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公开(公告)号：US4070253A
公开(公告)日：1978-01-24
申请号：US678826
申请日：1976-04-28
IPC分类号： C07D301/14 , C07D301/32 , B01D3/10 , C07D301/02
CPC分类号： C07D301/32
摘要： Process for separating a solution, which essentially contains propylene oxide, propylene, a carboxylic acid containing 1 to 4 carbon atoms and benzene, by distillation. The solution is fed to a first distillation stage in which propylene, propylene oxide and an amount of the benzene contained in the solution such that the top product from this first distillation contains 20 to 70% by weight of benzene are distilled off over the top at a pressure of 1.0 to 2.5 bars, and in which the carboxylic acid and the remaining benzene are obtained as the sump product. The top product from the first distillation is fed to a second distillation column in which propylene and possibly present small fractions of components which boil lower than propylene oxide are distilled off over the top and a sump product which essentially consists of propylene oxide and benzene is obtained and part of this is returned as reflux to the first distillation column.
摘要翻译： 通过蒸馏分离基本上含有环氧丙烷，丙烯，含有1至4个碳原子的羧酸和苯的溶液的方法。 将溶液进料到第一蒸馏阶段，其中丙烯，环氧丙烷和溶液中所含的一定量的苯，使得来自该第一次蒸馏的顶部产物含有20至70重量％的苯在顶部蒸馏掉 压力为1.0至2.5巴，其中获得羧酸和剩余的苯作为贮槽产物。 将第一蒸馏的顶部产物进料到第二蒸馏塔，其中丙烯和可能存在的沸点低于环氧丙烷的组分的小部分在顶部蒸馏掉，得到基本上由环氧丙烷和苯组成的集水槽产品 并且其一部分作为回流返回到第一蒸馏塔。
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2.发明授权Process for isolating propylene glycol diesters in the preparation of propylene oxide 失效在制备环氧丙烷中分离丙二醇二酯的方法
公开(公告)号：US4159925A
公开(公告)日：1979-07-03
申请号：US858319
申请日：1977-12-09
IPC分类号： C07D301/12 , C07D301/14 , B01D3/14 , C07D301/02
CPC分类号： C07D301/12 , C07C67/03 , C07C67/24 , C07C67/54 , C07D301/14
摘要： Process for isolating propylene glycol diacarboxylates in the preparation of propylene oxide by reaction of propylene with a solution of percarboxylic acid in an organic solvent, the boiling point of which is lower than that of the carboxylic acid which corresponds to the percarboxylic acid used as the epoxidizing agent, and higher than that of propylene oxide, separation, by distillation, of the reaction mixture which essentially contains propylene oxide, the carboxylic acid corresponding to the percarboxylic acid used as the epoxidizing agent and one or more of the by-products propyleneglycol, propylene glycol monocarboxylate and propylene glycol dicarboxylate as well as propylene and the organic solvent, into a fraction containing propylene oxide and propylene and a fraction containing the carboxylic acid, the by-products mentioned and the organic solvent and further separation of the fractions into the individual components by distillation. The fraction containing the carboxylic acid, one or more of the by-products propylene glycol, propylene glycol monocarboxylate and propylene glycol dicarboxylate, and the organic solvent is distilled in a column at pressures of 1.5 to 6 bars and with an average residence time of 10 to 90 minutes in the sump. The organic solvent is removed as the top product and the carboxylic acid and the corresponding propylene glycol dicarboxylate is obtained as the sump product. From the sump product the propylene glycol dicarboxylate is isolated in a manner which is in itself known.
摘要翻译： 通过丙烯与过羧酸在有机溶剂中的溶液反应制备环氧丙烷中的丙二醇二羧酸盐的分离方法，其沸点低于对应于用作环氧化物的过羧酸的羧酸 试剂，高于环氧丙烷，通过蒸馏分离基本上含有环氧丙烷的反应混合物，对应于用作环氧化剂的过羧酸的羧酸和一种或多种副产物丙二醇，丙烯 乙二醇单羧酸酯和丙二醇二羧酸酯以及丙烯和有机溶剂转化成含有环氧丙烷和丙烯的馏分和含有羧酸的馏分，所述副产物和有机溶剂，并将馏分进一步分离成单独组分 通过蒸馏。 将含有羧酸，一种或多种副产物丙二醇，丙二醇单羧酸酯和丙二醇二羧酸酯和有机溶剂的级分在1.5至6巴的压力下在柱中蒸馏，并且平均停留时间为10 在水槽中90分钟。 作为顶部产物除去有机溶剂，得到羧酸和相应的丙二醇二羧酸酯作为贮槽产物。 从贮槽产品中，以本身已知的方式分离丙二醇二羧酸酯。
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公开(公告)号：US4089892A
公开(公告)日：1978-05-16
申请号：US678829
申请日：1976-04-28
申请人： Willi Hofen , Gerd Schreyer , Rolf Wirthwein , Helmut Waldmann , Gerd Siekmann
发明人： Willi Hofen , Gerd Schreyer , Rolf Wirthwein , Helmut Waldmann , Gerd Siekmann
IPC分类号： C07C67/00 , C07C407/00 , C07C409/24 , C07C179/10 , B01D3/00
CPC分类号： C07C407/00 , C07C407/003
摘要： Process for continuous production of substantially anhydrous solutions of percarboxylic acid in solvent. Aqueous hydrogen peroxide is first reacted with the corresponding carboxylic acid in the presence of acid catalyst to form percarboxylic acid and water (1). The percarboxylic acid is extracted with solvent (5), to provide a solvent phase containing the percarboxylic acid (11) and an aqueous raffinate (7). The solvent phase is subjected to distillation (12) to provide the anhydrous solution (13). In this distillation (12) the hydrogen peroxide remaining in the solvent phase produced in the extraction (5), is distilled off together with water and some solvent, and the hydrogen peroxide is recovered as an aqueous phase and recycled (14). The aqueous raffinate, which contains hydrogen peroxide, is distilled to remove water (8) and the resulting concentrate is recycled (2) for use in the reaction (1).
摘要翻译： 连续生产基本上无水的过羧酸溶剂在溶剂中的方法。 首先在酸催化剂存在下，将过氧化氢水溶液与相应的羧酸反应生成过羧酸和水（1）。 用溶剂（5）萃取过羧酸，提供含有过羧酸（11）和含水萃余液（7）的溶剂相。 对溶剂相进行蒸馏（12）以提供无水溶液（13）。 在该蒸馏（12）中，在萃取（5）中产生的溶剂相中剩余的过氧化氢与水和一些溶剂一起蒸馏出去，并将过氧化氢作为水相回收并回收（14）。 含有过氧化氢的含水萃余液被蒸馏以除去水（8），并将所得浓缩物再循环（2）用于反应（1）。
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公开(公告)号：US4369096A
公开(公告)日：1983-01-18
申请号：US179316
申请日：1980-08-18
申请人： Hermann Seifert , Helmut Waldmann , Rolf Wirthwein , Willi Hofen
发明人： Hermann Seifert , Helmut Waldmann , Rolf Wirthwein , Willi Hofen
IPC分类号： C07D301/32 , C07D303/04 , B01D3/34
CPC分类号： C07D301/32 , C07D303/04
摘要： A process has been developed for the purification of expoxides containing carbonyl compounds as impurities wherein the carbonyl compound content is up to 2% by weight of epoxide. Purification is effected by treatment with compounds containing at least one NH.sub.2 group.
摘要翻译： 已经开发了用于纯化含有作为杂质的羰基化合物的含氧化合物的方法，其中羰基化合物含量高达2重量％的环氧化物。 通过用含有至少一个NH 2基团的化合物处理来进行纯化。
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公开(公告)号：USRE30945E
公开(公告)日：1982-05-25
申请号：US121605
申请日：1980-02-14
申请人： Guter Prescher , Gerd Schreyer , Otto Weiberg , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert , Wulf Schwerdtel , Wolf Swodenk
发明人： Guter Prescher , Gerd Schreyer , Otto Weiberg , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert , Wulf Schwerdtel , Wolf Swodenk
IPC分类号： C07C409/24 , C07D301/14
CPC分类号： C07C409/24 , C07C407/00 , C07C407/003 , C07D301/14
摘要： Process for continuous production of propylene oxide (FIG. 1) from propylene and aqueous hydrogen peroxide. The aqueous hydrogen peroxide is first reacted with propionic acid in the presence of acid catalyst to form perpropionic acid (1). The perpropionic acid is taken up by extraction in benzene (5, 12), and following drying of the benzene solution (16), the perpropionic acid in the solution is reacted with propylene (18) for oxidation of the propylene to propylene oxide and conversion of the perpropionic acid back to propionic acid. The reaction mixture is worked up to separate propylene oxide, propionic acid and benzene (25, 27, 31, 33), and the latter two are recycled. In the benzene extraction (5, 12), an aqueous raffinate (7) is formed containing hydrogen peroxide and acid catalyst. Water is removed from the aqueous raffinate (8) and the concentrate is recycled to the propionic acid reactor. Make-up hydrogen peroxide can be added to the aqueous raffinate before the removal of water.
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公开(公告)号：US4313879A
公开(公告)日：1982-02-02
申请号：US179622
申请日：1980-08-20
申请人： Herbert Klenk , Rolf Wirthwein , Gerd Siekmann , Wulf Schwerdtel
发明人： Herbert Klenk , Rolf Wirthwein , Gerd Siekmann , Wulf Schwerdtel
IPC分类号： C07D313/04 , C07D315/00
CPC分类号： C07D315/00
摘要： The invention relates to a process for the production of .epsilon.-caprolactone having a purity of 99.9% and increased color and storage stability which comprises feeding .epsilon.-caprolactone, which has been made by reacting cyclohexanone with a solution of a percarboxylic acid, into a first distillation unit, operating at 0.1 to 500 mbars and drawing off as the top product a mixture consisting of .epsilon.-caprolactone and lower-boiling impurities, feeding the bottom product of said first distillation unit into a second distillation unit, operating at 0.1 to 500 mbars and then drawing off the pure .epsilon.-caprolactone as the top product. The .epsilon.-caprolactone is useful as an intermediate for the production of known useful compounds such as polyesterols which are subsequently converted to polyurethanes.
摘要翻译： 本发明涉及一种生产纯度为99.9％，颜色和储存稳定性提高的ε-己内酯的方法，包括将环己酮与过羧酸反应制得的ε-己内酯进料到第一 蒸馏单元，操作为0.1至500mbar，并作为顶部产物抽出由ε-己内酯和低沸点杂质组成的混合物，将所述第一蒸馏单元的底部产物进料到第二蒸馏单元中，操作为0.1至500mbar 然后取出纯ε-己内酯作为顶级产品。 ε-己内酯可用作生产已知有用化合物如聚酯的中间体，随后将其转化为聚氨酯。
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公开(公告)号：US4137242A
公开(公告)日：1979-01-30
申请号：US678823
申请日：1976-04-28
申请人： Gunter Prescher , Gerd Schreyer , Otto Weiberg , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert , Wulf Schwerdtel , Wolfgang Swodenk
发明人： Gunter Prescher , Gerd Schreyer , Otto Weiberg , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert , Wulf Schwerdtel , Wolfgang Swodenk
IPC分类号： C07C409/24 , C07D301/14 , C07D301/32
CPC分类号： C07D301/14 , C07C407/00 , C07C407/003
摘要： Process for continuous production of propylene oxide (FIG. 1) from propylene and aqueous hydrogen peroxide. The aqueous hydrogen peroxide is first reacted with propionic acid in the presence of acid catalyst to form perpropionic acid (1). The perpropionic acid is taken up by extraction in benzene (5, 18) and following drying of the benzene solution (21), the perpropionic acid in the solution is reacted with propylene (24) for oxidation of the propylene to propylene oxide and conversion of the perpropionic acid back to propionic acid. The reaction mixture is worked up to separate propylene oxide, propionic acid and benzene (30, 32, 37, 39), and the latter two are recycled. In the benzene extraction (5, 18), an aqueous raffinate (7) is formed containing hydrogen peroxide and acid catalyst. The aqueous raffinate can be divided into a stream which is recycled to the propionic acid reactor (1), and a second stream which can be distilled to remove water with the concentrate being recycled to the propionic acid reactor. (1)
摘要翻译： 从丙烯和过氧化氢水溶液连续生产环氧丙烷（图1）的方法。 过氧化氢水溶液首先在酸催化剂存在下与丙酸反应形成过丙酸（1）。 通过在苯（5,18）中萃取并过滤苯溶液（21），将过丙酸吸收，将溶液中的丙酸与丙烯（24）反应，将丙烯氧化成环氧丙烷，并将 过丙酸回到丙酸。 处理反应混合物以分离环氧丙烷，丙酸和苯（30,32,37,39），后两者被再循环。 在苯提取（5,18）中，形成含有过氧化氢和酸催化剂的残液水溶液（7）。 含水萃余液可以分为循环到丙酸反应器（1）的料流，以及可以将浓缩物再循环到丙酸反应器中的蒸馏水以除去水的第二料流。
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8.发明授权
公开(公告)号：US4564514A
公开(公告)日：1986-01-14
申请号：US510162
申请日：1983-07-01
申请人： Karlheinz Drauz , Axel Kleemann , Rolf Wirthwein
发明人： Karlheinz Drauz , Axel Kleemann , Rolf Wirthwein
IPC分类号： C01B15/017 , C01B15/023
CPC分类号： C01B15/017
摘要： The production of organic hydrogen peroxide solutions which are practically water-free until now has had the problem of either too high a water content of the solution or too great a loss of hydrogen peroxide through decomposition and passing over as distillate during the distillative drying. By selection of specific esters in combination with commensurately high pressures in the azeotropic removal of water, these disadvantages can be avoided. Extremely low water content solutions of hydrogen peroxide in high boiling solutions are produced by mixing hydrogen peroxide solutions in solvents whose azeotropic boiling point with water is below the boiling point of hydrogen peroxide with higher boiling solvents which form the highest azeotrope with water, whose boiling point is near or above the boiling point of hydrogen peroxide. Thereupon, the mixture is freed from both water and the lower boiling solvent. The mixture can be formed by an in situ method. Production of extremely low water containing solutions of hydrogen peroxide in high boiling solvents are produced by mixing hydrogen peroxide solutions in solvents whose azeotrope boiling point with water is below the boiling point of hydrogen peroxide with higher boiling solvents which form the highest azeotrope with water, whose boiling point is near or above the boiling point of hydrogen peroxide. Thereupon, the mixture is freed from both water and the lower boiling solvent. The above-mentioned mixture can also be produced by an in situ method.
摘要翻译： 迄今为止几乎无水的有机过氧化氢溶液的生产具有溶液中水含量过高或分解过程中过氧化氢过多或蒸馏干燥过程中作为馏出物流失的问题。 通过选择特定的酯与共沸去除水中相当高的压力相结合，可以避免这些缺点。 过氧化氢在高沸点溶液中的极低含水量溶液是通过将过氧化氢溶液与共沸点与水低于过氧化氢沸点的溶剂混合，通过与沸水形成最高共沸物的较高沸点溶剂混合而制得的，其沸点 接近或高于过氧化氢的沸点。 因此，混合物从水和低沸点溶剂中释放出来。 混合物可以通过原位法形成。 在高沸点溶剂中生产极低含水量的过氧化氢的溶液是通过将过氧化氢溶液与沸点高于沸点溶剂的沸点高于沸点的溶剂在水中沸点高于沸点的溶剂混合， 沸点接近或高于过氧化氢的沸点。 因此，混合物从水和低沸点溶剂中释放出来。 上述混合物也可以通过原位法制备。
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公开(公告)号：USRE31381E
公开(公告)日：1983-09-13
申请号：US121604
申请日：1980-02-14
申请人： Gunter Prescher , Gerd Schreyer , Otto Weiberg , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert , Wulf Schwerdtel , Wolf Swodenk
发明人： Gunter Prescher , Gerd Schreyer , Otto Weiberg , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert , Wulf Schwerdtel , Wolf Swodenk
IPC分类号： C07C409/24 , C07D301/14 , C07D301/32
CPC分类号： C07D301/14 , C07C407/00 , C07C407/003
摘要： Process for continuous production of propylene oxide (FIG. 1) from propylene and aqueous hydrogen peroxide. The aqueous hydrogen peroxide is first reacted with propionic acid in the presence of acid catalyst to form perpropionic acid (1). The perpropionic acid is taken up by extraction in benzene (5, 18) and following drying of the benzene solution (21), the perpropionic acid in the solution is reacted with propylene (24) for oxidation of the propylene to propylene oxide and conversion of the perpropionic acid back to propionic acid. The reaction mixture is worked up to separate propylene oxide, propionic acid and benzene (30, 32, 37, 39), and the latter two are recycled. In the benzene extraction (5, 18), an aqueous raffinate (7) is formed containing hydrogen peroxide and acid catalyst. The aqueous raffinate can be divided into a stream which is recycled to the propionic acid reactor (1), and a second stream which can be distilled to remove water with the concentrate being recycled to the propionic acid reactor (1).
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公开(公告)号：US4113747A
公开(公告)日：1978-09-12
申请号：US678822
申请日：1976-04-28
申请人： Gunter Prescher , Gerd Schreyer , Otto Weiberg , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert , Wulf Schwerdtel , Wolfgang Swodenk
发明人： Gunter Prescher , Gerd Schreyer , Otto Weiberg , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert , Wulf Schwerdtel , Wolfgang Swodenk
IPC分类号： C07C409/24 , C07D301/14
CPC分类号： C07C409/24 , C07C407/00 , C07C407/003 , C07D301/14
摘要： Process for continuous production of propylene oxide (FIG. 1) from propylene and aqueous hydrogen peroxide. The aqueous hydrogen peroxide is first reacted with propionic acid in the presence of acid catalyst to form perpropionic acid (1). The perpropionic acid is taken up by extraction in benzene (5 , 12), and following drying of the benzene solution (16), the perpropionic acid in the solution is reacted with propylene (18) for oxidation of the propylene to propylene oxide and conversion of the perpropionic acid back to propionic acid. The reaction mixture is worked up to separate propylene oxide, propionic acid and benzene (25, 27, 31, 33), and the latter two are recycled. In the benzene extraction (5, 12), an aqueous raffinate (7) is formed containing hydrogen peroxide and acid catalyst. Water is removed from the aqueous raffinate (8) and the concentrate is recycled to the propionic acid reactor. Make-up hydrogen peroxide can be added to the aqueous raffinate before the removal of water.
摘要翻译： 从丙烯和过氧化氢水溶液连续生产环氧丙烷（图1）的方法。 过氧化氢水溶液首先在酸催化剂存在下与丙酸反应形成过丙酸（1）。 通过在苯（5,12）中萃取，过丙酸被吸收，然后在苯溶液（16）干燥后，将溶液中的过丙酸与丙烯（18）反应，将丙烯氧化成环氧丙烷并转化 的过丙酸回到丙酸。 处理反应混合物以分离环氧丙烷，丙酸和苯（25,27,31,33），后两者被再循环。 在苯提取（5,12）中，形成含有过氧化氢和酸催化剂的残液水溶液（7）。 水从残液（8）中除去，浓缩物再循环到丙酸反应器中。 在除去水之前，可以将补充过氧化氢加入含水残液中。
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