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A kind of preparation method of vat brown rp dye

A dye and material technology, applied in the field of vat brown RP dye preparation, can solve the problems of low cost and poor quality, and achieve the effects of good product quality, increased product yield, and reduced cost

Active Publication Date: 2016-08-17
安徽融创化工科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to: aim at the deficiencies such as low cost and poor quality in the above-mentioned prior art, and provide a reduction brown RP preparation method using a more reasonable ring structure agent and oxidation copper removal process

Method used

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  • A kind of preparation method of vat brown rp dye
  • A kind of preparation method of vat brown rp dye
  • A kind of preparation method of vat brown rp dye

Examples

Experimental program
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Effect test

Embodiment 1

[0026] 1) Condensation reaction: mix 220kg of 3,9-dibromobenzoxanthrone, 210kg of 1-aminoanthraquinone, 110kg of soda ash and 6kg of copper oxide, heat up to 260°C for 5 hours, keep warm for 6 hours, cool down naturally for 0.5 hours, and then pulverize , and at the same time lower the temperature to the internal temperature of the material at 100°C, add the material to water with a mass ratio of 19 times, boil in water at 90-100°C for 1 hour, dilute and discharge the material, filter, and dry to obtain the condensate brown RP imine with a moisture content of ≤1 %,spare.

[0027] 2) Closed-loop reaction: Add 400kg of anhydrous aluminum trichloride to the reactor, start stirring, level the material, add 150kg of pyridine, then raise the temperature to 130°C, and keep it at 130-160°C for 6 hours. After the heat preservation, cool down to 100 ℃, add brown RP imine 60Kg, control the temperature during the feeding process at 90±10℃, then raise the temperature to 120℃, and keep it a...

Embodiment 2

[0030] 1) Condensation reaction: mix 220kg of 3,9-dibromobenzoxanthrone, 220kg of 1-aminoanthraquinone, 110kg of soda ash and 6kg of copper oxide, heat up to 265°C for 5 hours, keep warm for 6 hours, cool down naturally for 0.5 hours, and then pulverize , and at the same time lower the temperature to the internal temperature of the material at 100°C, add the material to water with a mass ratio of 19 times, boil in water at 90-100°C for 1 hour, dilute and discharge the material, filter, and dry to obtain the condensate brown RP imine with a moisture content of ≤1 %,spare.

[0031] 2) Closed-loop reaction: Add 400kg of anhydrous aluminum trichloride to the reactor, start stirring, level the material, add 150kg of pyridine, then raise the temperature to 150°C, and keep it at 140-160°C for 6 hours. After the heat preservation, cool down to 100 ℃, add 80Kg of brown RP imine, control the temperature at 90±10℃ during the feeding process, then raise the temperature to 120℃, and keep i...

Embodiment 3

[0034] 1) Condensation reaction: mix 220kg of 3,9-dibromobenzoxanthrone, 230kg of 1-aminoanthraquinone, 110kg of soda ash and 6kg of copper oxide, heat up to 265°C for 6 hours, keep warm for 6 hours, cool down naturally for 0.5 hours, and then pulverize , and at the same time lower the temperature to the internal temperature of the material at 100°C, add the material to water with a mass ratio of 19 times, boil in water at 90-100°C for 1 hour, dilute and discharge the material, filter, and dry to obtain the condensate brown RP imine with a moisture content of ≤1 %,spare.

[0035] 2) Closed-loop reaction: add 400kg of anhydrous aluminum trichloride to the reactor, start stirring, level the material, add 150kg of pyridine, then raise the temperature to 140°C, and keep it at 130-160°C for 6 hours. After the heat preservation, cool down to 100 ℃, add brown RP imine 50Kg, control the temperature during the feeding process at 90±10℃, then raise the temperature to 120℃, and keep it a...

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Abstract

The invention provides a method for manufacturing vat brown RP dyestuffs. The method includes that 3,9-dibromo-benzanthrone and 1-amino-anthraquinone are subjected to condensation reaction under the effects of acid-binding agents and catalysts to generate condensate brown RP imine, then ring forming agents are added into the condensate brown RP imine, and the condensate brown RP imine and the ring forming agents are subjected to ring-closure reaction and are refined to obtain vat brown RP products. The method is characterized in that the ring forming agents for the ring-closure reaction are aluminum trichloride and pyridine, and sulfuric acid and sodium chlorate are oxidized to remove copper during refining. The method has the advantages that ring-closure reaction can be completely carried out, the product yield can be increased, the cost can be reduced, and the obtained products are high in quality; impurities such as the ring forming agents and the copper can be removed by the aid of an oxidization copper removing process, the products are high in purity, and the performance of the dyestuffs can be improved.

Description

technical field [0001] The invention belongs to the technical field of dye preparation, and relates to a preparation method of vat brown RP dye. Background technique [0002] Vat brown RP is an anthraquinone-type vat dye, also known as red brown 81. Its structural formula is as follows: [0003] [0004] Vat brown RP occupies an extremely important position in vat dyes. According to the nomenclature of dyes, it is expressed as a vat brown dye with red light. It has good level dyeing property and good affinity. It is mainly used for printing cotton fiber, viscose fiber, vinylon, etc. And dyeing, can also be used as organic pigments. [0005] The production process of reduced brown RP is as follows: the raw materials undergo condensation reaction under the action of an acid-binding agent and a catalyst to generate condensed brown RP imine, and then add a ring structure agent for ring-closing reaction to obtain a reduced brown RP product. [0006] In the preparation proces...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B5/26
Inventor 蒋大为徐卉香李进李振黄单单高鸿宇张文件
Owner 安徽融创化工科技股份有限公司
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