公开(公告)号：US4668807A

公开(公告)日：1987-05-26

申请号：US807566

申请日：1985-12-11

申请人： Jacques Darbellay ,  Gerald Dessauges

发明人： Jacques Darbellay ,  Gerald Dessauges

IPC分类号： C07D303/20 ,  C07D301/26 ,  C07D301/28 ,  C07D301/32 ,  C07D303/24 ,  C07D303/32 ,  C07D303/36 ,  C08G59/00 ,  C08G59/04

CPC分类号： C08G59/00 ,  C07D303/24 ,  C08G59/025

摘要： To reduce the content of hydrolyzable chlorine in glycidyl compounds, these are dissolved in a halogen-free organic solvent and treated with an equivalent excess of aqueous alkali metal hydroxide solution at elevated temperature, the excess being 100 to 200% of the equivalent amount theoretically required for complete dehydrochlorination of the hydrolyzable chlorine, the water is then removed from the organic solution, the organic solution is treated with 5 to 500 times the amount, based on the amount of alkali metal hydroxide employed, of moist cellulose containing up to 35% by weight of water at elevated temperature and, after filtration, the glycidyl compound is isolated from the organic solution.

摘要翻译： 为了降低缩水甘油基化合物中的可水解氯的含量，将它们溶解在无卤素的有机溶剂中，并在高温下用等量过量的碱金属氢氧化碱水溶液处理，其余量为理论上所需的当量的100至200％ 为了对可水解的氯进行完全的脱氯化氢，然后从有机溶液中除去水，有机溶液用基于所用碱金属氢氧化物的量的5至500倍的量处理含有至多35％的湿纤维素 在高温下的水重量，并且在过滤后，从有机溶液中分离缩水甘油基化合物。

公开(公告)号：US06211389B1

公开(公告)日：2001-04-03

申请号：US09578785

申请日：2000-05-23

申请人： Mark Thomas Dimke

发明人： Mark Thomas Dimke

IPC分类号： C07D30132

CPC分类号： C07D301/32 ,  C08G59/025

摘要： In accordance with the present invention, methods have been developed for the reduction of the chloride content of epoxy compound starting materials. Invention methods comprise subjecting specifically defined combinations comprising an epoxy resin starting material and other components to conditions sufficient to produce a treated epoxy compound (i.e., an epoxy compound having a chloride content which is reduced relative to that of the epoxy resin starting material), and separating the treated epoxy compound from the combination. Other components contemplated for use in the practice of the present invention comprise, alternatively, mixtures of crown ether, organic solvent and suitable base; mixtures of crown ether-like solvent and suitable base; mixtures of aprotic solvents and hydrides (other than tin hydride); mixtures of nonhalogenated organic solvent and reducing metal; and the like. In accordance with a further aspect of the present invention, products (i.e., treated epoxy compounds, encapsulants and fillers) are provided which have been produced by the invention methods.

摘要翻译： 根据本发明，已经开发了用于降低环氧化合物起始材料的氯化物含量的方法。 本发明的方法包括将包含环氧树脂起始材料和其它组分的具体限定的组合经受足以产生经处理的环氧化合物（即相对于环氧树脂原料的氯化物含量降低的环氧化合物）的条件，以及 将处理的环氧化合物与组合物分离。 考虑用于本发明实践的其它组分包括冠醚，有机溶剂和合适碱的混合物; 冠醚类溶剂和合适碱的混合物; 非质子溶剂和氢化物（除氢化锡之外）的混合物; 非卤代有机溶剂和还原金属的混合物; 等等。 根据本发明的另一方面，提供了通过本发明方法生产的产品（即经处理的环氧化合物，密封剂和填料）。

公开(公告)号：US5106923A

公开(公告)日：1992-04-21

申请号：US658968

申请日：1991-02-21

申请人： James L. Bertram ,  Louis L. Walker ,  Avis L. McCrary ,  Fermin M. Cortez

发明人： James L. Bertram ,  Louis L. Walker ,  Avis L. McCrary ,  Fermin M. Cortez

IPC分类号： C08G8/08 ,  C08G59/08 ,  C08G59/32 ,  C08G59/62

CPC分类号： C08G59/3218 ,  C08G59/025 ,  C08G59/08 ,  C08G59/621 ,  C08G8/08

摘要： The 2-functional component of substituted phenol-aldehyde novolac resins is reduced. Epoxy novolac resins prepared from the novolac resin containing reduced quantities of 2-functional product exhibit increased Tg values when cured.

摘要翻译： 取代酚醛酚醛清漆树脂的2官能组分被还原。 含有减少量2-功能产物的酚醛清漆树脂制备的环氧酚醛树脂在固化时表现出增加的Tg值。

公开(公告)号：US4026761A

公开(公告)日：1977-05-31

申请号：US703343

申请日：1976-07-08

申请人： Silvio Vargiu ,  Giancarlo Crespolini ,  Giulio Grazzini

发明人： Silvio Vargiu ,  Giancarlo Crespolini ,  Giulio Grazzini

IPC分类号： C07D303/24 ,  C08G59/00 ,  C08G59/06 ,  C09D5/46 ,  B01D1/22

CPC分类号： C08G59/00 ,  C08G59/025 ,  C08G59/063 ,  Y10S159/08 ,  Y10S159/15 ,  Y10S159/16

摘要： Diepoxides of the general formula: ##STR1## wherein n has an average value not exceeding 0.03 and R is the bisphenyl radical of bisphenol-A are recovered from an epoxy resin of the same general formula with n varying from 0.07 to 0.30, by removing the low-boiling substance from the epoxy resin at 0.1-1 mm Hg and 165.degree.-200.degree. C and distilling off said diepoxide from the thus treated epoxy resin at 0.1-0.005 mm Hg and a temperature not exceeding 240.degree. C. The low viscosity, narrow molecular weight distribution and excellent purity of these diepoxides allow their use in critical application fields.

摘要翻译： 其中n的平均值不超过0.03，R是双酚A的双苯基由具有相同通式的环氧树脂回收，其中n为0.07-0.30， 通过在0.1-1mmHg和165℃-200℃下从环氧树脂中除去低沸点物质，并将该二环氧化物从如此处理的环氧树脂中以0.1-0.005mm Hg和不超过240℃的温度蒸馏掉。 这些二环氧化物的低粘度，窄分子量分布和优异的纯度使其可用于关键应用领域。

公开(公告)号：US20160304660A1

公开(公告)日：2016-10-20

申请号：US15103097

申请日：2014-12-17

申请人： BLUE CUBE IP LLC

发明人： William W. Fan ,  Dennis W. Jewell ,  Stephen B. Wallace ,  Marvin L. Dettloff ,  Travis H. Larsen

IPC分类号： C08G59/02 ,  B01D3/32 ,  B01D5/00

CPC分类号： C08G59/025 ,  B01D3/32 ,  B01D5/006 ,  C08G59/08

摘要： A continuous process comprising a) separating an epoxy novolac resin comprising oligomers having an average functionality of greater than 2.5 and a hydrolyzable chlorine content of less than 450 ppm with a continuous evaporator apparatus to form i) a first distillate vapor fraction comprising epoxy novolac resin having more than 75 weight percent of 2 functional components and wherein the mass of the first distillate vapor fraction is in the range of from 15 to 40 weight percent of the starting epoxy novolac resin; and ii) a first bottom fraction comprising epoxy novolac resin having less than 5 weight percent of 2 functional components and having a glass transition temperature of at least 15 C higher compared to the starting epoxy novolac resin when cured; b) recovering the first bottom fraction product; and c) condensing the first distillate vapor fraction to form a first condensed distillate vapor fraction; d) separating the first condensed distillate vapor fraction with a second continuous evaporator apparatus to form i) a second distillate vapor fraction wherein the mass of the second distillate vapor fraction is in the range of from 40 to 70 weight percent of the first condensed distillate vapor fraction; and ii) a second bottom fraction; e) recovering the second bottom fraction product; and f) condensing the second distillate vapor fraction to form a second condensed distillate vapor fraction product comprising at least 98 weight percent of 2 functional components with a total chlorine content less than 900 ppm, is disclosed.

摘要翻译： 一种连续方法，其包括：a）第一蒸馏馏分，其包含环氧酚醛清漆树脂，其包含平均官能度大于2.5且低于450ppm的可水解氯含量小于450ppm的环氧酚醛清漆树脂， 大于75重量％的2个功能组分，并且其中第一馏出物蒸气馏分的质量在起始环氧酚醛清漆树脂的15至40重量％的范围内; 和ii）包含环氧酚醛清漆树脂的第一底部馏分，其与固化时的起始环氧酚醛清漆树脂相比，具有小于5重量％的2个功能组分并且玻璃化转变温度至少高15℃; b）回收第一底部馏分产物; 和c）冷凝第一馏出物蒸气馏分以形成第一冷凝馏出物蒸气馏分; d）用第二连续蒸发器装置分离第一浓缩馏出物蒸气馏分以形成i）第二馏出物蒸气馏分，其中第二馏出物蒸气馏分的质量在第一馏分馏出物的40至70重量％的范围内 分数; 和ii）第二底部馏分; e）回收第二底部馏分产物; 并且f）冷凝第二馏出物蒸气馏分以形成包含至少98重量％的总氯含量低于900ppm的2个功能组分的第二冷凝馏出物蒸气馏分产物。

公开(公告)号：US07932409B2

公开(公告)日：2011-04-26

申请号：US12057444

申请日：2008-03-28

申请人： Hazimah Abu Hassan ,  Tuan Noor Maznee Tuan Ismail ,  Mohd Norhisham Sattar ,  Seng Soi Hoong ,  Tian Lye Ooi ,  Salmiah Ahmad ,  Kosheela Devi a/p Poo Palam ,  Mei Yee Cheong

发明人： Hazimah Abu Hassan ,  Tuan Noor Maznee Tuan Ismail ,  Mohd Norhisham Sattar ,  Seng Soi Hoong ,  Tian Lye Ooi ,  Salmiah Ahmad ,  Kosheela Devi a/p Poo Palam ,  Mei Yee Cheong

IPC分类号： C07D301/32 ,  C08G65/02

CPC分类号： C07D301/32 ,  C08G18/36 ,  C08G59/025 ,  C08G59/027

摘要： A process for producing oleochemical polyols comprises the steps of epoxidizing unsaturated oil using an organic acid together with oxygenated water or a per-acid to obtain epoxidized oil; washing the epoxidized oil with salt water to remove unused organic acid together with oxygenated water or a per-acid; neutralizing acidic condition of the washed epoxidized oil with a base; washing the neutralized epoxidized oil with a salt solution until the pH of the neutralized epoxidized oil reaching 6.5 to 7.5 to removed the base residue; drying the washed neutralized epoxidized oil under vacuum; and reacting the washed neutralized dried epoxidized oil with polyhydric alcohol in the presence of boron trifluoride-diethylether complex to produce the oleochemical polyols. The oleochemical polyols are then subjected to the same washing, neutralizing, washing and drying process as in preparing the washed neutralized dried epoxidized oil.

摘要翻译： 一种制备油化多元醇的方法包括以下步骤：使用有机酸与含氧水或过酸环氧化不饱和油，得到环氧化油; 用盐水洗涤环氧化油，除去未使用的有机酸与氧化水或过酸; 用碱中和洗涤后的环氧化油的酸性条件; 用盐溶液洗涤中和的环氧化油直到中和的环氧化油的pH达到6.5-7.5以除去碱残渣; 在真空下干燥洗涤的中和的环氧化油; 并在三氟化硼 - 二乙醚络合物的存在下使洗涤的中和的干燥的环氧化油与多元醇反应，以产生油化学多元醇。 然后将油化多元醇进行与制备洗涤的中和的干燥的环氧化油相同的洗涤，中和，洗涤和干燥过程。

公开(公告)号：US06620907B2

公开(公告)日：2003-09-16

申请号：US09974201

申请日：2001-10-09

申请人： Roger A. Mader

发明人： Roger A. Mader

IPC分类号： C08F628

CPC分类号： C07D301/32 ,  C07D303/24 ,  C08G59/00 ,  C08G59/025 ,  Y10S525/93

摘要： The present invention provides a process for eliminating contaminants from epihalohydrin-derived epoxy resins. Another embodiment of the present invention is an epoxy product formed using said process. Yet another embodiment of the present invention is an epoxy derived in part from epihalohydrin wherein said epoxy is has a hydrolyzable halogen content of less than 10 ppm and an epoxide equivalent weight within 2 percent of the theoretical epoxide equivalent weight.

公开(公告)号：US20180319934A1

公开(公告)日：2018-11-08

申请号：US15770779

申请日：2016-10-19

申请人： Dow Global Technologies LLC

发明人： Troy E. Knight ,  Thomas C. Young ,  Gerald W. Dare ,  Hannah L. Crampton ,  Bruce D. Hook ,  Pasquale Sirignano ,  Daviele Vinci

IPC分类号： C08G65/24 ,  C08G65/12 ,  C08G65/46

CPC分类号： C08G59/04 ,  C08G59/022 ,  C08G59/025 ,  C08G59/22

摘要： Produce diglycidyl-capped polyalkylene glycol by (a) providing epihalohydrin, a polyalkylene glycol that contains and ethylene oxide component and a Lewis acid; (b) coupling the epihalohydrin to the polyalkylene glycol using the Lewis acid as a catalyst to produce a coupling product; (c) stripping 1,4-dioxane from the coupling product; and (d) epoxidation of the coupling product by addition of a base to form diglycidyl-capped polyalkylene glycol in an organic phase.

公开(公告)号：US09644067B2

公开(公告)日：2017-05-09

申请号：US15103100

申请日：2014-12-17

申请人： BLUE CUBE IP LLC

发明人： William W. Fan ,  Dennis W. Jewell ,  Stephen B. Wallace ,  Travis H. Larsen

IPC分类号： C08G59/02 ,  C08G59/08 ,  C08F6/28

CPC分类号： C08G59/025 ,  C08G59/08

摘要： A continuous process comprising: a) separating a starting epoxy novolac resin comprising oligomers having an average functionality of greater than 2.5 and a hydrolyzable chlorine content of less than 450 ppm with a first continuous evaporator apparatus under a vaporization temperature in the range of from 150° C. to 250° C. and an absolute pressure of from 0.05 to 1 mmHg absolute to form a first vapor fraction comprising epoxy novolac resin having more than 95 weight percent of 2-functional components and wherein the mass of the first vapor fraction is in the range of from 5 to 20 weight percent of the starting epoxy novolac resin; and a first bottom fraction comprising epoxy novolac resin having a lower weight percent of 2-functional components in comparison with the weight percent of 2-functional components of the starting epoxy novolac resin; b) recovering the first bottom fraction; and c) condensing from 95 weight percent to 99.95 weight percent of the first vapor fraction at a temperature in the range of from 50° C. to 200° C. to form a first partially condensed vapor fraction product having at least 95 weight percent of 2-functional components and having a total chlorine content of less than 900 ppm and an uncondensed vapor product comprising halogenated impurities, is disclosed.

公开(公告)号：US08962792B2

公开(公告)日：2015-02-24

申请号：US13816258

申请日：2011-09-07

申请人： Robert E. Hefner, Jr.

发明人： Robert E. Hefner, Jr.

IPC分类号： C08G59/02 ,  C08G59/14 ,  C08G65/26 ,  C07D301/28 ,  C07D301/32 ,  C08G65/04 ,  C08G59/00

CPC分类号： C08G65/2696 ,  C07D301/28 ,  C07D301/32 ,  C08G59/025 ,  Y02P20/582

摘要： A process for preparing an aliphatic or cycloaliphatic epoxy resin including the steps of: (I) reacting a mixture of (a) an aliphatic or cycloaliphatic hydroxyl containing material, (b) an epihalohydrin, (c) a basic acting substance, (d) a non-Lewis acid catalyst, and (e) optionally, a solvent, forming an epoxy resin composition; (II) subjecting the epoxy resin composition produced in step (I) to a separation process to remove (A) “light” components such as, for example, solvent used in the epoxidation reaction, if any, unreacted epihalohydrin, and co-products such as di(epoxypropyl)ether; (B) unreacted aliphatic or cycloaliphatic hydroxyl containing material, if any; (C) partially epoxidized aliphatic or cycloaliphatic hydroxyl containing material, such as, for example, MGE; (D) fully epoxidized aliphatic or cycloaliphatic hydroxyl containing material, such as, for example, DGE, such that the (E) aliphatic or cycloaliphatic polyfunctional epoxy resin product remaining contains no more than 50% by weight of said fully epoxidized aliphatic or cycloaliphatic hydroxyl containing material (D); and (III) recycling the isolated partially epoxidized aliphatic or cycloaliphatic hydroxyl containing material (C) and any mixtures of partially epoxidized aliphatic or cycloaliphatic hydroxyl containing material (C) with fully epoxidized aliphatic or cycloaliphatic hydroxyl containing material (D) from step (II) to a new reaction mixture of step (I).

摘要翻译： 一种制备脂族或环脂族环氧树脂的方法，包括以下步骤：（I）使（a）含脂肪族或脂环族羟基的材料，（b）表卤代醇，（c）碱性作用物质，（d） 非路易斯酸催化剂和（e）任选的形成环氧树脂组合物的溶剂; （II）将步骤（I）中制备的环氧树脂组合物进行分离处理以除去（A）“轻”成分，例如环氧化反应中使用的溶剂（如果有的话）未反应的表卤代醇和共同产物 如二（环氧丙基）醚; （B）未反应的脂肪族或脂环族羟基的物质，如果有的话; （C）部分环氧化脂族或脂环族羟基的材料，例如MGE; （D）完全环氧化的脂族或脂环族羟基的材料，例如DGE，使得（E）脂族或脂环族多官能环氧树脂产物含有不超过50重量％的所述完全环氧化的脂族或脂环族羟基 （D）; 和（III）将来自步骤（II）的分离的部分环氧化脂族或脂环族羟基的材料（C）和部分环氧化的含脂肪族或含脂环族羟基的材料（C）的混合物与完全环氧化的脂族或脂环族羟基化合物（D） 与步骤（I）的新的反应混合物。