公开(公告)号：JPS5527150A

公开(公告)日：1980-02-27

申请号：JP9998778

申请日：1978-08-18

Applicant: UBE INDUSTRIES

Inventor： KUMAKAHA KIYOSHI ,  MIYAZAKI HARUHIKO ,  KUNIYASU KENJI

IPC: C07D223/02 ,  C07C45/00 ,  C07C45/51 ,  C07C49/403 ,  C07C67/00 ,  C07C253/00 ,  C07C255/19 ,  C07D201/02

Abstract: PURPOSE:To obtain 11-cyanoundecanoic acid, an intermediate for nylon 12, in high purity, by treating a thermal decomposition product of 1,1'-peroxydicyclohexylamine without effecting direct distillation under heating. CONSTITUTION:A reaction product, obtained by thermal decomposition of 1,1'- peroxydicyclohexylamine (PXA) at 300-1,000 deg.C, is treated with a mixed solvent of toluene and water, etc. and separated into an aqueous and an oil layers. epsilon- caprolactam (LC) is isolated from the aqueous layer, and ammonium salt of 11- cyanoundecanoic acid (CUA) is crystallized and isolated from the extract of the oil layer with aqueous ammonia. Cyclohexanone (ON) is isolated from the raffinate by distillation. Discoloration and impurity formation by direct heating can be prevented.

公开(公告)号：JPS55104226A

公开(公告)日：1980-08-09

申请号：JP1040679

申请日：1979-02-02

Applicant: UBE INDUSTRIES

Inventor： YAMANE HIDETO ,  KUMAKAHA KIYOSHI ,  MIYAZAKI HARUHIKO ,  KUNIYASU KENJI

IPC: C07C55/21 ,  C07C51/00 ,  C07C51/487 ,  C07C67/00

Abstract: PURPOSE:To prepare the highly pure title compound useful as a raw material of synthetic high polymers such as polyesters, by heating the crude title compound obtained by the hydrolysis of 11-cyanoundecanoic acid ammonium salt, in the presence of a specific alkali compound. CONSTITUTION:A crude 1,12-dodecanedioic acid obtained by the hydrolysis of 11-cyanoundecanoic acid ammonium slat with an alkali hydroxide, is heated at 100-150 deg.C, pref. 115-130 deg.C, in the presence of 0.01-5pts.wt. pref. 0.1-1 parts, based on 100 parts of the dioic acid, of ethylenediaminetetraacetic acid alkali salt (pref. sodium or potassium salt) to obtain the purified title product.

公开(公告)号：JPS5598145A

公开(公告)日：1980-07-25

申请号：JP226079

申请日：1979-01-16

Applicant: UBE INDUSTRIES

Inventor： YAMANE HIDETO ,  KUMAKAHA KIYOSHI ,  MIYAZAKI HARUHIKO ,  KUNIYASU KENJI

IPC: C07C227/04 ,  C07C67/00 ,  C07C227/00 ,  C07C227/06 ,  C07C227/42 ,  C07C229/08

Abstract: PURPOSE:A product containing 12-aminododecanoic acid resulting from hydrogenation of 11-cyanoundecanoic acid is crystallized using a specific aqueous solution by the temperature difference, thus producing title compound of high-purity. CONSTITUTION:11-Cyanoundecanoic acid is catalytically hydrogenated in the presence of a catalyst as Raney nickle to form a product containing 12-aminododecanoic acid. The resulting product is dissolved in an aqueous solution containing a lower aliphatic alcohol and ammonia and the solution is introduced into the first crystallizer kept at 0-30 deg.C. The crude crystals of 12-aminodedecanoic acid are separated and redissolved in a lower aliphatic alcohol and ammonia solution. The solution is intorduced in the second crystallizer kept at 30-60 deg.C and purified 12-aminododecanoic acid is separated. EFFECT:The crystallization at a high temperature helps the formation of large-size crystals to facilitate the separation. USE:The starting material of nylon 12.

公开(公告)号：JPS5587767A

公开(公告)日：1980-07-02

申请号：JP16010878

申请日：1978-12-27

Applicant: UBE INDUSTRIES

Inventor： HIROZAWA KAZUHIKO ,  KUMAKAHA KIYOSHI ,  MIYAZAKI HARUHIKO ,  KUNIYASU KENJI

IPC: C07D201/16 ,  C07C67/00 ,  C07C253/00 ,  C07C255/19 ,  C07D223/10

Abstract: PURPOSE:To recover the title compound, an intermediate for nylon 6, in high purity, by saparation of the oily layer (Ol) from the thermal decomposition product of 1,1'-peroxydicyclohexylamine, and by mixing of the aqueous layer with a water extract of Ol, followed by concentration distillation, crystallization of the mixture. CONSTITUTION:1,1'-Peroxydicyclohexylamine (PXA) is thermally decomposed with steam at 300-1000 deg.C, and epsilon-caprolactam (LC) is recovered from the product. The process comprises the following steps: (A) separation of product 1 into the aqueous layer 2 consisting mainly of 11-cyanoundecanoic acid, and the oily layer 3, (B) mixing of the extract of the layer 3 with water 4, (C) removal of water and low-boiling substances 6 from the mixture 5 to give the concentrate LC7 and distillation of the LC cut 9, and (D) crystallization and separation of the LC cut 9 from the toluene 10 to give the LC crystals 12.