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31. 发明授权

US4147724A Process for the preparation of polyamines 失效
标题翻译：制备多胺的方法
公开(公告)号：US4147724A
公开(公告)日：1979-04-03
申请号：US751625
申请日：1976-12-17
申请人： Hartmut Knofel , Gunther Ellendt
发明人： Hartmut Knofel , Gunther Ellendt
IPC分类号： C07C211/50 , C07C20060101 , C07C67/00 , C07C209/00 , C07C209/78 , C08G8/16 , C08G12/08 , C07C85/145
摘要： This invention relates to a new and improved process for the preparation of polyamines based on diphenylmethane by acid condensation of aromatic amines with formaldehyde followed by processing of the condensation mixture. Compared with similar processes known in the art, the process according to the invention combines the advantage of requiring less distillation for processing the reaction mixture with the advantage of a wide scope for variation of the composition of the product finally obtained, particularly with regard to its concentration of 2,4'-isomers and greatly reduced concentration of 2,2'-isomers. More particularly, the instant invention is directed to a process for the preparation of multinuclear aromatic polyamines by condensation of aromatic amines with formaldehyde in the presence of aqueous acid catalysts in a condensation reaction carried out in at least two stages, followed by neutralization of the catalyst and recovery of aromatic polyamines characterized in that free amine is removed from the condensation reaction mixture by means of a hydrophobic solvent after the first condensation stage and before the final condensation stage, and the amine thus removed is returned to the aqueous, catalyst-containing phase by returning the resulting amine-containing solvent phase to said aqueous phase before the first condensation stage.
摘要翻译：本发明涉及通过芳族胺与甲醛的酸缩合，然后加工缩合混合物制备基于二苯基甲烷的多胺的新的和改进的方法。与本领域已知的类似方法相比，根据本发明的方法结合了需要较少蒸馏以处理反应混合物的优点，其优点在于最终获得的产物组成变化的范围广泛，特别是关于其浓度为2,4'-异构体并大大降低了2,2'-异构体的浓度。更具体地说，本发明涉及一种制备多核芳族多胺的方法，该方法是在含水酸性催化剂的存在下，在至少两个阶段进行的缩合反应中，将芳族胺与甲醛缩合，然后中和催化剂芳族多胺的回收，其特征在于在第一缩合阶段之后和最后的冷凝阶段之前借助于疏水性溶剂从缩合反应混合物中除去游离胺，并且将这样除去的胺返回到含水催化剂的相通过在第一冷凝阶段之前将所得含胺溶剂相返回所述水相。

32. 发明授权

US3996283A Process for the production of polyamines 失效
标题翻译：多胺生产工艺
公开(公告)号：US3996283A
公开(公告)日：1976-12-07
申请号：US383921
申请日：1973-07-30
申请人： Hartmut Knofel
发明人： Hartmut Knofel
IPC分类号： C08G18/32 , C07C87/28
CPC分类号： C08G18/3225
摘要： An improved process for the production of multi-nuclear aromatic polyamines by condensing an aromatic amine with formaldehyde in the presence of an acid catalyst, obtaining the condensation product in an aqueous medium and then extracting the aqueous condensation mixture with a hydrophobic solvent in order to obtain a solvent phase and a separate aqueous phase. Thereafter polyamine product is recovered from the solvent phase. If desired, polyamine product can be obtained from both the solvent phase and the aqueous phase. Alternatively, the aqueous phase can be recycled to the initial condensation step, thus providing a continuous process without loss of acid catalysts.
摘要翻译：一种用于通过在酸催化剂存在下将芳族胺与甲醛缩合制备多核芳族多胺的改进方法，在水性介质中获得缩合产物，然后用疏水性溶剂萃取水性缩合混合物，以获得溶剂相和单独的水相。此后，从溶剂相回收多胺产物。如果需要，可以从溶剂相和水相中获得多胺产物。或者，水相可以循环到初始缩合步骤，从而提供连续的方法而不损失酸催化剂。

33. 发明授权

US5043471A Process for the preparation of polyisocyanates 失效
标题翻译：制备多异氰酸酯的方法
公开(公告)号：US5043471A
公开(公告)日：1991-08-27
申请号：US519190
申请日：1990-05-04
申请人： Gunter Hammen , Hartmut Knofel , Wolfgang Friederichs
发明人： Gunter Hammen , Hartmut Knofel , Wolfgang Friederichs
IPC分类号： C07C263/04 , C07C263/20 , C07C265/14
CPC分类号： C07C263/20 , C07C263/04
摘要： 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.
摘要翻译：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。

34. 发明授权

US4094907A Process for the preparation of polyamines 失效
标题翻译：制备多胺的方法
公开(公告)号：US4094907A
公开(公告)日：1978-06-13
申请号：US751626
申请日：1976-12-17
申请人： Hartmut Knofel , Gunther Ellendt
发明人： Hartmut Knofel , Gunther Ellendt
IPC分类号： C07C211/50 , C07C20060101 , C07C67/00 , C07C209/00 , C07C209/78 , C08G8/16 , C08G12/08 , C08G73/02 , C07C85/24
CPC分类号： Y02P20/584
摘要： The instant invention is directed to a process for the preparation of multinuclear aromatic polyamines by condensation of aromatic amines with formaldehyde in the presence of aqueous acid catalysts followed by neutralization of the catalyst and processing of the resulting reaction mixture in known manner, characterized in that free amine is removed from the reaction mixture leaving the last condensation stage by means of a hydrophobic solvent, optionally after partial neutralization of the catalyst but before neutralization of the total quantity of catalyst put into the process, and the amine thus removed is returned to the catalyst-containing aqueous phase by return of the resulting amine-containing solvent phase into said aqueous, catalyst-containing phase at any point before the last condensation stage.
摘要翻译：本发明涉及通过芳族胺与甲醛在含水酸催化剂的存在下缩合制备多核芳族多胺的方法，然后中和催化剂并以已知的方式处理所得反应混合物，其特征在于游离胺从反应混合物中除去，通过疏水性溶剂离开最后的冷凝阶段，任选地在部分中和催化剂之后但在中和催化剂的总量之前，将这样除去的胺返回催化剂的含水相通过在最后的冷凝阶段之前的任何点将所得的含胺溶剂相返回到含水的含催化剂的相中。

35. 发明授权

US4061678A Process for the preparation of aromatic polyamines 失效
标题翻译：芳香族多胺的制备方法
公开(公告)号：US4061678A
公开(公告)日：1977-12-06
申请号：US645042
申请日：1975-12-29
申请人： Hartmut Knofel , Gunther Ellendt
发明人： Hartmut Knofel , Gunther Ellendt
IPC分类号： C07C211/50 , C07C67/00 , C07C209/00 , C07C209/54 , C07C209/60 , C07C209/78 , C08G20060101 , C08G8/16 , C08G12/08 , C08G73/02 , C07C85/24
CPC分类号： C07C209/78 , Y02P20/582
摘要： The instant invention is directed to a novel process for the production of aromatic polyamines. The process of the invention comprisesA. condensing an aromatic amine with formaldehyde in the presence of a hydrophobic solvent and in the absence of an acid catalyst to produce a pre-condensate mixture containing the corresponding N,N'-disubstituted aminals,B. removing substantially all the water from said pre-condensate mixture to produce a first organic phase,C. extracting said first organic phase with an aqueous solution containing an acid catalyst thereby producing a second organic phase and an aqueous pre-condensate phase which contains said aminals,D. subjecting said aqueous pre-condensate phase to a rearrangement reaction thereby producing an aqueous condensation mixture containing said aromatic polyamines,E. extracting said aqueous condensation mixture with a hydrophobic solvent to provide a solvent phase and an aqueous phase which comprises an aqueous solution containing the acid catalyst as an amine salt of said aromatic amine, and said aromatic polyamines,F. recovering aromatic polyamines from said solvent phase, andG. returning said aqueous phase to step (c).In the presently preferred embodiment, the organic phase of step (c) is returned to step (a).
摘要翻译：本发明涉及用于制备芳族多胺的新方法。本发明的方法包括A.在一种疏水溶剂中存在一种具有甲醛的芳族胺和在酸性催化剂的存在下制备含有相应的N，N'-二取代胺的预混合物B.去除实质上所有的水从预先混合的混合物中产生第一有机相，C.用含有酸性催化剂的水溶液提取第一有机相，产生第二有机相和含有氨基酸的水性预凝胶相， D.将标准水凝胶预先凝结成相对于生产含有芳族聚酰胺的水性浓缩混合物的回收反应，E.用提供溶剂相的水溶性溶剂提供的水性浓缩混合物和包含含水溶液的水性相的提取反应混合物酸性催化剂作为芳香胺的胺盐，并且含有芳香族聚酰胺，F. RECOVERI 来自固体溶剂相的NG芳族聚酰胺，以及G.将所述酸性水相回到步骤（C）。

36. 发明授权

US3952042A Process for the production of polyisocyanates 失效
标题翻译：多异氰酸酯的制备方法
公开(公告)号：US3952042A
公开(公告)日：1976-04-20
申请号：US522618
申请日：1974-11-11
申请人： Hartmut Knofel
发明人： Hartmut Knofel
IPC分类号： C07C265/14 , C07C67/00 , C07C241/00 , C07C263/10 , C07C265/12 , C07C271/06 , C08G18/76 , C07C118/02 , C07C119/048
CPC分类号： C07C263/20 , C07C263/10 , C08G18/7664
摘要： A process is provided for making a mixture of diisocyanate and polyisocyanates having more than two amino groups of the diphenylmethane series which has a low content of the o-isomers wherein a mixture of aniline and a polyamine prepared by condensation of aniline and formaldehyde is condensed with formaldehyde, at least 90% of the amino groups in the mixture being protonized with an acid, and phosgenating the resulting condensation product to form corresponding polyisocyanates.
摘要翻译：提供了一种制备二苯基甲烷系列具有多于两个氨基的二异氰酸酯和多异氰酸酯的混合物的方法，所述二苯基甲烷系列具有低含量的异构体，其中通过苯胺和甲醛的缩合制备的苯胺和多胺的混合物与甲醛中，混合物中至少90％的氨基被酸质子化，并使得到的缩合产物光气化以形成相应的多异氰酸酯。

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