PREPARATION OF CHLOROBENZOIC ACID
    11.
    发明专利

    公开(公告)号:JPS57167943A

    公开(公告)日:1982-10-16

    申请号:JP5244381

    申请日:1981-04-09

    Abstract: PURPOSE:To prepare the titled compound in high yield, and to elongate the life of the catalyst, by oxidizing chlorotoluene using acetic acid as a solvent, a Co compound as a catalyst, and paraldehyde, tec. as a reaction accelerator, crystal- lizing the reaction product, removing the by-products from the mother liquid, and recycling the residual liquid. CONSTITUTION:Chlorotoluene is oxidized with a gas containing molecular oxygen using acetic acid as a solvent, a Co compound (e.g. cobalt acetate, cobalt carbonate, etc.) as a catalyst and paraldehyde or acetaldehyde as a reaction accelerator. The obtained oxidation reaction liquid is cooled to crystallize and separate chlorobenzoic acid. By-produced acetic acid, water and chloroacetic acid are removed from the mother liquid, and the residual liquid is circulated to the oxidation reaction system to obtain chlorobenzoic acid. The compound can be prepared economically, in high purity. USE:Raw material of pesticides, pharmaceuticals, dyes, etc.

    PURIFICATION OF TEREPHTHALIC ACID
    12.
    发明专利

    公开(公告)号:JPS56113738A

    公开(公告)日:1981-09-07

    申请号:JP1473180

    申请日:1980-02-12

    Abstract: PURPOSE:To purify terephthalic acid to a purity required as a fiber material for direct polymerization, by subjecting an alkaline aqueous solution of crude terephthalic acid to specific three stages treatment. CONSTITUTION:An alkaline aqueous solution of terephthalic acid containing impurities which cause the lowering of the light transmission at 340nm, is oxidized by contacting with gas containing molecular oxygen at 160-270 deg.C. After the reaction, an acid is added to the solution, and the precipitated terephthalic acid is heated at 170-250 deg.C together with hydrous acetic acid to obtain purified terephthalic acid. Preferably, the oxidation process with a permanganate is inserted between the acid treatment and the precipitation with acid. By combination of these purification processes, the coloring impurities can be completely removed, the average particle diameter of the terephthalic acid is increased to >=several tens mum, and the fluidity of the ethylene glycol slurry of the terephthalic acid can be improved.

    PRODUCTION OF AROMATIC CARBOXYLIC ACID

    公开(公告)号:JPS5444630A

    公开(公告)日:1979-04-09

    申请号:JP11049977

    申请日:1977-09-16

    Abstract: PURPOSE:A benzene derivative substituted with at least one alkyl group is oxidized in liquid phase with an oxygen-containing gas in a solvent of aliphatic carboxylic acid in the presence of a specific catalyst and praldehyde to produce high-purity aromatic carboxylic acid. CONSTITUTION:The liquid phase oxidation of benzene derivative substituted with at least one alkyl group such as p-xylene with an oxygen-containing gas in conducted in the presence of a reaction accelerator such as paraldehyde and/or acetaldehyde and a combination of cobalt compound, nickel compound and alkaline earth metal compound in a solvent of aliphatic carboxylic acid such as acetic acid to produce aromatic carboxylic acid such as terephthalic acid. Each compound of the catalyst is preferably the salt of the aliphatic carboxylic acid used as the solvent. EFFECT:The catalyst activity markedly increases and the catalyst can be reused without any treatment for reactivation and the product contains reduced amounts of aldehydes and colored substances.

    PREPARATION OF SACCHARIN
    16.
    发明专利

    公开(公告)号:JPS5879985A

    公开(公告)日:1983-05-13

    申请号:JP17806081

    申请日:1981-11-06

    Abstract: PURPOSE:To obtain saccharin as a sweetening agent, medicine and intermediate for agricultural chemicals industrially advantageously, by oxidizing o-toluenesulfonamide with a gas containing molecular oxygen in place of dichromic acid in acetic acid solvent in the presence of a catalyst. CONSTITUTION:o-Toluenesulfonamide is catalytically oxidized with a gas containing molecular oxygen, e.g. air, in acetic acid solvent in an amount of preferably 2-10 times that of the o-toluenesulfonamide in the presence of a catalyst constituted of cobalt and/or manganese preferably in 0.04-2wt% total Co and Mn concentration based on the acetic acid solvent and a bromine compound, preferably cobalt bromide or manganese bromide, at 110-180 deg.C and 5-30atm. The reaction mixture is then cooled to crystallize the aimed saccharin. The mother liquor after the separation of the crystal can be repeatedly circulated through the reaction system.

    PRODUCTION OF AROMATIC CARBOXYLIC ACID

    公开(公告)号:JPS57193422A

    公开(公告)日:1982-11-27

    申请号:JP7724381

    申请日:1981-05-21

    Abstract: PURPOSE:When an aromatic compound bearing methyl groups is catalytically oxidized into the titled compound, acetic acid which contains a specific amount of water is used as a solvent and the above aromatic compound is added to the distillate mix of water and acetic acid originating from the reaction mixture, then concentration is conducted again to separate the water formed as a by- product advantageously. CONSTITUTION:An aromatic compound having at least one of methyl groups is oxidized with a gas containing molecular oxygen in the presence of a heavy metal catalyst in a solvent of acetic acid containing 5-25wt% water. Then, the distillate mix that is mainly composed of water and acetic acid orginating from the reaction mixture is combined with the aromatic compound newly fed and they are subjected to concentration to distil off almost the same amount of water as that of the water formed in the oxidation and recover the remaining containing acetic acid. The remaining is circulated to the above oxidation stage, whereby the water formed in the oxidation is separated from the acetic acid solvent without precise rectification operations and the objective aromatic carboxylic acid is produced economically.

    PREPARATION OF P-NITROBENZOIC ACID
    18.
    发明专利

    公开(公告)号:JPS57185238A

    公开(公告)日:1982-11-15

    申请号:JP6764481

    申请日:1981-05-07

    Abstract: PURPOSE:To obtain the titled compound, by reacting p-nitrotoluene with O2 gas in the presence of a specific amount of acetic acid and a Co-Mn-Br catalyst at a relatively low temperature to give a specified conversion, concentrating the reaction product solution, and circulating the concentrated solution through the reaction system. CONSTITUTION:p-Nitrotoluene is oxidized with O2 gas to give p-nitrobenzoic acid. In the process, a catalyst containing Co, Mn and Br essentially is used, and the reaction is carried out at 120-190 deg.C, preferably 140-180 deg.C, in the presence of acetic acid in an amount of 0.2-1.3wt%, preferably 0.3-0.8wt%, based on the raw material to give a conversion of the p-nitrotoluene in the range of 10-70%. The resultant reaction product solution is then concentrated before or after the separation of the formed p-nitrobenzoic acid to distill off a mixture of the formed water with the acetic acid, and the remaining solution is circulated through the reaction system. EFFECT:Economical with good yield. USE:A raw material for agricultural chemicals, medicines, dyes, resins, etc.

    PREPARATION OF P-CHLOROBENZOIC ACID

    公开(公告)号:JPS57181034A

    公开(公告)日:1982-11-08

    申请号:JP6427881

    申请日:1981-04-30

    Abstract: PURPOSE:To obtain the titled compound having high purity, with a simple fractional distillation, by oxidizing p-chlorotoluene with an O2-containing gas in the presence of a specific catalyst and a specific amount of acetic acid under the condition to attain a specific conversion, removing the by-produced water from the system, and concentrating the reaction product liquid. CONSTITUTION:p-Chlorotoluene is oxidized with an O2-containing gas using a catalyst composed mainly of Co, Mn and Br in the presence of 0.1-1.0pt.wt. of acetic acid per 1pt. of p-chlorotoluene under the condition to attain the p-chlorotoluene conversion of 20-70%. The total reaction pressure is 2-40atm and the oxygen partial pressure is selected to give the oxygen concentration in the exhaust gas from the reactor of 1-8vol%. p-Chlorobenzoic acid is isolated from the reaction mixture by removing the by-product water from the mixture before or after separating the produced solid p-chlorobenzoic acid. The residual liquid is recycled to the oxidation reaction system. USE:Raw material of pesticides, pharmaceuticals, dyes, resins, etc.

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