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1. 发明授权

US4313879A Process for the manufacture of very pure .epsilon.-caprolactone 失效
标题翻译：用于制造非常纯的ε-己内酯的方法
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。

2. 再颁专利

USRE30945E Process for the preparation of propylene oxide 失效
标题翻译：环氧丙烷的制备方法
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.

3. 发明授权

US4137242A Process for the preparation of propylene oxide 失效
标题翻译：环氧丙烷的制备方法
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。

4. 再颁专利

USRE31381E Process for the preparation of propylene oxide 失效
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).

5. 发明授权

US4113747A Process for the preparation of propylene oxide 失效
标题翻译：环氧丙烷的制备方法
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。

6. 发明授权

US4059619A Process for the preparation of percarboxylic acid solutions 失效
标题翻译：过羧酸溶液的制备方法
公开(公告)号：US4059619A
公开(公告)日：1977-11-22
申请号：US678828
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： C07C67/00 , C07C407/00 , C07C409/24 , C07C179/10 , C01B15/02
CPC分类号： C07C409/24 , C07C407/00 , C07C407/003
摘要： Process for continuous production of substantially anhydrous solutions of perpropionic acid in benzene. Aqueous hydrogen peroxide is first reacted with propionic acid in the presence of acid catalyst to form perpropionic acid and water (1). The perpropionic acid is extracted with benzene (5), to provide a benzene phase containing the perpropionic acid (11) and an aqueous raffinate (7). The benzene phase is subjected to an extraction with water (12) involving at least 3 stages, to remove hydrogen peroxide, and the resulting benzene extract (15) is subjected to azeotropic distillation (26) to provide the anhydrous solution (17). 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：在苯中连续生产基本无水的过丙酸溶液的方法。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和水（1）。用苯（5）萃取过丙酸，得到含有过丙酸（11）和含水萃余液（7）的苯相。苯相用至少3个阶段的水（12）进行萃取，除去过氧化氢，所得到的苯提取物（15）进行共沸蒸馏（26），得到无水溶液（17）。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）。

7. 发明授权

US4089892A Process for the preparation of percarboxylic acid solutions 失效
标题翻译：过羧酸溶液的制备方法
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）。

8. 发明授权

US4360682A Stabilizing caprolactones with dihydroxybenzenes 失效
标题翻译：用二羟基苯稳定己内酯
公开(公告)号：US4360682A
公开(公告)日：1982-11-23
申请号：US148869
申请日：1980-05-12
申请人： Herbert Klenk , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert
发明人： Herbert Klenk , Rolf Wirthwein , Helmut Waldmann , Hermann Seifert
IPC分类号： C07D313/04 , C07D315/00
CPC分类号： C07D315/00
摘要： Caprolactones such as .epsilon.-caprolactone are stabilized against discoloration with dihydroxybenzenes such as hydroquinone or compounds of the formula ##STR1## in which R.sub.1 is alkyl of 1 to 8 carbon atoms, andR.sub.2 is hydrogen or alkyl of 1 to 8 carbon atoms.Even the presence of air is not detrimental.
摘要翻译：己内酯如ε-己内酯通过二羟基苯如氢醌或其中R 1为1至8个碳原子的烷基，且R 2为氢或1至8个碳原子的烷基的式“IMAGE”的化合物稳定化。即使空气的存在也不是有害的。

9. 发明授权

US4564514A Process for the production of water-free organic hydrogen peroxide solution 失效
标题翻译：生产无水有机过氧化氢溶液的方法
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。

10. 发明授权

US4369096A Process for the purification of epoxides 失效
标题翻译：环氧化物纯化方法
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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