PRODUCTION OF VAT DYE
    3.
    发明专利

    公开(公告)号:JPS60179462A

    公开(公告)日:1985-09-13

    申请号:JP3440584

    申请日:1984-02-27

    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.

    RECOVERY OF SOLVENT
    5.
    发明专利

    公开(公告)号:JPS5683423A

    公开(公告)日:1981-07-08

    申请号:JP15924979

    申请日:1979-12-10

    Abstract: PURPOSE:To recover a halogenated aliphatic hydrocarbon solvent, easily, in high recovery, and sufficiently high purity for recycling, preventing frothing of the solvent, from a reaction liquid obtained by the nitration of an anthraquinone compound in the presence of said solvent, by introducing the liquid into a water layer of a specific temperature, thereby immediately distilling out the solvent as the azeotropic mixture. CONSTITUTION:An anthraquinone compound is nitrated in the presence of a halogenated aliphatic hydrocarbon solvent (e.g. methylene chloride, 1,2-dichloroethane, etc.), and the solvent is recovered from the reaction products by introducing the reaction liquid into a water layer (pure water or dilute sulfuric acid) maintained at a temperature above the azeotropic point of the solvent and water, and cooling the distilled azeotropic mixture. The process has no adverse effect to the qualities and yield of the produced nitroanthraquinone compound.

    PRODUCTION OF DIANTHRAQUINONE-N, N-DIHYDROAZINE

    公开(公告)号:JPS601169A

    公开(公告)日:1985-01-07

    申请号:JP10678983

    申请日:1983-06-16

    Abstract: PURPOSE:To produce the titled substance useful as a vat dye, in high yield and quality, by condensing 1-aminoanthraquinone in the presence of 1,3-dimethyl-2- imidazolidinone using an oxidizing agent and an alkaline condensation agent. CONSTITUTION:1-Aminoanthraquinone is condensed in the presence of an oxidizing agent (e.g. air, oxygen, etc.) using 0.2-2.5 times weight, based on the raw material, of an alkaline condensation agent (preferably KOH) to obtain the titled substance. The reaction is carried out in the presence of 1.0-3.0 times weight, based on the raw material, of 1,3-dimethyl-2-imidazolidine, at 80-150 deg.C. Since 1,3-dimethyl-2-imidazolidinone is stable under alkaline condition, it can be recovered by distillation under atmospheric or reduced pressure or by solvent extraction.

    WATER-INSOLUBLE BLACK DISPERSE DYE COMPOSITION AND DYEING OF POLYESTER TYPE FIBER USING IT

    公开(公告)号:JPS57115461A

    公开(公告)日:1982-07-17

    申请号:JP30681

    申请日:1981-01-07

    Abstract: PURPOSE:The titled dye composition dyeing or printing polyester type fibers into black, having improved fastness to washing, light, sublimation, etc., especially low pollution of white area after reductive washing, obtained by blending specific three or more dyes in a specified composition ratio. CONSTITUTION:(A) 20-70wt% dye (e.g., a compound shown by the formula II) shown by the formula I(X1 and X2 are halogen; R is lower alkyl, lower alkoxy) is blended with (B) 10-40wt% dye (e.g., compound shown by the formula IV, etc.) shown by the formula III(X is halogen; Y is lower alkoxy; R1 and R2 are R), (C) 10-40wt% (e.g., a compound shown by the formula VI, etc.) shown by the formula V(Y is H, lower alkyl, or lower alkoxy), and, if necessary, (D) 0-10wt% red type dye (e.g., a compound shown by the formula VII, etc.), to give the desired dye composition.

    IMPROVED PROCESS FOR 1-NITROANTHRAQUINONE PRODUCTION

    公开(公告)号:JPS57193426A

    公开(公告)日:1982-11-27

    申请号:JP7858381

    申请日:1981-05-26

    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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