction when such a process is scaled up to commercial level.
摘要翻译：涉及用四氢呋喃（THF）任选与一种或多种共聚单体（例如3-甲基THF，环氧乙烷，环氧丙烷等）一起使用固体酸催化剂聚合的改进的聚四亚甲基二酯的方法（例如，Nafion3 ）和羧酸与羧酸酐（例如乙酸与乙酸酐）作为分子量控制剂，其中设定反应器的压力同时通过在溶剂/单体蒸发反应条件下操作来实现去除反应热有效地控制反应温度。这种方法可用于生产高纯度商业级PTMEA，其有利地避免当这种方法扩大到商业水平时由高的反应热引起的问题。

6. 发明申请

WO1997021755A1 PREVENTION OF GEL FORMATION DURING USE OF AND PRESERVING/REGENERATING ACTIVITY OF NAFION-TYPE POLYMERIZATION CATALYST 审中-公开
标题翻译：在使用和保存/再生NAFION型聚合催化剂活性期间防止凝胶形成
公开(公告)号：WO1997021755A1
公开(公告)日：1997-06-19
申请号：PCT/US1996019354
申请日：1996-12-05
申请人： E.I. DU PONT DE NEMOURS AND COMPANY
发明人： E.I. DU PONT DE NEMOURS AND COMPANY , SCHULTZ, James, A. , DORAI, Suriyanarayan
IPC分类号： C08G65/20
CPC分类号： C08G65/2696 , C08G65/20 , Y02P20/584
摘要： A method of suspending the manufacture of diesters of polytetramethylene ethers by polymerizing THF or the like in a reactor utilizing a solid catalyst containing sulfonic acid groups in a liquid reaction medium containing a carboxylic acid with carboxylic acid anhydride (e.g., acetic acid/acetic anhydride) as molecular weight control agents involving the stopping of the addition of reactant THF and carboxylic acid anhydride and simultaneously increasing the concentration of carboxylic acid in said reactor to sustain and preserve catalyst activity. Also, a spent solid acid catalyst containing sulfonic acid catalytic reactive sites deactivated from sustained use during such ring-opening polymerization of THF can be regenerated by contacting the spent catalyst with a solution of THF and carboxylic acid for a time sufficient to convert any alkylated sulfonic acid reactive site to the reactive sulfonic acid site. In both the suspending of polymerization and regeneration of spent catalyst, a 7 weight percent or greater solution of acetic acid in THF has been found to be effective in preserving/restoring catalyst activity.
摘要翻译：在含有羧酸酐的液体反应介质（例如乙酸/乙酸酐）中，通过在含有磺酸基的固体催化剂的反应器中聚合THF等来悬浮聚四亚甲基二醇二酯的方法，作为涉及停止加入反应物THF和羧酸酐的分子量控制剂，同时增加所述反应器中羧酸的浓度以维持并保持催化剂活性。此外，在THF的这种开环聚合期间，含有在持续使用中失活的磺酸催化反应性位点的废固体酸催化剂可以通过使废催化剂与THF和羧酸的溶液接触足以将任何烷基化磺酸酸反应性位点与反应性磺酸位点。在废催化剂的聚合和再生的悬浮液中，发现乙酸在THF中的7重量％或更多的溶液在保存/恢复催化剂活性方面是有效的。

7. 发明申请

WO1992014773A1 PREPARATION OF POLYTETRAMETHYLENE ETHER GLYCOL USING AN ACIDIC ZIRCONIA CATALYST 审中-公开
标题翻译：使用酸性ZIRCONIA催化剂制备聚丙烯酰胺乙二醇
公开(公告)号：WO1992014773A1
公开(公告)日：1992-09-03
申请号：PCT/US1992000693
申请日：1992-02-06
申请人： E.I. DU PONT DE NEMOURS AND COMPANY
发明人： E.I. DU PONT DE NEMOURS AND COMPANY , BAKER, Melvin, Charles , DORAI, Suriyanarayan , SCHULTZ, James, Arnold
IPC分类号： C08G65/20
CPC分类号： C08G65/266 , C08G65/20
摘要： A process for polymerizing tetrahydrofuran to produce polytetramethylene ether glycol or ester-capped polytetramethylene ether glycol is disclosed. The reaction mass is carried out at 10° to 80 °C and preferably 20° to 60 °C. In a preferred aspect of the invention, a mixture of acetic anhydride and acetic acid is present in the reaction mixture.

8. 发明申请

WO1992014548A1 POLYMERIZING TETRAHYDROFURAN TO PRODUCE POLYTETRAMETHYLENE ETHER GLYCOL USING A MODIFIED FLUORINATED RESIN CATALYST CONTAINING SULFONIC ACID GROUPS 审中-公开
标题翻译：聚四氟乙烯生产聚亚甲基乙二醇的方法，使用含有磺酸基团的改性氟化树脂催化剂
公开(公告)号：WO1992014548A1
公开(公告)日：1992-09-03
申请号：PCT/US1992000695
申请日：1992-02-06
申请人： E.I. DU PONT DE NEMOURS AND COMPANY
发明人： E.I. DU PONT DE NEMOURS AND COMPANY , DORAI, Suriyanarayan , MARSI, Marianne , PRUCKMAYR, Gerfried , QUON, Willard, L.
IPC分类号： B01J31/10
CPC分类号： C08G65/20 , C07C41/01 , C07C43/135
摘要： A catalyst and process for preparing it and its use in polymerizing tetrahydrofuran to produce polytetramethylene ether glycol ether are disclosed. The catalyst is a blend of a fluorinated resin containing sulfonic acid groups and a fluorinated resin containing carboxylic acid groups. The catalyst is partially dried to contain from 1,000 to 2,000 ppm water, so that when it is used to polymerized tetrahydrofuran, the product polytetramethylene ether glycol will have a number average molecular weight of from 250 to 4,000.

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