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    PRODUCTION OF VAT DYE
    11.
    发明专利
    PRODUCTION OF VAT DYE 失效

    公开(公告)号：JPS60179462A

    公开(公告)日：1985-09-13

    申请号：JP3440584

    申请日：1984-02-27

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KATOU KIMITOSHI ,  AIGA HIROSHI ,  MIKOTA TAMIO ,  SAKAI TSUNEHIRO

    IPC: C09B17/00 ,  C09B5/48 ,  C09B5/58 ,  C09B9/02 ,  C09B67/28

    Abstract: PURPOSE:To obtain a vat dye of good quality in a high yield, by chlorinating a specified condensation product obtd. by a reaction in the presence of 1,3-dimethyl-2-imidazolidinone. CONSTITUTION:0.1-10pts.wt. alkaline condensing agent such as KOH and optionally a wetting agent such as an alkali metal naphthalenesulfonate are added to one pt. 1-aminoanthraquinone in the form of a powder or a slurry while introducing an oxidizing agent such as air. A condensation reaction is conducted in the presence of 0.1-10pts.wt. 1,3-dimethyl-2-imidazolidinone at 80-150 deg.C to obtain a condensation reaction product. The product is slurried in water and reduced with hydrotalcite in the presence of an alkali metal hydroxide. The resulting crystal is recovered by filtration and slurried in water. The resulting dianthraquinone-N,N-dihydroamine or the above product is chlorinated in sulfuric acid. The product is recovered by filtration and the filter cake is completely dissolved in 98% sulfuric acid and reduced with Al powder to obtain a vat dye of the formula, wherein n is 1, 2.

    PRECIPITATION OF ANTHRAQUINONE
    13.
    发明专利
    PRECIPITATION OF ANTHRAQUINONE 失效

    公开(公告)号：JPS5675449A

    公开(公告)日：1981-06-22

    申请号：JP15058779

    申请日：1979-11-22

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： SAKAI TSUNEHIRO ,  YOSHIURA KOUICHI ,  FUJII SHIROU

    IPC: C07C46/10 ,  C07C45/00 ,  C07C50/18 ,  C07C67/00 ,  C07C201/00 ,  C07C205/47

    Abstract: PURPOSE:To prepare a slurry of anthraquinone fine crystals in sulfuric acid, by dissolving anthraquinone in concentrated sulfuric acid with heating, and adjusting the concentration of sulfuric acid first by adding sulfuric acid of specific concentration, and if necessary adding dilute sulfuric acid or water to the solution. CONSTITUTION:Anthraquinone is dissolved completely in concentrated sulfuric acid (>=95%) by heating at 60-150 deg.C. The objective slurry of anthraquinone fine crystals in sulfuric acid can be obtained by adding first a sulfuric acid of 50-80% concentration to the solution at 50-120 deg.C to reduce the concentration of the sulfuric acid, and if necessary, adding a dilute sulfuric acid or water to the mixture at 50- 120 deg.C to adjust the concentration of the sulfuric acid to 95-70%. The anthraquinone may have a substituent group such as halogen, OH, alkyl, allyloxy, acylamino, etc. EFFECT:The use of the above fine crystalline slurry enables the smooth nitrification of anthraquinone.

    IMPROVED PROCESS FOR 1-NITROANTHRAQUINONE PRODUCTION
    19.
    发明专利
    IMPROVED PROCESS FOR 1-NITROANTHRAQUINONE PRODUCTION 失效

    公开(公告)号：JPS57193426A

    公开(公告)日：1982-11-27

    申请号：JP7858381

    申请日：1981-05-26

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KATOU KIMITOSHI ,  SAKAI TSUNEHIRO ,  KURODA SHIZUO ,  SHIMAZOE KIKUO ,  YOSHIURA KOUICHI

    IPC: C07B61/00 ,  B01J31/00 ,  B01J31/02 ,  C07C67/00 ,  C07C201/00 ,  C07C201/10 ,  C07C205/47

    Abstract: PURPOSE:When anthraquinone is nitrated in the presence of a halogenated aliphatic hydrocarbon to produce the titled compound, a small amount of anthrone is made to coexist to make the particle size of the product uniform, thus facilitating the purification and separation and increasing the yield. CONSTITUTION:Anthraquinone is nitrated with a mixed acid in the presence of a halogenated aliphatic hydrocarbon such as methylene chloride, using high-concentration sulfuric acid, preferably of 80-95%, in an amount of 1.5-7.0, preferably 2.0-4.0 times the weight of the anthraquinone, and anthrone in an amount of 0.002-0.05, preferably 0.004-0.02pt. per 1pt. of the antraquinone to given 1-nitroanthraquinone. The reaction temperature is 0-60, preferably 10- 45 deg.C. An example of the halogenated aliphatic hydrocarbon is methylene chloride or 1,2-dichloroethane.

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