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1. 发明授权

US07939027B2 Process for the synthesis of DMAPA 有权
标题翻译：合成DMAPA的方法
公开(公告)号：US07939027B2
公开(公告)日：2011-05-10
申请号：US12683015
申请日：2010-01-06
申请人： Martin Ernst , Steffen Oehlenschläger , Frank Kuhnke , Karl-Heinz Roβ , Roland Deeg , Johann-Peter Melder
发明人： Martin Ernst , Steffen Oehlenschläger , Frank Kuhnke , Karl-Heinz Roβ , Roland Deeg , Johann-Peter Melder
IPC分类号： B01J10/00 , C07C209/00 , B01J35/02 , B01J19/00 , B01J8/00
CPC分类号： C07C209/48 , B01J2219/00006 , C07C253/30 , C07C211/11 , C07C255/24
摘要： The present invention relates to a process for the industrial preparation of a diamine starting from a corresponding alkenyl nitrile comprising at least one C—C double bond, which comprises the steps (a) reaction of the alkenyl nitrile with a corresponding monoamine in a first reactor so that the monoamine adds exothermically onto the at least one double bond to form an aminoalkyl nitrile, with the monoamine and water being charged initially and the alkenyl nitrile being fed in; (b) evaporation of unreacted alkenyl nitrile and monoamine to increase the concentration of the aminoalkyl nitrile product in the bottoms of the first reactor; (c) transfer of the aminoalkyl nitrile bottom product from step (b) to a second reactor; (d) batchwise catalytic hydrogenation of the aminoalkyl nitrile transferred in step (c) to the diamine in the second reactor, with each batch being obtained by initially charging a catalyst suitable for the hydrogenation of nitriles to amines and also water, the desired diamine and a base, introducing hydrogen into the second reactor and feeding in the aminoalkyl nitrile transferred in step (c); and (e) isolation of the diamine and, if appropriate, repetition of the steps (a) to (e). The invention further relates to an apparatus for preparing these diamines and the use of the apparatuses. A preferred diamine is 3-dimethylaminopropylamine (DMAPA).
摘要翻译：本发明涉及从包含至少一个C-C双键的相应链烯基腈开始工业制备二胺的方法，其包括步骤（a）在第一反应器中烯基腈与相应的单胺反应使得单胺在至少一个双键上放热添加以形成氨基烷基腈，最初加入单胺和水，并加入链烯基腈; （b）蒸发未反应的烯基腈和单胺以增加第一反应器底部氨基烷基腈产物的浓度; （c）将氨基烷基腈底部产物从步骤（b）转移至第二反应器; （d）将步骤（c）中转移的氨基烷基腈分批催化氢化为第二反应器中的二胺，每个批次通过首先将适合于将腈氢化成的催化剂加入到胺中而得到，并且还需要水，所需的二胺和碱，将氢气引入第二反应器并进料步骤（c）中转移的氨基烷基腈; 和（e）分离二胺，如果合适，重复步骤（a）至（e）。本发明还涉及一种用于制备这些二胺的装置和该装置的用途。优选的二胺是3-二甲基氨基丙胺（DMAPA）。

2. 发明授权

US07723547B2 Process for the synthesis of DMAPA 有权
标题翻译：合成DMAPA的方法
公开(公告)号：US07723547B2
公开(公告)日：2010-05-25
申请号：US12092684
申请日：2006-10-31
申请人： Martin Ernst , Steffen Oehlenschläger , Frank Kuhnke , Karl-Heinz Roβ , Ronald Deeg , Johann-Peter Melder
发明人： Martin Ernst , Steffen Oehlenschläger , Frank Kuhnke , Karl-Heinz Roβ , Ronald Deeg , Johann-Peter Melder
IPC分类号： C07C209/48
CPC分类号： B01J8/20 , B01D3/14 , B01J2219/00006 , B01J2219/00029 , B01J2219/0004 , C07C209/48 , C07C211/11
摘要： The present invention relates to a process for the industrial preparation of a diamine starting from a corresponding alkenyl nitrile comprising at least one C—C double bond, which comprises the steps (a) reaction of the alkenyl nitrile with a corresponding monoamine in a first reactor so that the monoamine adds exothermically onto the at least one double bond to form an aminoalkyl nitrile, with the monoamine and water being charged initially and the alkenyl nitrile being fed in; (b) evaporation of unreacted alkenyl nitrile and monoamine to increase the concentration of the aminoalkyl nitrile product in the bottoms of the first reactor; (c) transfer of the aminoalkyl nitrile bottom product from step (b) to a second reactor; (d) batchwise catalytic hydrogenation of the aminoalkyl nitrile transferred in step (c) to the diamine in the second reactor, with each batch being obtained by initially charging a catalyst suitable for the hydrogenation of nitriles to amines and also water, the desired diamine and a base, introducing hydrogen into the second reactor and feeding in the aminoalkyl nitrile transferred in step (c); and (e) isolation of the diamine and, if appropriate, repetition of the steps (a) to (e). The invention further relates to an apparatus for preparing these diamines and the use of the apparatuses. A preferred diamine is 3-dimethylaminopropylamine (DMAPA).
摘要翻译：本发明涉及从包含至少一个C-C双键的相应链烯基腈开始工业制备二胺的方法，其包括步骤（a）在第一反应器中烯基腈与相应的单胺反应使得单胺在至少一个双键上放热添加以形成氨基烷基腈，最初加入单胺和水，并加入链烯基腈; （b）蒸发未反应的烯基腈和单胺以增加第一反应器底部氨基烷基腈产物的浓度; （c）将氨基烷基腈底部产物从步骤（b）转移至第二反应器; （d）将步骤（c）中转移的氨基烷基腈分批催化氢化为第二反应器中的二胺，每个批次通过首先将适合于将腈氢化成的催化剂加入到胺中而得到，并且还需要水，所需的二胺和碱，将氢气引入第二反应器并进料步骤（c）中转移的氨基烷基腈; 和（e）分离二胺，如果合适，重复步骤（a）至（e）。本发明还涉及一种用于制备这些二胺的装置和该装置的用途。优选的二胺是3-二甲基氨基丙胺（DMAPA）。

3. 发明授权

US07405327B2 Method for the continuous production of an amine 失效
标题翻译：连续生产胺的方法
公开(公告)号：US07405327B2
公开(公告)日：2008-07-29
申请号：US11596292
申请日：2005-05-04
申请人： Frank Haese , Arnd Bottcher , Bernd Stein , Wolfgang Reif , Johann-Peter Melder , Karl-Heinz Roβ , Heinz Rutter , Shelue Liang , Stefan Rittinger
发明人： Frank Haese , Arnd Bottcher , Bernd Stein , Wolfgang Reif , Johann-Peter Melder , Karl-Heinz Roβ , Heinz Rutter , Shelue Liang , Stefan Rittinger
IPC分类号： C07C209/26
CPC分类号： C07C209/26 , C07C209/16 , C07C213/02 , C07D295/027 , C07D295/03 , C07D295/088 , C08G59/50 , Y02P20/582 , C07C211/06 , C07C211/08 , C07C211/35 , C07C217/08
摘要： Process for the continuous preparation of an amine by reaction of a primary or secondary alcohol, aldehyde and/or ketone with hydrogen and a nitrogen compound selected from the group consisting of ammonia, primary and secondary amines at a temperature in the range from 60 to 300° C. in the presence of a copper-containing catalyst, wherein the catalytically active composition of the catalyst prior to reduction with hydrogen comprises from 20 to 85% by weight of aluminum oxide (Al2O3), zirconium dioxide (ZrO2), titanium dioxide (TiO2) and/or silicon dioxide (SiO2), from 1 to 70% by weight of oxygen-containing compounds of copper, calculated as CuO, from 0 to 50% by weight of oxygen-containing compounds of magnesium, calculated as MgO, oxygen-containing compounds of chromium, calculated as Cr2O3, oxygen-containing compounds of zinc, calculated as ZnO, oxygen-containing compounds of barium, calculated as BaO, and/or oxygen-containing compounds of calcium, calculated as CaO, and less than 30% by weight of oxygen-containing compounds of nickel, calculated as NiO, based on the oxygen-containing compounds of copper, calculated as CuO, and the reaction is carried out isothermally in the gas phase in a tube reactor.
摘要翻译：通过伯醇或仲醇，醛和/或酮与氢和选自氨，伯胺和仲胺的氮化合物在60至300℃的温度下反应来连续制备胺的方法在含铜催化剂存在下，其中催化剂在用氢还原之前的催化活性组合物包含20至85重量％的氧化铝（Al 2 O 3 > 3），二氧化锆（ZrO 2），二氧化钛（TiO 2）和/或二氧化硅（SiO 2）），1至70重量％的以CuO计的铜的含氧化合物，0至50重量％的以MgO计的含氧化合物的镁，含氧化合物的铬，其计算为Cr 以ZnO计算的含氧化合物锌，以BaO表示的含氧化合物的钡，以BaO计算， /或以CaO计的钙的含氧化合物，以NiO计，以CuO计的含铜化合物计，小于30重量％的含氧化合物的镍，反应为在管式反应器中在气相中等温进行。

4. 发明授权

US08193390B2 Method for the production of N,N-dimethylacetamide (DMAC) 有权
标题翻译：制备N，N-二甲基乙酰胺（DMAC）的方法
公开(公告)号：US08193390B2
公开(公告)日：2012-06-05
申请号：US11720770
申请日：2005-12-03
申请人： Horst Grafmans , Steffen Maas , Alexander Weck , Heinz Rütter , Michael Schulz , Karl-Heinz Roβ
发明人： Horst Grafmans , Steffen Maas , Alexander Weck , Heinz Rütter , Michael Schulz , Karl-Heinz Roβ
IPC分类号： C07C231/02
CPC分类号： C07C231/02 , C07C233/05
摘要： A process for preparing N,N-dimethylacetamide (DMAC) by continuously reacting methyl acetate (MeOAc) with dimethylamine (DMA) in the presence of a basic catalyst, wherein MeOAc is used in the form of a methanolic solution and the continuous distillative workup is effected in such a way that methanol and any other low boilers are initially removed overhead in a column A and the bottom effluent of column A is fed to a column B in which DMAC is removed via a side draw a purity of ≧99.7% by weight.
摘要翻译：在碱性催化剂存在下，通过使乙酸甲酯（MeOAc）与二甲胺（DMA）连续反应制备N，N-二甲基乙酰胺（DMAC）的方法，其中MeOAc以甲醇溶液的形式使用，连续蒸馏处理是以甲醇和任何其他低沸点物最初在塔A中塔顶除去并且塔A的底部流出物进料到其中通过侧面抽取DMAC的柱B，其中汲取的纯度为≥99.7重量％。

5. 发明授权

US07518020B2 Method for controlling the reactor admission temperature during the production of methylamine 有权
标题翻译：在甲胺生产过程中控制反应器入口温度的方法
公开(公告)号：US07518020B2
公开(公告)日：2009-04-14
申请号：US10573185
申请日：2004-09-24
申请人： Werner Reutemann , Rolf Wambsganβ , Frank Poplow , Theodor Weber , Karl-Heinz Roβ , Manfred Julius
发明人： Werner Reutemann , Rolf Wambsganβ , Frank Poplow , Theodor Weber , Karl-Heinz Roβ , Manfred Julius
IPC分类号： C07C209/16
CPC分类号： C07C209/16 , C07C211/04
摘要： The invention relates to a process for preparing methylamines by gas-phase reaction of methanol and ammonia as starting materials at a pressure in the range from 15 to 30 bar in the presence of heterogeneous catalyst. The starting materials are vaporized in one or more heat exchangers (1, 2, 3), superheated to produce a feed gas stream and subsequently fed into a reactor (4), with the mixing of the starting materials being able to be carried out in the feed stream to one of the heat exchangers (1, 2, 3) or at any desired position in a heat exchanger (1, 2, 3). A product gas stream comprising monomethylamine, dimethylamine and trimethylamine and also reaction by-products is taken off from the reactor (4). To control the reactor inlet temperature of the starting materials to a temperature in the range from 360° C. to 370° C., all or some of the feed gas stream or the product gas stream is passed through an adjustable valve (5) in order to vary the pressure and thus the condensation temperature.
摘要翻译：本发明涉及通过甲醇和氨作为起始原料在非均相催化剂存在下在15至30巴的压力下气相反应制备甲胺的方法。起始材料在一个或多个热交换器（1,2,3）中蒸发，过热以产生进料气流，并随后进料到反应器（4）中，原料的混合能够进行到一个热交换器（1,2,3）或在热交换器（1,2,3）中的任何期望位置的进料流。从反应器（4）中取出包含一甲胺，二甲胺和三甲胺以及反应副产物的产物气流。为了将原料的反应器入口温度控制在360℃至370℃的温度范围内，所有或一些进料气流或产物气流通过可调节阀（5），其中以改变压力，从而改变冷凝温度。

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