公开(公告)号：US20080167495A1

公开(公告)日：2008-07-10

申请号：US11900385

申请日：2007-09-11

申请人： Jih-Dar Hwang ,  Hsiu-Li Cheng ,  Shou-Li Luo

发明人： Jih-Dar Hwang ,  Hsiu-Li Cheng ,  Shou-Li Luo

IPC分类号： C07C249/08

CPC分类号： C01B21/1418

摘要： A recycling system for hydroxylamine formation and oximation is proposed. The recycling system includes a hydroxylamine formation zone, an oximation zone, a purification zone, and an adjusting zone having a nitrate absorption tower. An inorganic process solution, used by the recycling system, partially enters the nitrate absorption tower supplementing nitrate, followed by mixing with the residual inorganic process solution, thereby reducing the loss rate of hydroxylamine in the inorganic process solution due to degradation. In addition, the organic impurities with high boiling point in the inorganic process solution can be effectively removed in the purification zone. As a result, the reduced activity or selectivity of the catalyst for hydroxylamine formation, caused by the toxic effects of these organic impurities on the catalyst, can be avoided, and hence, a high concentration of hydroxylamine can be obtained.

摘要翻译： 提出了羟胺形成和肟化的循环系统。 回收系统包括羟胺形成区，肟化区，净化区和具有硝酸盐吸收塔的调节区。 由再循环系统使用的无机工艺溶液部分地进入补充硝酸盐的硝酸盐吸收塔，然后与剩余的无机工艺溶液混合，从而降低由于降解导致的无机工艺溶液中羟胺的损失率。 此外，可以在净化区域中有效地除去无机工艺溶液中具有高沸点的有机杂质。 结果，可以避免由这些有机杂质对催化剂的毒性作用引起的羟胺形成催化剂的活性降低或选择性降低，因此可以获得高浓度的羟胺。

公开(公告)号：US07671236B2

公开(公告)日：2010-03-02

申请号：US11986366

申请日：2007-11-20

申请人： Jih-Dar Hwang ,  Kai-Hung Haung ,  Hsiu-Li Cheng ,  Shou-Li Luo

发明人： Jih-Dar Hwang ,  Kai-Hung Haung ,  Hsiu-Li Cheng ,  Shou-Li Luo

IPC分类号： C07C249/08

CPC分类号： C07C249/08 ,  C07C2601/14 ,  C07C251/44

摘要： Provided is a process of producing cyclohexanone oxime comprising the steps of: pre-mixing an inorganic process solution containing a high concentration of hydroxylamine phosphate with a first stream of cyclohexanone such that the concentration of hydroxylamine phosphate is reduced to 80% or less of its initial concentration; and subjecting hydroxylamine phosphate in the premixed inorganic process solution to an oximation reaction with a second stream of cyclohexanone. According to the process, oximation is performed after the inorganic process solution containing a high concentration of hydroxylamine phosphate has been pre-mixed with the first stream of cyclohexanone to reduce the concentration of hydroxylamine phosphate. As a result, not only that the efficiency of oximation and the yield of cyclohexanone oxime are increased, but also the organic content of the inorganic process solution discharged from the oximation tower is reduced.

摘要翻译： 提供了制备环己酮肟的方法，包括以下步骤：将含有高浓度磷酸羟胺的无机工艺溶液与第一环己酮流预混合，使得磷酸羟胺的浓度降低至其初始浓度的80％以下 浓度; 并将预混合的无机工艺溶液中的磷酸羟胺与第二个环己酮流进行肟化反应。 根据该方法，在含有高浓度磷酸羟胺的无机处理溶液与第一环己酮流预混合后，进行肟化，以降低磷酸羟胺的浓度。 结果，不仅提高了肟化的效率和环己酮肟的收率，还降低了从肟化塔排出的无机工艺溶液的有机含量。

公开(公告)号：US20080167496A1

公开(公告)日：2008-07-10

申请号：US11986366

申请日：2007-11-20

申请人： Jih-Dar Hwang ,  Kai-Hung Haung ,  Hsiu-Li Cheng ,  Shou-Li Luo

发明人： Jih-Dar Hwang ,  Kai-Hung Haung ,  Hsiu-Li Cheng ,  Shou-Li Luo

IPC分类号： C07C249/08

CPC分类号： C07C249/08 ,  C07C2601/14 ,  C07C251/44

摘要： Provided is a process of producing cyclohexanone oxime comprising the steps of: pre-mixing an inorganic process solution containing a high concentration of hydroxylamine phosphate with a first stream of cyclohexanone such that the concentration of hydroxylamine phosphate is reduced to 80% or less of its initial concentration; and subjecting hydroxylamine phosphate in the premixed inorganic process solution to an oximation reaction with a second stream of cyclohexanone. According to the process, oximation is performed after the inorganic process solution containing a high concentration of hydroxylamine phosphate has been pre-mixed with the first stream of cyclohexanone to reduce the concentration of hydroxylamine phosphate. As a result, not only that the efficiency of oximation and the yield of cyclohexanone oxime are increased, but also the organic content of the inorganic process solution discharged from the oximation tower is reduced.

摘要翻译： 提供了制备环己酮肟的方法，包括以下步骤：将含有高浓度磷酸羟胺的无机工艺溶液与第一环己酮流预混合，使得磷酸羟胺的浓度降低至其初始浓度的80％以下 浓度; 并将预混合的无机工艺溶液中的磷酸羟胺与第二个环己酮流进行肟化反应。 根据该方法，在含有高浓度磷酸羟胺的无机处理溶液与第一环己酮流预混合后，进行肟化，以降低磷酸羟胺的浓度。 结果，不仅提高了肟化的效率和环己酮肟的收率，还降低了从肟化塔排出的无机工艺溶液的有机含量。

公开(公告)号：US06063958A

公开(公告)日：2000-05-16

申请号：US218613

申请日：1998-12-22

申请人： Kuang-Ruei Chen ,  Jih-Dar Hwang ,  Shu-Hui Chen

发明人： Kuang-Ruei Chen ,  Jih-Dar Hwang ,  Shu-Hui Chen

IPC分类号： C07C51/215 ,  C07B61/00 ,  C07C51/31 ,  C07C51/44 ,  C07C51/48 ,  C07C55/14 ,  C07C59/105 ,  C07C51/42

CPC分类号： C07C51/44 ,  C07C51/313 ,  C07C51/48

摘要： A method of recovering adipic acid and 6-hydroxycaproic acid from the waste solution of alkali metal salts of organic acids coming from the process of cyclohexane oxidation, which comprises:(i) basifying the reaction mixture coming from cyclohexane oxidation with an aqueous solution of an alkali-metal base so that the organic acids essentially comprising adipic acid and 6-hydroxycaproic acid therein, are saponified, extracting the formed alkali metal salts of organic acids from the mixture with water, then acidifying the aqueous extract comprising the alkali metal salts of organic acids to a pH value of 3 or lower with an aqueous solution of a protic inorganic acid, as a result, said aqueous extract is separated into an oily layer and an aqueous layer;(ii) extracting the organic acid from said oily layer obtained from the step (i) with an aqueous solution of a protic inorganic acid, to obtain an aqueous extract;(iii) extracting the organic acid from the aqueous layer obtained from the step (i) with an organic solvent selected from alcohols, ketones, esters or the mixtures thereof, to obtain an oily extract;(iv) extracting the organic acid from the aqueous extract obtained from the step (ii) with an organic solvent selected from alcohols, ketones, esters or mixtures thereof, to obtain an oily extract; and(v) combining and distilling the oily extracts obtained from the steps (iii) and (iv), to recover the organic acid essentially comprising adipic acid and 6-hydroxycaproic acid.

摘要翻译： 从环己烷氧化方法的有机酸的碱金属盐的废溶液中回收己二酸和6-羟基己酸的方法，该方法包括：（i）将来自环己烷氧化的反应混合物用 碱金属碱，使得其中主要含有己二酸和6-羟基己酸的有机酸被皂化，从水中与混合物中提取形成的有机酸碱金属盐，然后酸化含有机碱的碱金属盐的含水提取物 酸与酸性无机酸的水溶液的pH值为3以下，结果将所述含水提取物分离成油层和水层; （ii）用质子性无机酸的水溶液从所述步骤（i）得到的所述油层中提取有机酸，得到水提取物; （iii）使用选自醇，酮，酯或其混合物的有机溶剂从由步骤（ⅰ）获得的水层萃取有机酸，得到油状提取物; （iv）用选自醇，酮，酯或其混合物的有机溶剂从步骤（ii）获得的水提取物中萃取有机酸，得到油状提取物; 和（v）合并并蒸馏由步骤（iii）和（iv）得到的油状提取物，以回收基本上包含己二酸和6-羟基己酸的有机酸。

公开(公告)号：US07785549B2

公开(公告)日：2010-08-31

申请号：US11900385

申请日：2007-09-11

申请人： Jih-Dar Hwang ,  Hsiu-Li Cheng ,  Shou-Li Luo

发明人： Jih-Dar Hwang ,  Hsiu-Li Cheng ,  Shou-Li Luo

IPC分类号： B01J8/00 ,  B01J8/04 ,  C07C259/00

CPC分类号： C01B21/1418

摘要： A recycling system for hydroxylamine formation and oximation is proposed. The recycling system includes a hydroxylamine formation zone, an oximation zone, a purification zone, and an adjusting zone having a nitrate absorption tower. An inorganic process solution, used by the recycling system, partially enters the nitrate absorption tower supplementing nitrate, followed by mixing with the residual inorganic process solution, thereby reducing the loss rate of hydroxylamine in the inorganic process solution due to degradation. In addition, the organic impurities with high boiling point in the inorganic process solution can be effectively removed in the purification zone. As a result, the reduced activity or selectivity of the catalyst for hydroxylamine formation, caused by the toxic effects of these organic impurities on the catalyst, can be avoided, and hence, a high concentration of hydroxylamine can be obtained.

摘要翻译： 提出了羟胺形成和肟化的循环系统。 回收系统包括羟胺形成区，肟化区，净化区和具有硝酸盐吸收塔的调节区。 由再循环系统使用的无机工艺溶液部分地进入补充硝酸盐的硝酸盐吸收塔，然后与剩余的无机工艺溶液混合，从而降低由于降解导致的无机工艺溶液中羟胺的损失率。 此外，可以在净化区域中有效地除去无机工艺溶液中具有高沸点的有机杂质。 结果，可以避免由这些有机杂质对催化剂的毒性作用引起的羟胺形成催化剂的活性降低或选择性降低，因此可以获得高浓度的羟胺。