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Method for preparing vat brilliant red RB

A technology of brilliant red and perylenetetraic acid dianhydride is applied in the field of preparation of reduced brilliant red RB, which can solve the problems of long reaction time, high production cost, and high toxicity of solvents, etc.

Inactive Publication Date: 2012-05-16
上海华元实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The fatal shortcoming of the above process is that the solvent is highly toxic, pollutes seriously, and is harmful to the human body.
And the solvent recovery is cumbersome, the reaction time is long, and the production cost is high

Method used

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  • Method for preparing vat brilliant red RB
  • Method for preparing vat brilliant red RB

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Preparation of Vat Red RB, namely N,N'-bis(p-chlorophenyl)-3,4,9,10-perylenetetracarboximide (C.I. Vat Red 32)

[0022] 62.6 g (0.16 mol) of 3,4,9,10-perylenetetraacid dianhydride was added to 1200 g of 6% by weight KOH aqueous solution, and the temperature was raised to 90° C. to completely dissolve it. Cool to 50°C, add dropwise 65g of 98% by weight H 2 SO 4 The solution was stirred evenly (PH=5-6), filtered and washed. The perylenetetracarboxylic acid filter cake was mixed with water, and the total amount was adjusted to 724g. Add 51.1g of p-chloroaniline (0.401mol) and 28.4g of pyridine (0.360mol), mix evenly, transfer the material to an autoclave, seal it, heat up to 145-150°C (0.3-0.4MPa), keep stirring for 4h, Sampling and testing, if the perylenetetraic dianhydride in the reactant is exhausted, the reaction is over, cooled to room temperature, and filtered. Wash with hot water until there is no green fluorescence, and obtain the crude product filter cake of ...

Embodiment 2

[0024] 62.6 g (0.16 mol) of 3,4,9,10-perylenetetraacid dianhydride was added to 1200 g of 6% by weight KOH solution, and the temperature was raised to 90° C. to completely dissolve it. Cool to 50°C, add dropwise 65g of 98% by weight H 2 SO 4 The solution was stirred evenly (PH=5-6), filtered and washed. The perylenetetracarboxylic acid filter cake was mixed with water, and the total amount was adjusted to 724g. Add 51.1g of p-chloroaniline (0.401mol) and 28.4g of pyridine (0.360mol), mix evenly, transfer the material to an autoclave, seal it, heat up to 135-140°C (0.2-0.3mPa), keep stirring for 4h, Sampling and testing, if the perylenetetraic dianhydride in the reactant is exhausted, the reaction is over, cooled to room temperature, and filtered. Wash with hot water until there is no green fluorescence, and obtain the crude product filter cake of reduced brilliant red RB. The filter cake is beaten with water, and 10% by weight of sodium hypochlorite solution is added to ad...

Embodiment 3

[0026] 62.6 g (0.16 mol) of 3,4,9,10-perylenetetraacid dianhydride was added to 1200 g of 6% by weight KOH solution, and the temperature was raised to 90° C. to completely dissolve it. Cool to 50°C, add dropwise 65g of 98% by weight H 2 SO 4 After the solution was stirred evenly (PH=5-6), it was filtered and washed. The perylenetetracarboxylic acid filter cake was mixed with water, and the total amount was adjusted to 724g. Add 81.3g of p-chloroaniline (0.638mol) and 28.4g of pyridine (0.360mol), mix evenly, transfer the material to an autoclave, seal it, heat up to 135-140°C (0.2-0.3MPa), keep stirring for 4h, Sampling and testing, if the perylenetetraic dianhydride in the reactant is exhausted, the reaction is over, cooled to room temperature, and filtered. Wash with hot water until there is no green fluorescence, and obtain the crude product filter cake of reduced brilliant red RB. The filter cake is beaten with water, and 10% by weight of sodium hypochlorite solution i...

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Abstract

The invention relates to a method for preparing vat brilliant red RB (Algol Scarlet B), comprising the following steps: adding 3, 4, 9, 10-perylene tetracid dianhydride into KOH water solution and heating the solution to fully dissolve it, and cooling the solution to 50 degrees centigrade and neutralizing KOH in the solution by H2SO4 until the pH value equals to 5-6, and orange perylene tetra-formic acid is separated out; filtering and washing the perylene tetra-formic acid, and mixing a perylene tetra-formic acid filter cake with water, and adding parachloroaniline and pyridine into the solution, and uniformly stirring them, and transferring the material into a pressure kettle and closing the kettle, and raising the temperature to 130-150 degrees centigrade and performing heat preservation reaction until the perylene tetracid dianhydride is used up, wherein the reaction pressure is 0.2-0.4 MPa; cooling the material to the room temperature, and filtering it and washing it by hot water until no green fluorescence to obtain a vat brilliant red RB rough product filter cake, and heating and processing the rough product filter cake by sodium hypochlorite solution, and filtering, water washing and drying the cake to obtain a vat red RB dry product. The invention provides a safe, environment-friendly and economic preparation method.

Description

1. Technical field [0001] The invention relates to a preparation method of reduced brilliant red RB (Algol Scarlet B). 2. Background technology [0002] High-grade vat dyes are now widely used in dyeing and printing of linen, cotton, viscose and other fabrics. Among them, vat brilliant red RB (Algol Scarlet B) is an important species in vat dyes. It has bright shade; good application performance and excellent color matching performance. As a pigment, it is the brightest of the red perylene (Perylene) pigments, and is mainly used in the paint of the French red car. Its structure is as follows: [0003] [0004] The dye is registered as Vat Red 32 and Pigment Red 189 (CI.71135; CAS: 2379-77-3) in the "Dye Index". [0005] Reduced Brilliant Red RB can be prepared by reacting perylenetetracarboxylic acid or its anhydride with p-chloroaniline. The reaction can be carried out in water or in an organic solvent. If the former, according to US Patent US2543747, the reaction n...

Claims

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Application Information

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IPC IPC(8): C09B5/62
Inventor 丁国跃何可立
Owner 上海华元实业有限公司
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