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Process for the continuous preparation of high molecular weight polyesters and device for carrying out the method.

机译:连续制备高分子量聚酯的方法和实施该方法的装置。

摘要

Process for the continuous preparation of polyesters of high molecular weight by esterification of dicarboxylic acids and / or transesterification of dicarboxylic acid esters with diols in the presence of catalysts with formation of a prepolymer and polycondensation to polyesters of high molecular weight, wherein a1) a paste and / or a suspension of the dicarboxylic acid and the diol is prepared, maintaining a mole ratio of diol to dicarboxylic acid of 0.8 to 1.8, a temperature between 20 and 90 ° C and a pressure between 10 and 100 kPA, or a2) the dicarboxylic acid ester is melted and mixed with the diol in a mole ratio of diol to dicarboxylic acid ester of 1.2 to 1.8 with a temperature of 145 to 165 ° C, b) products a1) and / or a2) are fed continuously to a tower reactor and the reactor tower is then performed continuously, simultaneously and without disruption esterification and / or transesterification until precondensation, the following provisos: b1) products of a1) and / or a2) are subjected to a treatment at a temperature of 170-270 ° C and a pressure of 30 to 300 kPa, being added in the first step reaction a partial amount of the catalyst and eliminating in situ reaction vapors of the reaction mixture by a hydrocyclone, b2) the product of reaction step b1) is carried continuously by a tubular section and is maintained at a pressure of 100 to 1000 kPa and a temperature of 200 to 280 ° C, being added in this reaction step 0.03 to 0.3 mol of diol, b3) the product of step b2 reaction) is carried continuously through a cascade of downstream with at least two plates, which are automatically reduced pressures in the range of 20 to 100 kPa and temperatures automatically increase of 230-280 ° C, being added in the third zone of 0.02 to remain 0.2 moles of diol and a partial amount of catalyst b4) the product from reaction step b3) is subjected to further reaction in a reaction zone falling film to 1 to 10 kPa and 240 to 280 ° C, and b5 ) the reaction product water or methanol, by-products and excess diol from reaction steps b1) and b3) to b4) are removed and after purification the diol is reintroduced in the different reaction steps c1) the prepolymer obtained from b4) is continuously polycondensed in the conventional polycondensation apparatus at temperatures of 240-290 ° C and pressures of 0.02 to 0.3 kPa or c2) the obtained prepolymer is frozen, it becomes pellets and subjected a postcondensation in solid phase at temperatures between 160 and 230 ° C under conditioned inert gas.
机译:在催化剂的存在下通过二羧酸的酯化和/或二羧酸酯与二醇的酯交换连续制备高分子量的聚酯的方法,其形成预聚物并缩聚成高分子量的聚酯,其中a1)糊剂和/或制备二羧酸和二醇的悬浮液,保持二醇与二羧酸的摩尔比为0.8至1.8,温度在20至90℃之间,压力在10至100kPA之间,或a2)将二羧酸酯熔融并以二醇与二羧酸酯的摩尔比在145至165°C下以1.2至1.8的摩尔比与二醇混合,将b)产物a1)和/或a2)连续进料到塔中然后连续,同时且不中断酯化和/或酯交换反应进行反应器塔直至预缩合,以下条件如下:b1)a1)和/或a2)的产物在170-270°C的温度和30至300 kPa的压力下进行处理,在第一步反应中添加部分量的催化剂,并通过水力旋流器消除反应混合物的原位反应蒸汽, b2)反应步骤b1)的产物连续地由管段携带,并保持在100至1000 kPa的压力和200至280°C的温度,在该反应步骤中添加0.03至0.3 mol的二醇, b3)步骤b2反应的产物)连续通过至少两个塔板在下游的级联中进行输送,这些塔板在20至100 kPa范围内自动降低压力,温度自动升高230-280°C。在0.02的第三区中保留0.2摩尔的二醇和部分量的催化剂b4)将来自反应步骤b3)的产物在反应区降膜中进一步反应至1-10kPa和240-280℃,和b5)反应产物水或除去反应步骤b1)和b3)至b4)中的甲醇,副产物和过量的二醇,并在纯化后将二醇重新引入不同的反应步骤c1)中,将由b4)获得的预聚物在常规缩聚设备中连续缩聚。在240-290°C的温度和0.02至0.3 kPa或c2的压力下)将得到的预聚物冷冻,使其成为粒料,并在160-230°C的温度下于条件惰性气体下进行固相后缩合。

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