公开(公告)号：JPH06720B2

公开(公告)日：1994-01-05

申请号：JP11323985

申请日：1985-05-28

Applicant: MITSUI TOATSU CHEMICALS

Inventor： KANBARA YOSHIHIKO ,  ASANO SHIRO ,  ISOZAKI WATARU ,  ASAO KOICHI

IPC: C07C67/26 ,  C07C69/54

公开(公告)号：JPS6383041A

公开(公告)日：1988-04-13

申请号：JP22500286

申请日：1986-09-25

Applicant: MITSUI TOATSU CHEMICALS

Inventor： ARASHIBA NOBUMASA ,  ASANO SHIRO ,  SAKAMOTO TOSHIHIKO

IPC: B01J27/24 ,  B01J23/74 ,  B01J27/00 ,  C07B61/00 ,  C07C51/00 ,  C07C51/285 ,  C07C59/153 ,  C07C67/00

Abstract: PURPOSE:To obtain the titled compound useful as an intermediate for various chemicals such as drug modulator, cosmetic, perfume, agricultural chemical, etc., by extremely simple operation and device industrially advantageously, by oxidizing glyoxal with hydrogen peroxide in the presence of ferrous ion. CONSTITUTION:1mol glyoxal is oxidized with hydrogen peroxide as an oxidizing agent in the presence of preferably about 0.01-5mol, more preferably about 0.05-0.5mol ferrous ion such as ferrous sulfate, etc., at about 0-30 deg.C, preferably about 0-15 deg.C and glyoxylic acid is extremely simply obtained without requiring specific separating operation and treating device, etc. Oxalic acid and a small amount of formic acid are produced as by-products in this method and organic coloring components are not produced since the reaction is carried out at low temperature. Consequently a high-quality aqueous solution containing the aimed compound is simply obtained.

公开(公告)号：JPS62181245A

公开(公告)日：1987-08-08

申请号：JP2200886

申请日：1986-02-05

Applicant: MITSUI TOATSU CHEMICALS

Inventor： ASANO SHIRO ,  SEI KOHEI ,  KANBARA YOSHIHIKO

IPC: C07B61/00 ,  B01J23/00 ,  B01J23/72 ,  C07C67/00 ,  C07C231/00 ,  C07C231/06 ,  C07C233/09

Abstract: PURPOSE:In obtaining acrylamide by using a metallic copper catalyst as a suspension bed and reacting acrylonitrile with water in a liquid phase, to stop a reactor while preventing abrupt deactivation of the catalyst, by discharging the catalyst from the reactor in order to prevent polymerization which will occur immediately after the reaction. CONSTITUTION:Acrylonitrile is reacted with water in suspension of a metallic copper catalyst, the catalyst is discharged from a reactor after continuation of the reaction and the reactor is stopped to give acrylamide. In the reaction, the discharging is carried out in such a way that the amount of copper oxide of the metallic copper catalyst remaining the reactor is made

公开(公告)号：JPS6341441A

公开(公告)日：1988-02-22

申请号：JP18430186

申请日：1986-08-07

Applicant: MITSUI TOATSU CHEMICALS

Inventor： KANBARA YOSHIHIKO ,  ASANO SHIRO ,  ISOZAKI WATARU ,  ASAO KOICHI

IPC: C07C69/54 ,  C07C67/54

Abstract: PURPOSE:To prevent the polymerization of product in the production of the titled compound from (meth)acrylic acid and an alkylene oxide, by introducing a liquid monomer from the top of a vertical double-pipe or multitubular heat- exchanger, countercurrently contacting the monomer with vapor introduced from the bottom of the exchanger and collecting the condensed vapor. CONSTITUTION:(Meth)acrylic acid is made to react with an alkylene oxide and the obtained reaction liquid is distilled to obtain the objective 2- hydroxyalkyl (meth)acrylate. In the above process, a cooling condenser 14 having a structure of vertical double-pipe or multitubular heat-exchanger is used as a vertical falling film cooling condenser. Condensed liquid is supplied to the condenser from the top, flowed down along the inner wall of a heat-transfer pipe and made to countercurrently contact with monomer vapor introduced from the bottom of the condenser to effect quick condensation of the vapor and cooling of the condensed liquid. The titled compound is obtained as the condensate. EFFECT:Superheated vapor sufficiently effective in preventing the polymerization can be condensed and collected to enable smooth continuous distillation operation.

公开(公告)号：JPS6341440A

公开(公告)日：1988-02-22

申请号：JP18430086

申请日：1986-08-07

Applicant: MITSUI TOATSU CHEMICALS

Inventor： KANBARA YOSHIHIKO ,  ASANO SHIRO ,  ISOZAKI WATARU ,  ASAO KOICHI

IPC: C07C69/54 ,  C07C67/54

Abstract: PURPOSE:To prevent the polymerization of product in the production of the titled compound, by reacting (meth)acrylic acid with an alkylene oxide using a reactor and/or distillation apparatus made of stainless steel and preparatorily treated its inner wall surface with nitric acid. CONSTITUTION:The inner wall surface of a reactor and/or a distillation apparatus made of stainless steel is made to contact with nitric acid. Acrylic acid or methacrylic acid is reacted with an alkylene oxide using the treated reactor and the obtained reaction liquid is distilled with the distillation apparatus to obtain 2-hydroxyalkyl acrylate or 2-hydroxyalkyl methacrylate. The polymerization of the product in the synthetic reaction and distillation steps can be prevented by the use of the treated apparatus. EFFECT:The objective compound can be smoothly produced on commercial base.

公开(公告)号：JPS61271248A

公开(公告)日：1986-12-01

申请号：JP11323985

申请日：1985-05-28

Applicant: MITSUI TOATSU CHEMICALS

Inventor： KANBARA YOSHIHIKO ,  ASANO SHIRO ,  ISOZAKI WATARU ,  ASAO KOICHI

IPC: C07C67/26 ,  C07C69/54

Abstract: PURPOSE:To obtain the titled compound while preventing a synthesis solution which is repeatedly synthesized by batch method, by treating a reaction zone with oxygen in the intervals of batch reactions, and reacting (meth)acrylic acid with an alkylene oxide in the presence of a catalyst by a batch method. CONSTITUTION:(Meth)acrylic acid is reacted with an alkylene oxide in the presence of a catalyst such as chromic chloride, etc., and, if necessary, a polymerization inhibitor such as phenothiazine, etc. at 20-70 deg.C for 5min-10hr in a batch method to give a 2-hydroxyalkyl (meth)acrylate, the reaction product is exhausted after the reaction is over. Before the following reaction is carried out, the reaction zone of the reactor is treated with O2 or an O2-containing gas, and just before or after (meth)acrylic acid, etc. are fed to the reactor, atmosphere in the container is replaced with an inert gas such as N2 gas, etc. to avoid danger of explosion in the reactor, the alkylene oxide is fed to it and the reaction is started. EFFECT:The polymerization of synthesis solution can be prevented simply almost without dropping production efficiency.