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    PREPARATION OF P-NITROBENZOIC ACID
    11.
    发明专利
    PREPARATION OF P-NITROBENZOIC ACID 失效

    公开(公告)号：JPS57185238A

    公开(公告)日：1982-11-15

    申请号：JP6764481

    申请日：1981-05-07

    Applicant: TORAY INDUSTRIES

    Inventor： TORIGATA HAJIME ,  NAKAOKA KENJI

    IPC: C07B61/00 ,  B01J27/00 ,  B01J27/08 ,  B01J31/00 ,  B01J31/04 ,  C07C67/00 ,  C07C201/00 ,  C07C205/59

    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
    12.
    发明专利
    PREPARATION OF P-CHLOROBENZOIC ACID 失效

    公开(公告)号：JPS57181034A

    公开(公告)日：1982-11-08

    申请号：JP6427881

    申请日：1981-04-30

    Applicant: TORAY INDUSTRIES

    Inventor： TORIGATA HAJIME ,  NAKAOKA KENJI

    IPC: C07C63/70 ,  B01J27/00 ,  B01J27/08 ,  B01J31/00 ,  B01J31/02 ,  C07B61/00 ,  C07C51/00 ,  C07C51/265 ,  C07C67/00

    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.

    PREPARATION OF HIGHHGRADE TEREPHTHALIC ACID
    13.
    发明专利
    PREPARATION OF HIGHHGRADE TEREPHTHALIC ACID 失效

    公开(公告)号：JPS5446737A

    公开(公告)日：1979-04-12

    申请号：JP11224277

    申请日：1977-09-20

    Applicant: TORAY INDUSTRIES

    Inventor： MORIMOTO HIROSHI ,  TOUDA YASOJI ,  TORIKAI HAJIME ,  NAKAOKA KENJI

    IPC: C07C63/26 ,  B01J31/00 ,  B01J31/04 ,  C07B61/00 ,  C07C51/00 ,  C07C67/00

    Abstract: PURPOSE:To obtain high-grade terephthalic acid, by liquid phase oxidation of p-xylene with O2 in the presence of a catalyst consisting of a heavy metal compound, e.g. Co, Mn, Fe, etc. and a bromine compound in a specific combination in a solvent, e.g. a lower aliphatic corboxylic acid, etc. CONSTITUTION:p-Xylene is oxidized in the liquid phase with an O2-containing gas in the presence of a catalyst consisting of a heavy metal compound and/or a bromine compound[at least a cobalt, a manganese, and an iron compounds are used as the heavy metal compound in the following amounts: Co;>=200 times the amount of the solvent, Mn: >=0.1wt% based on the amount of Co+Mn: 300- 3,000wt.ppm based on the amount of the solvent, Fe: 3-200wt.ppm based on the amount of the solvent] in a solvent, e.g. acetic acid containing an adequate amount of water, consisting mainly of a lower aliphatic carboxylic acid to give terephthalic acid. EFFECT:Terephthalic acid can be obtained at a relatively high temperature of 200- 230 deg.C in a high yield with little loss of solvent due to the decomposition.

    METHOD FOR PURIFYING O-METHYLACETOPHENONE
    18.
    发明专利
    METHOD FOR PURIFYING O-METHYLACETOPHENONE 失效

    公开(公告)号：JPS62277338A

    公开(公告)日：1987-12-02

    申请号：JP11917486

    申请日：1986-05-26

    Applicant: TORAY INDUSTRIES

    Inventor： NAKAJI KENJI ,  NAKAOKA KENJI

    IPC: C07C49/78 ,  C07C45/00 ,  C07C45/82 ,  C07C67/00

    Abstract: PURPOSE:To remove isophorone as a by-product simply and to obtain the titled compound useful as a raw material for drugs and agricultural chemicals from inexpensive raw material in high purity and in high yield, by reacting O-toluic acid with acetic acid or acetone, hydrogenating the prepared crude reaction product and distilling the hydrogenated substance. CONSTITUTION:O-Toluic acid and acetic acid or acetone as raw materials are reacted in a gaseous phase to give crude O-methylacetophenone. Then, the crude reaction product is firstly hydrogenated and then distilled to give the aimed compound. The hydrogenation treatment is carried out in the presence of 1-20wt%, preferably 5-10wt% based on the crude reaction product of a catalyst such an nickel, palladium, etc., under hydrogen pressure at normal pressure - 100atm., preferably 1-about 50atom. at room temperature - 100 deg.C, preferably 20-50 deg.C. The catalyst is removed from the crude reaction product having finished the hydrogenation treatment and the crude reaction product is distilled. The molar ratio of the O-toluic acid as the raw material to acetic acid or acetone fed is preferably 1:1-10.

    PREPARATION OF P-CYANOBENZALDEHYDE
    20.
    发明专利
    PREPARATION OF P-CYANOBENZALDEHYDE 失效

    公开(公告)号：JPS60166655A

    公开(公告)日：1985-08-29

    申请号：JP1986884

    申请日：1984-02-08

    Applicant: TORAY INDUSTRIES

    Inventor： WADA SEIKICHI ,  NAKAOKA KENJI

    IPC: C07C255/56 ,  C07C67/00 ,  C07C253/00

    Abstract: PURPOSE:To obtain the titled compound of good hue useful as a raw material for liquid crystals, etc. in high yield in one step using an inexpensive oxidizing agent, by treating p-cyanobenzyl chloride with an aqueous solution of hexamethylenetetramine in the two-layer system of oil and water. CONSTITUTION:p-Cyanobenzyl chloride is dissolved in a water-immiscible hydrophobic inert organic solvent, e.g. benzene, toluene or xylene, and reacted with an aqueous solution of hexamethylenetetramine in the two-layer system of oil and water at 60-100 deg.C to give the aimed substance. The molar amount of the hexamethylenetetramine to be used is 1-2 times that of the p-cyanobenzyl chloride, and the amount of the solvent to be used is 1-6 times that of the p- cyanobenzyl chloride. The p-cyanobenzyl chloride is obtained by reacting p-tolunitrile with chlorine in the presence of light or a radical initiator.

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