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    • 2. 发明授权
    • Continuous manufacture of polyamides
    • US4060517A
    • 1977-11-29
    • US559255
    • 1975-03-17
    • Friedrich MertesHelmut DoerfelEduard HeilClaus Cordes
    • Friedrich MertesHelmut DoerfelEduard HeilClaus Cordes
    • C08G69/00C08G69/04C08G69/28C08G69/36G01N30/91
    • C08G69/28C08G69/04C08G69/36G01N30/91
    • An improved process for the continuous manufacture of polyamides by continuously conveying the aqueous solution of a salt of essentially equivalent amounts of a diamine, or of a mixture of several diamines, and of a dicarboxylic acid, or of a mixture of several dicarboxylic acids, or of mixtures of such salts with lactams and/or aminocarboxylic acids, through several reaction zones under polyamide-forming conditions, wherein the mixture of starting materials is heated, in a first reaction zone, to from 200.degree. to 300.degree. C, preferably from 220.degree. to 280.degree. C, at pressures which are above the corresponding saturation vapor pressure of water and prevent the formation of a vapor phase, the pressure action on the polycondensation mixture is released in a second reaction zone and condensation of the mixture, to form high molecular weight polyamides, is then completed in further reaction stages. According to the invention,A. the mixture of starting materials is heated, in the first reaction zone, until the polycondensation conversion is at least 80% and preferably 90%,B. in the second zone the pressure acting on the polycondensation mixture is released, adiabatically, to levels of not less than 3 atmospheres, preferably not less than 5 atmospheres, and not more than 20 atmospheres, preferably not more than 15 atmospheres, so as to reach temperatures below 215.degree. C, preferably 210.degree. C,c. the polycondensation mixture is then heated in a third reaction zone, comprising a heat exchanger consisting of heat exchange elements connected in parallel, to from 220.degree. to 330.degree. C, preferably from 250.degree. to 300.degree. C, in the course of less than 5 minutes and preferably less than 1 minute, the heating being carried out preferably in the presence of the water vapor formed during the adiabatic release of the pressure (in stage b), with application of heat and evaporation of the bulk of the water, at the pressure level to which the pressure has previously been released or at a lower pressure, andD. in further reaction stages, the condensation is completed, under the conditions prevailing at the end of the third reaction zone and, finally, by conventional methods, to form high molecular weight polyamides.
    • 3. 发明授权
    • Manufacture of polylactams with initial pressures above vapor pressures
of starting materials
    • 初始压力高于原料蒸气压的聚内酰胺的制造
    • US4049638A
    • 1977-09-20
    • US609693
    • 1975-09-02
    • Helmut DoerfelClaus Cordes
    • Helmut DoerfelClaus Cordes
    • C08G69/00C08G69/04C08G69/16C08G69/24
    • C08G69/16C08G69/04
    • A process for continuous production of polyamides by continuous transport of a mixture of one or more lactams and from 1 to 15% and preferably from 3 to 8% of water and optionally other polyamide-forming compounds such as the salts of dicarboxylic acids and diamines or aminocarboxylic acids through a number of reaction zones under polyamide-forming conditions, said mixture of starting materials being heated in a first reaction zone to temperatures of from 210.degree. to 330.degree. C and preferably from 220.degree. to 280.degree. C, whereupon the polycondensation mixture is adiabatically vented in a further reaction zone and is then polymerized to completion in yet another reaction state to form high molecular weight polyamides. The process is characterized in thatA. the mixture of starting materials is heated in the first reaction zone at pressures which are above the respective vapor pressures of the starting materials and prevent the formation of a vapor phase, said heating being effected for from 5 minutes to 2 hours and preferably from 10 minutes to 1 hour until a conversion of at least 70% and preferably 80% has been reached;B. the polycondensation mixture is vented in the second zone to pressures of from 1 to 11 bars and preferably from 1 to 6 bars and is then immediately heated in a third reaction zone, preferably together with the steam formed during adiabatic venting, with the application of heat and evaporation of the major portion of the water at the said pressure obtained by venting or a lower pressure, said heating being carried out for less than 10 minutes and preferably less than 5 minutes at temperatures of from 250.degree. to 350.degree. C and preferably from 260.degree. to 280.degree. C, whereuponC. the polymerization mixture is separated from the steam in a fourth reaction zone and is polymerized to completion in a further reaction stage to form high molecular weight polyamides.
    • 通过连续输送一种或多种内酰胺和1至15%,优选3至8%的水和任选其它形成酰胺的化合物如二羧酸和二胺的盐的混合物连续输送聚酰胺的方法,或 氨基羧酸通过多个反应区在聚酰胺形成条件下,所述起始原料混合物在第一反应区中加热至210至330℃,优选220至280℃,然后缩聚混合物 在另一个反应区中绝热排出,然后在另一个反应状态下聚合完成以形成高分子量聚酰胺。 该过程的特征在于A.起始材料的混合物在第一反应区中在起动材料的相应蒸汽压力之上的压力下加热并防止形成蒸发相,加热从5分钟 至2小时,优先从10分钟至1小时,至少70%优先,80%已达到; B.多功能混合物在第二区被发布到1至11个酒吧的压力,优选从1至6个酒吧,并且在第三个反应区中立即加热,优选地与在安全性通风期间形成的蒸汽一起使用 在通过通风或低压获得的固体压力下,水的主要部分的热和蒸发,加热进行的时间不超过10分钟,优选在250℃至350℃的温度下不超过5分钟, 优选为260℃至280℃,因此C.聚合混合物在第四反应区域内与蒸汽分离,并在进一步反应阶段完成以形成高分子量聚酰胺。