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    • 37. 发明授权
    • Polybutylene terephthalates having a low carboxyl content and continuous
process for the production thereof
    • 具有低羧基含量的聚对苯二甲酸丁二酯和用于生产的连续方法
    • US4212963A
    • 1980-07-15
    • US968892
    • 1978-12-13
    • Gunter LehrRudolf Binsack
    • Gunter LehrRudolf Binsack
    • C08G63/00C08G63/78C08G63/18
    • C08G63/785C08G63/78
    • Polybutylene terephthalates having a narrow molecular weight distribution, a low carboxyl group content and an intrinsic viscosity of from 0.2 to 1.4 dl/g can be continuously produced by transporting a molten reaction mixture of terephthalic acid mono- and/or bis-(hydroxybutyl) ester or low viscosity polybutylene terephthalate at 160.degree. to 300.degree. C., together with a heated inert gas, in a diphasic annular stream through an externally heated spiral reaction tube (of substantially constant pitch) having a diameter of from 3 to 100 mm and a diameter/length ratio of from 1:400 to 1:2000 by the maintenance of a pressure difference between the beginning and the end of the reaction tube, under conditions such that the absolute pressure, determined at the point of entry of the reaction mixture into the tube, is from 1 to 100 bar and the viscosity of the annular stream is from 1 to 10,000 poises (determined at the reaction temperature), and a circular stream between the surface of the melt and the wall of the tube is produced by the curvature of the tube and a stream of gas flowing at a velocity of from 20 to 300 m/sec to accelerate the transport of material between the melt and the inert gas, whereby the reaction takes place in the liquid phase and/or at the melt/gas interface.
    • 通过将对苯二甲酸单 - 和/或双 - (羟基丁基)酯的熔融反应混合物输送,可以连续制备具有窄分子量分布,低羧基含量和特性粘度为0.2-1.4dl / g的聚对苯二甲酸丁二醇酯 或低粘度聚对苯二甲酸丁二醇酯在160℃至300℃下与加热的惰性气体一起通过直径为3至100mm的外部加热的螺旋反应管(基本上恒定的间距)和二价环状流 通过维持反应管的开始和结束之间的压力差,在使反应混合物进入点确定的绝对压力为 管子为1至100巴,环形流的粘度为1至10,000泊(在反应温度下确定),并且在熔体表面之间的圆形流 d管的壁由管的曲率和以20-300m / sec的速度流动的气流产生,以加速在熔体和惰性气体之间的材料的输送,从而发生反应 在液相和/或在熔体/气体界面处。
    • 39. 发明授权
    • Stabilization of polycondensates of polyethylene terephthalate
    • 聚对苯二甲酸乙二醇酯缩聚物的稳定化
    • US4115371A
    • 1978-09-19
    • US802858
    • 1977-06-02
    • Peter BierRudolf Binsack
    • Peter BierRudolf Binsack
    • C08L67/00C08G63/00C08G63/78C08G63/82C08K3/32D01F6/92C08G63/34C08G63/32
    • C08K3/32
    • A process for the production of high molecular weight low color polyethylene terephthalates using a particulaarly effective polycondensation catalyst is disclosed. Titanium tetrabutylate is added to the reaction mixture after the initial esterification or transesterification reaction is about 95% complete and the polycondensation is completed at temperatures between about 200 and 270.degree. C under reduced pressure. Metaphosphoric acid or its alkali or alkaline earth metal salts are added with the titanium tertrabutylate to control the color. Commonly accepted catalysts may be employed for the initial esterification or transesterification. Polymers with intrinsic viscosities in excess of 0.7 dl/g and yellowness numbers less than 6 can be produced.
    • 公开了一种使用特别有效的缩聚催化剂生产高分子量低颜色聚对苯二甲酸乙二醇酯的方法。 在初始酯化反应或酯交换反应完成约95%之后,向反应混合物中加入四丁基钛,缩聚反应在约200-270℃的温度下在减压下完成。 将偏磷酸或其碱金属或碱土金属盐与叔丁醇钛一起加入以控制颜色。 常用的催化剂可用于初始酯化或酯交换。 特性粘度超过0.7dl / g,黄度数小于6的聚合物。