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公开(公告)号：JPS57203032A
公开(公告)日：1982-12-13
申请号：JP8570581
申请日：1981-06-05
Applicant: TORAY INDUSTRIES
Inventor： NAKAOKA KENJI , HASEGAWA SAKIE
Abstract: PURPOSE:To prepare the titled substance useful as a raw material of polymers such as polyester, etc., or an intermediate of dyes, in high yield, in a form separable easily from the byproducts, by using dicyclohexyl naphthalene derived economically from naphthalene as the raw material, and oxidizing the raw material. CONSTITUTION:The objective compound is prepared by contacting dicyclohexyl naphthalene with O2-containing gas in the presence of an oxidation catalyst, preferably in acetic acid solvent. The amount of the acetic acid used as the solvent is >=3 times, preferably >=10 times weight of dicyclohexyl naphthalene. The oxidation catalyst is composed of cobalt and/or manganese and bromine. The reaction temperature is preferably 100-250 deg.C, especially 110-140 deg.C. The dicyclohexyl naphthalene used as the raw material can be synthesized by reacting naphthalene with a cyclohexylation agent such as a halogenated cyclohexane, etc., in a solvent such as carbon disulfide, in the presence of a Friedel-Crafts catalyst.
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公开(公告)号：JPS57175143A
公开(公告)日：1982-10-28
申请号：JP5978381
申请日：1981-04-22
Applicant: TORAY INDUSTRIES
Inventor： TORIGATA HAJIME , NAKAOKA KENJI
Abstract: PURPOSE:To obtain the titled compound at a high reaction rate in a high conversion with the inhibited formation of a tarry substance as a by-product, by oxidizing chlorotoluene with a gas containing molecular oxygen in the presence of a reaction product and a catalyst containing Co, Mn and Br without using a solvent. CONSTITUTION:o-or m-Chlorotoluene is oxidixed with a gas containing molecular oxygen to prepare the corresponding chlorobenzoic acid. In the process, a catalytic system containing Co, Mn and Br essentially is used, and chlorobenzoic acid which is the aimed product in an amount of 20wt% or more based on the raw material chlorotoluene is present in the reaction system to carry out the reaction at 120-200 deg.C, preferably 130-180 deg.C. Preferably the amounts of the Co, Mn and Br are as follows: 0.02-0.7wt%, expressed in terms of Co metal, based on the chlorotoluene, Co compound, 2-20wt%, expressed in terms of Mn metal, based on the Co metal, Mn compound and a Br compound in an amount of 2-5 times that of Co metal expressed in terms of Br atom.
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公开(公告)号：JPS57167943A
公开(公告)日：1982-10-16
申请号：JP5244381
申请日：1981-04-09
Applicant: TORAY INDUSTRIES
Inventor： TORIGATA HAJIME , NAKAOKA KENJI
IPC: C07C63/70 , B01J23/00 , B01J23/74 , B01J31/00 , B01J31/04 , C07B61/00 , C07C51/00 , C07C51/265 , C07C67/00
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.
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Patent Agency Ranking
公开(公告)号：JPS56113738A
公开(公告)日：1981-09-07
申请号：JP1473180
申请日：1980-02-12
Applicant: TORAY INDUSTRIES
Inventor： TORIGATA HAJIME , NAKAOKA KENJI , SUEMATSU MASAAKI
IPC: C07C63/26 , C07C51/00 , C07C51/487 , C07C67/00
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.
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公开(公告)号：JPS55153738A
公开(公告)日：1980-11-29
申请号：JP6152579
申请日：1979-05-21
Applicant: TORAY INDUSTRIES
Inventor： NAKAOKA KENJI , MIYAZAKI KEN
Abstract: PURPOSE:To prepare high purity terephthalic acid by oxidizing p-xylene with air in liquid phase at a relatively low temperature using a reaction promotor, e.g. paraldehyde etc., heat-treating the reaction product at a specific temperature, and substituting the liquid layer with a new solvent using a counter current washing tower. CONSTITUTION:p-Xylene is oxidized in liquid phase in acetic acid at 110-140 deg.C in the presence of a Co compound catalyst and paraldehyde and/or acetaldehyde as a reaction promotor. The obtained slurry of the oxidized product is heat treated at 170-250 deg.C and then introduced into a washing tower. The slurry is washed counter-currently with acetic acid supplied from the bottom of the tower. The precipitated particles of terephthalic acid are taken out from the tower. EFFECT:Terephthalic aicd thus obtained are consisted of fine particles with large specific surface area. The diameter of the particles remarkably increases by the heat-treatment.
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公开(公告)号：JPS5444630A
公开(公告)日：1979-04-09
申请号：JP11049977
申请日：1977-09-16
Applicant: TORAY INDUSTRIES
Inventor： TORIGATA HAJIME , NAKAOKA KENJI
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.
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公开(公告)号：JPS5371026A
公开(公告)日：1978-06-24
申请号：JP14468876
申请日：1976-12-03
Applicant: TORAY INDUSTRIES
Inventor： UCHIYAMA TAKESHI , TANIGUCHI SUSUMU , NOGUCHI YOSHIO , NAKAOKA KENJI
Abstract: PURPOSE:To prepare the title acid by washing crude terephthalic acid, obtd. by oxidation of p-xylene with air in acetic acid as a solvent at 120-200 deg.C in a reactor whose internal surface material is specific stainless steel.
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公开(公告)号：JPS5334739A
公开(公告)日：1978-03-31
申请号：JP10785776
申请日：1976-09-10
Applicant: TORAY INDUSTRIES
Inventor： TORIGATA HAJIME , SUEMATSU MASAAKI , NAKAOKA KENJI
Abstract: PURPOSE:In a continuous process for producing terephthalic acid, useful as raw material for polyesters, by oxidation of p-xylene with oxygen in liquid phase in the presence of a cobalt catalyst and an accelerator of aldehyde series, higher product purity can be maintained by recycling the oxidation mother liquor which is previously dehydrated and specifically treated.
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