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    • 2. 发明授权
    • Methods of reducing the chloride content of epoxy compounds
    • 降低环氧化合物氯化物含量的方法
    • US06211389B1
    • 2001-04-03
    • US09578785
    • 2000-05-23
    • Mark Thomas Dimke
    • Mark Thomas Dimke
    • C07D30132
    • C07D301/32C08G59/025
    • 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.
    • 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)。
    • 5. 发明申请
    • DISTILLED EPOXY NOVOLAC RESINS
    • 蒸馏环氧NOVOLAC树脂
    • US20160304660A1
    • 2016-10-20
    • US15103097
    • 2014-12-17
    • BLUE CUBE IP LLC
    • William W. FanDennis W. JewellStephen B. WallaceMarvin L. DettloffTravis H. Larsen
    • C08G59/02B01D3/32B01D5/00
    • C08G59/025B01D3/32B01D5/006C08G59/08
    • 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.
    • 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。
    • 9. 发明授权
    • Distilled epoxy novolac resins
    • US09644067B2
    • 2017-05-09
    • US15103100
    • 2014-12-17
    • BLUE CUBE IP LLC
    • William W. FanDennis W. JewellStephen B. WallaceTravis H. Larsen
    • C08G59/02C08G59/08C08F6/28
    • C08G59/025C08G59/08
    • 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.
    • 10. 发明授权
    • Process for preparing epoxy resins
    • 制备环氧树脂的方法
    • US08962792B2
    • 2015-02-24
    • US13816258
    • 2011-09-07
    • Robert E. Hefner, Jr.
    • Robert E. Hefner, Jr.
    • C08G59/02C08G59/14C08G65/26C07D301/28C07D301/32C08G65/04C08G59/00
    • C08G65/2696C07D301/28C07D301/32C08G59/025Y02P20/582
    • 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).
    • 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。