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1. 发明授权

US4087459A Process for the preparation of polyamines 失效
标题翻译：制备多胺的方法
公开(公告)号：US4087459A
公开(公告)日：1978-05-02
申请号：US696662
申请日：1976-06-16
申请人： Hartmut Knofel , Gunther Ellendt
发明人： Hartmut Knofel , Gunther Ellendt
IPC分类号： C07C209/78 , C07C20060101 , C07C67/00 , C07C209/00 , C07C211/50 , C08G20060101 , C08G12/08 , C07C85/24
CPC分类号： C07C209/78
摘要： The instant invention is directed to a process for the preparation of multinuclear aromatic polyamines by the condensation of aniline with formaldehyde in the presence of water and acid catalysts, in which the completely reacted aqueous condensation mixture is extracted with a hydrophobic solvent in extraction stage (I), optionally with the addition of aniline, the resulting solvent phase is worked-up in known manner to isolate the polyamine and the aqueous phase is recycled to the beginning of the process, the improvement characterised in that before the aqueous phase is returned to the beginning of the process, it is extracted in one or more separate extractors (II) with a hydrophobic solvent which may contain aniline and/or aniline/formaldehyde condensates with an increased proportion of ortho-isomers, the resulting solvent phase or phases is or are extracted with the aqueous acid condensation mixture in one or more separate extractors (III) at any one or more points after the first condensation stage and before the main extraction stage (I), and the resulting solvent phase or phases is or are returned to extractor or extractors (II).
摘要翻译：本发明涉及通过在水和酸催化剂存在下苯胺与甲醛的缩合制备多核芳族多胺的方法，其中完全反应的水性缩合混合物在萃取阶段用疏水性溶剂萃取（I ），任选地加入苯胺，所得溶剂相以已知方式处理以分离多胺，水相再循环至该方法的开始，其改进之处在于在水相返回到在该方法开始时，它用一种或多种单独的萃取器（II）萃取，其中疏水性溶剂可以含有具有增加比例的邻位异构体的苯胺和/或苯胺/甲醛缩合物，所得溶剂相或相是在第一个之后的任何一个或多个点处，用一种或多种单独的提取器（III）中的含水酸缩合混合物萃取冷凝阶段和主萃取阶段（I）之前，所得到的溶剂相或相返回萃取器或萃取器（II）。

2. 发明授权

US4405527A 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：US4405527A
公开(公告)日：1983-09-20
申请号：US397652
申请日：1982-07-12
申请人： Gerhard Wegener , Hartmut Knofel , Gunther Ellendt , Marcel Petinaux
发明人： Gerhard Wegener , Hartmut Knofel , Gunther Ellendt , Marcel Petinaux
IPC分类号： C07C265/14 , C07C67/00 , C07C241/00 , C07C263/10 , C08G18/10 , C08G18/76 , C07C118/02
CPC分类号： C07C263/10
摘要： Polyisocyanates are prepared by reacting a polyamine solution with a phosgene solution. Excess phosgene and hydrogen chloride formed during the reaction are removed from the reaction mixture. The solvent is subsequently removed from the reaction mixture (e.g., by evaporation and condensation) and treated with a compound containing isocyanate reactive hydrogen atoms to convert any isocyanates present into urethanes and/or ureas. The thus-treated solvent may then be reused, preferably after any urethanes and/or ureas present in the solvent have been removed.
摘要翻译：聚异氰酸酯通过多胺溶液与光气溶液反应来制备。从反应混合物中除去反应过程中形成的过量光气和氯化氢。随后将溶剂从反应混合物中除去（例如通过蒸发和缩合），并用含有异氰酸酯反应性氢原子的化合物处理以将存在的任何异氰酸酯转化成氨基甲酸酯和/或脲。这样处理的溶剂可以重新使用，优选在溶剂中存在的任何氨基甲酸酯和/或脲之后已被去除。

3. 发明授权

US4093658A 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：US4093658A
公开(公告)日：1978-06-06
申请号：US645041
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 , C08G12/08 , C07C85/24
CPC分类号： C08G12/08
摘要： The instant invention is directed to a novel process for the production of aromatic polyamines. In one embodiment, the process comprises(A) condensing an aromatic amine with formaldehyde in the presence of a hydrophobic solvent and in the absence of an acid catalyst to produce a precondensate mixture containing the corresponding N,N'-disubstituted aminals,(B) removing substantially all the water from said precondensate mixture to produce a first organic phase,(C) mixing said first organic phase with an aqueous solution containing an acid catalyst thereby producing a first two-phase mixture,(D) subjecting said first two-phase mixture to a first rearrangement reaction wherein a mono-N-substituted aminal is formed and wherein a second two-phase mixture is produced,(E) separating said second two-phase mixture into a second organic phase and a first aqueous phase,(F) subjecting said first aqueous phase to at least one more rearrangement reaction thereby producing an aqueous condensation mixture containing said aromatic polyamines,(G) extracting said aqueous condensation mixture with a hydrophobic solvent to provide a solvent phase and a second aqueous phase comprising an aqueous solution containing the acid catalyst as an amine salt of said aromatic amine, and of said aromatic polyamines,(H) recovering aromatic polyamines from said solvent phase, and(I) returning said second aqueous phase to step (C).
摘要翻译：本发明涉及用于制备芳族多胺的新方法。在一个实施方案中，该方法包括（A）在疏水性溶剂的存在下和不存在酸催化剂的情况下将芳族胺与甲醛缩合以产生含有相应的N，N'-二取代的胺的预缩合物混合物，（B）从所述预缩合混合物中去除基本上所有的水以产生第一有机相，（C）将所述第一有机相与含有酸催化剂的水溶液混合，从而产生第一两相混合物，（D）使所述第一两相混合物形成第一重排反应，其中形成单-N-取代的缩醛，其中制备第二两相混合物，（E）将所述第二两相混合物分离成第二有机相和第一水相（F ）对所述第一水相进行至少一次重排反应，从而产生含有所述芳族多胺的水性缩合混合物，（G）提取所述水性缩合混合物用疏水性溶剂提供溶剂相，第二水相包含含有作为所述芳族胺的胺盐的酸催化剂和所述芳族多胺的水溶液，（H）从所述溶剂相回收芳族多胺，和（ I）将所述第二水相返回到步骤（C）。

4. 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。

5. 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。

6. 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）。

7. 发明授权

US5672737A Fractionation and purification of mixtures of aromatic polyamines and use thereof 失效
标题翻译：分离和纯化芳族多胺的混合物及其用途
公开(公告)号：US5672737A
公开(公告)日：1997-09-30
申请号：US623285
申请日：1996-03-28
申请人： Hartmut Knofel , Michael Brockelt
发明人： Hartmut Knofel , Michael Brockelt
IPC分类号： C08J3/00 , C07C209/72 , C07C209/84 , C07C209/86 , C07C211/34 , C07C211/50 , C07C263/10 , C07C265/14 , C08G18/32
CPC分类号： C07C209/86
摘要： The invention relates to a process for the fractionation and purification of mixtures of aromatic polyamines and to the use thereof.
摘要翻译：本发明涉及芳族多胺混合物的分级和纯化方法及其用途。

8. 发明授权

US4786751A Dissocyanates, diisocyanate mixtures and a process for their production 失效
标题翻译：二异氰酸酯，二异氰酸酯混合物及其生产方法
公开(公告)号：US4786751A
公开(公告)日：1988-11-22
申请号：US797072
申请日：1985-11-12
申请人： Hartmut Knofel , Michael Brockelt , Stefan Penninger , Herbert Stutz
发明人： Hartmut Knofel , Michael Brockelt , Stefan Penninger , Herbert Stutz
IPC分类号： C08G18/00 , C07C67/00 , C07C241/00 , C07C265/04 , C07C265/10 , C07C265/12 , C07C265/14 , C08G18/10 , C08G18/72 , C08G18/74 , C08G18/76 , C09D175/00 , C07C71/00
CPC分类号： C07C265/12 , C08G18/74
摘要： Diisocyanates and isomeric mixtures of diisocyanates corresponding to the formula ##STR1## in which R.sub.1, R.sub.2, R.sub.3, m and n are as defined herein are made by phosgenating diamines corresponding to the formula ##STR2## in which R.sub.1, R.sub.2, R.sub.3, m and n are as defined herein at a temperature of from -20.degree. to 250.degree. C. These diisocyanates are particularly useful as starting materials for the production of polyurethanes by the isocyanate polyaddition process.
摘要翻译： R 1，R 2，R 3，m和n如本文所定义的对应于式“IMAGE”的二异氰酸酯的二异氰酸酯和异构体混合物通过对应于式“IMAGE”的二胺光气化制备，其中R 1，R 2，R 3，m和 n在-20℃至250℃的温度下定义。这些二异氰酸酯特别可用作通过异氰酸酯加聚方法生产聚氨酯的原料。

9. 发明授权

US4720582A Diamines and a process for their production 失效
标题翻译：二胺及其生产工艺
公开(公告)号：US4720582A
公开(公告)日：1988-01-19
申请号：US523211
申请日：1983-08-15
申请人： Hartmut Knofel , Michael Brockelt , Stefan Penninger
发明人： Hartmut Knofel , Michael Brockelt , Stefan Penninger
IPC分类号： C07B61/00 , B01J23/00 , C07C67/00 , C07C209/00 , C07C209/36 , C07C209/72 , C07C211/49 , C08G18/32 , C07C87/52
CPC分类号： C08G18/3234
摘要： Diamines corresponding to the general formula ##STR1## wherein R.sup.1, R.sup.2 and R.sup.3 may be identical or different and represent hydrogen or straight- or branched-chain C.sub.1 -C.sub.12 alkyl groups, provided that two of the radicals,R.sup.1, R.sup.2 and R.sup.3, represent hydrogen, m and n each represent 0 or 1, provided that m+n=1; where m or n=0, the free valence is saturated by hydrogen, optionally in the form of isomeric mixtures, and optionally containing up to 35%, by weight, of the corresponding perhydrogenated diamines, and up to 10%, by weight, of the corresponding unhydrogenated aromatic diamines.Also, a process for preparing these diamines by catalytically-hydrogenating the corresponding aromatic diamines with 3 moles of hydrogen per mole of diamine, or catalytically-hydrogenating the corresponding dinitro compounds with 9 moles of hydrogen per mole of dinitro compound.
摘要翻译：对应于通式“IMAGE”的二胺，其中R 1，R 2和R 3可以相同或不同，表示氢或直链或支链C 1 -C 12烷基，条件是基团R 1，R 2和R 3中的两个表示氢，m和n各自表示0或1，条件是m + n = 1; 其中m或n = 0，任选地以异构混合物形式的氢饱和，并且任选地含有至多35重量％的相应的过氢化二胺，以及至多10重量％的相应的未氢化芳族二胺。另外，通过用相对于每摩尔二胺的3摩尔氢催化氢化相应的芳族二胺或每摩尔二硝基化合物以9摩尔氢催化氢化相应的二硝基化合物来制备这些二胺的方法。

10. 发明授权

US4593117A Process for the preparation of N- and O-substituted diurethanes and/or polyurethanes 失效
标题翻译：用于制备N-和O-取代的二氨基甲酸酯和/或聚氨酯的方法
公开(公告)号：US4593117A
公开(公告)日：1986-06-03
申请号：US678430
申请日：1984-12-05
申请人： Hartmut Knofel , Stefan Penninger , Gunther Hammen , Peter Heitkamper
发明人： Hartmut Knofel , Stefan Penninger , Gunther Hammen , Peter Heitkamper
IPC分类号： C07C269/04 , C07C67/00 , C07C209/00 , C07C209/62 , C07C211/44 , C07C239/00 , C07C271/12 , C07C271/24 , C07C271/26 , C07C271/28 , C07C271/44 , C08G18/70 , C07C125/073 , C07C125/077
CPC分类号： C08G18/701
摘要： Low molecular weight N- and O-substituted diurethanes and/or polyurethanes are prepared by reacting a diamine and/or polyamine containing a primary amino group with an N-aryl-0-alkyl urethane in the presence of at least one high boiling alcohol. This reaction may be carried out at a temperature of from 180.degree. to 350.degree. C. and a pressure of approximately 0.1 to 1,500 mbar. The arylamine corresponding to the N-ary-0-alkyl urethane which forms during this reaction is continuously removed from the reaction mixture.
摘要翻译：在至少一种高沸点醇的存在下，使含有伯氨基的二胺和/或多胺与N-芳基-O-烷基氨基甲酸酯反应制备低分子量N-和O-取代的二氨基甲酸酯和/或聚氨酯。该反应可以在180℃至350℃的温度和约0.1至1,500毫巴的压力下进行。对应于在该反应期间形成的N-芳基 - 烷基氨基甲酸酯的芳基胺从反应混合物中连续除去。

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