Preparation method of solvent red 195

Preparation method of solvent red 195

  • CN 107,501,988 B
  • Filed: 08/26/2017
  • Issued: 09/25/2020
  • Est. Priority Date: 08/26/2017
  • Status: Active Grant
First Claim
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1. A preparation method of solvent red 195 is characterized by comprising the following preparation steps:

  • (1) diazotization reactionPumping 500 parts by weight of sulfuric acid 200-containing material with the mass concentration of 95-105% into a reaction kettle, slowly adding 100 parts by weight of diazo auxiliary agent through a feeding bin while stirring, stirring for 20-120min at 40-70 ℃

    , cooling the material to 0-5 ℃

    after the material is completely dissolved, pumping 200 parts by weight of nitrosyl sulfuric acid into the diazo kettle, and reacting for 1-5 h;

    slowly putting the materials into a dilution kettle which is added with 500 plus 1000 parts of ice water for hydrolysis, and reacting for 1-5 h;

    then adding 1-5 parts of the diazonium salt ionic liquid stabilizer to obtain diazonium hydrolysate;

    (2) coupling reactionPumping 100-200 parts by weight of dilute sulfuric acid and 150 parts by weight of coupling assistant into a material preparation kettle, then pumping 100-150 parts by weight of coupling assistant, putting the diazo hydrolysate into a coupling reaction kettle, then slowly adding the coupling solution into the diazo solution, controlling the reaction temperature at 0-10 ℃

    , reacting for 4-10h, and filtering, washing and drying the materials after the reaction is finished to obtain a solvent red 195 finished product;

    the preparation method of the diazonium salt ionic liquid stabilizer comprises the following steps;

    according to parts by weight, 100 parts of 1-propylsulfonic acid-3-methylimidazole tetrafluoroborate and 0.01-0.1 part of 2, 4-bromophenyl benzoxazole are added into a reaction kettle, 0.1-0.5 part of boron sulfide tribromodimethyl complex, 0.001-0.01 part of tris (6,6,7,7,8,8, 8-heptafluoro-2, 2-dimethyl-3, 5-octanedionate) europium and 20-50 parts of oxonium tetrafluoroborate are added, and the mixture is mechanically stirred for 10-20 hours to prepare the diazonium salt ionic liquid stabilizer.

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