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    • 3. 发明授权
    • Continuous process for thermal splitting of carbamic acid esters
    • 氨基甲酸酯热分解的连续工艺
    • US4692550A
    • 1987-09-08
    • US485347
    • 1983-04-15
    • Theodor EngbertGunter HammenHartmut KnofelKlaus Konig
    • Theodor EngbertGunter HammenHartmut KnofelKlaus Konig
    • C07C263/04C07C27/00C07C31/02C07C31/125C07C67/00C07C241/00C07C265/00C07C265/04C07C265/12C07C118/00
    • C07C263/04
    • N-monosubstituted carbamic acid esters are thermally split on a continuous basis in a tube reactor. The carbamic acid ester which is flowed down or passed over the inner wall of a tube reactor is thermally split at a temperature of from 150.degree. to 450.degree. C. and under a pressure of from 0.001 to 20 bar into at least two fractions. One fraction is predominantly isocyanate and a second fraction is predominantly hydroxyl compound. These fractions may be separated by removing one as a gaseous fraction formed under the splitting conditions from the head of the reactor and collecting the second fraction as a liquid which accumulates at the base of the reactor. If both fractions are gaseous under the splitting conditions, they are both removed from the head of the reactor and subsequently separated by fractionating columns for example. This process is particularly advantageous in that isocyanate and hydroxyl fractions are obtained in high yield without using a solvent.
    • N-单取代氨基甲酸酯在管式反应器中以连续的方式热分解。 流过或流过管式反应器内壁的氨基甲酸酯在150℃至450℃的温度和0.001至20巴的压力下热分解成至少两个馏分。 一个部分主要是异氰酸酯,第二部分主要是羟基化合物。 这些级分可以通过除去在分离条件下从反应器的头部形成的气态馏分来分离,并将第二馏分作为积聚在反应器底部的液体进行收集。 如果两个馏分在分解条件下都是气态的,则它们都从反应器的头部移出,并随后通过分馏塔例如分离。 该方法特别有利的是在不使用溶剂的情况下以高产率获得异氰酸酯和羟基部分。
    • 4. 发明授权
    • Process for the preparation of polyisocyanates
    • 制备多异氰酸酯的方法
    • US5043471A
    • 1991-08-27
    • US519190
    • 1990-05-04
    • Gunter HammenHartmut KnofelWolfgang Friederichs
    • Gunter HammenHartmut KnofelWolfgang Friederichs
    • C07C263/04C07C263/20C07C265/14
    • C07C263/20C07C263/04
    • The present invention relates to a process for the preparation of a polyisocyanate comprising(a) thermally decomposing in a tube reactor a solution of an N-substituted carbamic acid ester corresponding to said polyisocyanate in a solvent used as decompositoin medium, wherein said solvent (i) is capable of dissolving the carbamic acid ester, (ii) is stable at the decomposition temperature and chemically inert towards the carbamic acid esters and the polyisocyanate product, (iii) can be distilled without decomposing under the conditions of decomposition of carbamic acid estes, and (iv) has at least one miscibility gap with an extracting agent used according to the extraction step (c), said solutions being carried along the internal wall of reactor;(b) separating the gaseous materials formed in the tube reactor by fractional condensation into a fraction I comprised mainly of the alcohol by-product and a fraction II comprised mainly of polyisocyanates, isocyanatourethanes, unreacted carbamic acid ester, and the solvent used in step (a);(c) extracting the polyisocyanate from said fraction II with an extracting agent that is at least partly immiscible with the decomposition medium and is a solvent for the polyisocyanate, and optionally distilling the resultant solution of the polyisocyanate in the extracting agent; and(d) recycling the portion of fraction II remaining after the polyisocyanate is extracted.
    • 本发明涉及一种制备多异氰酸酯的方法,其包含(a)在管式反应器中将在所述多异氰酸酯中的N-取代氨基甲酸酯的溶液在用作分解介质的溶剂中热分解,其中所述溶剂(i )能够溶解氨基甲酸酯,(ii)在分解温度下稳定并对氨基甲酸酯和多异氰酸酯产物具有化学惰性,(iii)可以在氨基甲酸酯分解条件下不分解而蒸馏, 和(iv)与根据提取步骤(c)使用的萃取剂具有至少一个混溶性间隙,所述溶液沿反应器内壁运送; (b)通过分级冷凝将形成在管式反应器中的气态物质分离成主要由醇副产物组成的馏分I和主要由多异氰酸酯,异氰酸酯基氨基甲酸酯,未反应的氨基甲酸酯和步骤( 一个); (c)使用与分解介质至少部分不混溶并且是多异氰酸酯的溶剂的提取剂从所述级分II中提取多异氰酸酯,并且任选地将得到的多异氰酸酯溶液蒸馏在萃取剂中; 和(d)回收在提取多异氰酸酯之后残留的馏分II的部分。
    • 5. 发明授权
    • Process for the preparation of isocyanates
    • 异氰酸酯的制备方法
    • US5925783A
    • 1999-07-20
    • US836294
    • 1997-05-12
    • Klaus JostGunter HammenRudolf Sundermann
    • Klaus JostGunter HammenRudolf Sundermann
    • C07C263/10C07C265/14C07C263/00
    • C07C263/10
    • Isocyanates are prepared by a continuous process by reacting appropriate primary amines with phosgene in the presence of an isocyanate as solvent, the primary amine optionally dissolved in an inert organic solvent being reacted with phosgene, which is dissolved in the isocyanate, at temperatures of 60 to 150.degree. C. and at pressures of 1 to 30 bar (10.sup.5 to 3.10.sup.6 Pa) to obtain the corresponding isocyanate, wherein the molar ratio of phosgene to amine used is 4:1 to 1:1, and the isocyanate used as solvent is solids-free and has a value for hydrolysable chlorine of less than 2%.
    • PCT No.PCT / EP95 / 04354 Sec。 371日期:1997年5月12日 102(e)日期1997年5月12日PCT提交1995年11月6日PCT公布。 出版物WO96 / 1602800 日期1996年5月30日异氰酸酯通过连续方法通过在异氰酸酯作为溶剂的存在下使适当的伯胺与光气反应制备,伯胺任选地溶解在惰性有机溶剂中,与溶解在异氰酸酯中的光气反应, 温度为60〜150℃,压力为1〜30巴(105〜3.106Pa),得到相应的异氰酸酯,其中光气与胺的摩尔比为4:1〜1:1,异氰酸酯 因为溶剂是无固体的,并且具有小于2%的可水解氯的值。