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标题翻译：用于生产FORMIC的二氧化碳与氢反应

公开(公告)号：WO2013050367A2

公开(公告)日：2013-04-11

申请号：PCT/EP2012069458

申请日：2012-10-02

申请人： BASF SE , SCHAUB THOMAS , BEY OLIVER , MEIER ANTON , FRIES DONATA MARIA , HUGO RANDOLF

发明人： SCHAUB THOMAS , BEY OLIVER , MEIER ANTON , FRIES DONATA MARIA , HUGO RANDOLF

IPC分类号： C07C51/02

CPC分类号： C07C51/02 , B01J31/0202 , B01J31/0237 , B01J31/24 , B01J31/2414 , B01J2231/625 , B01J2531/821 , B01J2531/98 , C07C51/41 , C07C51/48 , C07C53/02 , C07C53/06

摘要： The invention relates to a method for producing formic acid, comprising the following steps: (a) reacting, in a homogeneously catalyzed manner, a reaction mixture (Rg) containing carbon dioxide, hydrogen, at least one polar solvent selected from the group comprising methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl-1-propanol, and water, and at least one tertiary amine of general formula (A1) NR1R2R3, in which R1, R2, and R3 represent independently of one another an unbranched or branched, acyclic or cyclic, aliphatic, araliphatic, or aromatic group having 1 to 16 carbon atoms, wherein individual carbon atoms can also be substituted independently of one another with a hetero group selected from the groups -O- and >N- and two or all three residues can also be bonded to one another to from a chain comprising at least four atoms, in the presence of at least one coordination catalyst, which contains at least one element selected from groups 8, 9, and 10 of the periodic system, in a hydrogenation reactor in order to obtain, optionally after adding water, a two-phase hydrogenation mixture (H) containing an upper phase (O1), which contains the at least one coordination catalyst and the at least one tertiary amine (A1), and a lower phase (U1), which contains the at least one polar solvent, residues of the at least one coordination catalyst, and at least one formic acid/amine adduct of general formula (A2), NR1R2R3 * xi HCOOH, in which xi is in the range of 0.4 to 5 and R1, R2, R3 have the meanings stated above; (b) processing the hydrogenation mixture (H) obtained in step (a) according to one of the following steps: (b1) phase-separating the hydrogenation mixture (H) obtained in step (a) in a first phase-separating device into the upper phase (O1) and the lower phase (U1), or (b2) extracting the at least one coordination catalyst from the hydrogenation mixture (H) obtained in step (a) in an extraction unit with an extracting agent containing the at least one tertiary amine (A1) in order to obtain a raffinate (R1) containing the at least one formic acid/amine adduct (A2) and the at least one polar solvent and an extract (E1) containing the at least one tertiary amine (A1) and the at least one coordination catalyst, or (b3) phase-separating the hydrogenation mixture (H) obtained in step (a) in a first phase-separating device into the upper phase (O1) and the lower phase (U1) and extracting the residues of the at least one coordination catalyst from the lower phase (U1) in an extraction unit by means of an extracting agent containing the at least one tertiary amine (A1) in order to obtain a raffinate (R2) containing the at least one formic acid/amine adduct (A2) and the at least one polar solvent and an extract (E2) containing the at least one tertiary amine (A1) and the residues of the at least one coordination catalyst; (c) separating the at least one polar solvent from the lower phase (U1), from the raffinate (R1), or from the raffinate (R2) in a first distillation device in order to obtain a distillate (D1) containing the at least one polar solvent, which is fed back into the hydrogenation reactor in step (a), and a two-phase bottom mixture (S1) containing an upper phase (O2), which contains the at least one tertiary amine (A1), and a lower phase (U2), which contains the at least one formic acid/amine adduct (A2); (d) optionally processing the bottom mixture (S1) obtained in step (c) by phase separation in a second phase-separating device into the upper phase (O2) and the lower phase (U2); (e) cleaving the at least one formic acid/amine adduct (A2) contained in the bottom mixture (S1) or optionally in the lower phase (U2) in a thermal cleaving unit in order to obtain the at least one tertiary amine (A1), which is fed back to the hydrogenation reactor in step (a), and formic acid, which is discharged from the thermal cleaving unit, wherein carbon monoxide is added to the lower phase (U1), the raffinate (R1), or the raffinate (R2) directly before and/or during step (c) and/or carbon monoxide is added to the bottom mixture (S1) or optionally the bottom phase (U2) directly before and/or during step (e).

摘要翻译：本发明涉及一种用于生产甲酸的方法，包括以下步骤：（a）均匀催化的反应混合物的反应含有二氧化碳，氢气，选自甲醇，乙醇，1-丙醇组成的组中选择的至少一种极性溶剂，2（RG）丙醇，1-丁醇，2-丁醇，2-甲基-1-丙醇和水，并且所述通式（A1）NR1R2R3中的至少一种叔胺，其中R1，R2，R3彼此独立地，无支链的或支链的，无环或环状代表脂族，芳脂族或芳族基具有在每种情况下为1〜16个碳原子，其特征在于，单独的碳原子可以被选自组中选择的杂原子基团-O-和> N-取代，以及两个独立地或所有三个基团，以形成至少四个包含链原子可一起还可以连接在至少一个Komplexkatalysato的存在含选自8,9和在氢化反应器含有上层相周期表的第10选择的至少一种元素RS获得的，如果适当添加WASER后，对应于所述至少一个配位化合物催化剂的两相加氢混合物（H）（01）和包含所述至少一种极性溶剂中的至少一种叔胺（A1），和下部相（U1）中，至少一个配位化合物催化剂和通式中的至少一种甲酸 - 胺加合物（A2）的残基，NR1R2R3 * XI HCOOH， xi是在从0.4到5的范围内，R1，R2，R3具有以上给出的含义，（一）（H）根据相分离的下面（b1）的一个获得的氢化混合物（b）的后处理步骤步骤（a）获得在上部相（O1）第一相分离器氢化混合物（H）和下层相（U1）或（b2）提取从所述至少一个配合物催化剂在步骤氢化混合物（a）中获得（H）在萃取单元用含有包含至少一个甲酸 - 胺加合物（A2）和所述至少一种极性溶剂中的至少一种叔胺（A1），以获得萃余液（R1）的提取剂和含有至少一种叔胺（A1）和所述至少一个配合物催化剂或在步骤（b3）中的相分离的提取物氢化混合物（E1）（a）以在上部相（O1）的第一相分离器和下部相中获得（H）（ U1），并用含有包含至少一个甲酸 - 胺加合物的至少一种叔胺（A1），以获得萃余液（R2）萃取剂从下部相（D1）至少一种配合物催化剂在提取单元中的残基的提取（A2）和所述至少一种极性溶剂和含有至少一种叔胺（A1）和RES的提取物（E2）所述至少一个配合物催化剂的叔，（c）从所述提余液（R1）或者从在第一蒸馏装置的提余液（R2）分离下层相（U1）的所述至少一种极性溶剂，得到含有至少一种馏出物（D1）中相应的氢化反应器中在步骤（a）再循环极性溶剂，和包含含有至少一种叔胺（A1）的上层相（O 2），和下部相（U2），其是至少两相塔底混合物（S1）包含甲酸 - 胺加合物（A2），（d）任选地，在后处理步骤（c）中获得通过相分离产物塔底混合物（S1）在第二相分离器进入上部相（O 2）和下层相（U2），（e）中裂解在底部（S1）（U2）的混合物，并且如果合适，在下层相包含在热裂解单元的至少一种甲酸 - 胺加合物（A2），以获得所述至少一个叔胺（A1），其中（a）再循环到在步骤氢化反应器，以及甲酸，其从该热裂解单元放电，之前和/或期间，步骤（c）的下部相（U1）中，萃余液（R1 ）或提余液（R2），一氧化碳被添加和/或直接之前和/或期间，步骤（e）的底部混合物（S1）和，如果合适的话，下层相（U2），一氧化碳加入。

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