Preparation method of vat violet 1

A technology of isoviolanthrone dichloride and isovinanthrone, which is applied in the field of dye preparation, can solve the problems of toxic substances and difficult recycling, and achieve the effects of high raw powder strength, obvious chlorination effect, and saving drying process

Active Publication Date: 2018-05-18
江苏嘉利精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Technical problem to be solved: Aiming at the technical problems in the prior art that a large amount of organic solvents are used to cause recovery difficulties, and the organic solvents used will bring toxic substances, the invention provides a method for preparing isoviolanthrone dichloride. The product has the advantages of high strength and bright red light, while avoiding the use of a large amount of organic solvents, energy saving and environmental protection

Method used

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  • Preparation method of vat violet 1
  • Preparation method of vat violet 1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Put 41.45g of isoviolanthrone wet filter cake (water content 45wt.%), and put 22.8 g of 100% isviolanthrone dry product into a container, add 30 g of water, 50 g of 98 wt.% sulfuric acid, grind and pulverize Fineness reaches 20 μm, then add 45 g of 1,1,2-trichloroethane. The temperature of the material is 30~35°C, then add 100 mL of sodium hypochlorite solution evenly under the liquid surface within 6 hours (the content of available chlorine is 13 wt.%), and then add 80 mL of sodium hypochlorite evenly within 6 hours at 35~45°C Solution (the content of available chlorine is 13wt.%), keep warm for another 2 h, and reach the reaction end point when the chlorine content of the sample is determined to be 13~14 wt.%. After the end point is reached, add 3wt.% sodium hydroxide solution to adjust the pH= 7~7.5, heat up to reflux, steam trichloroethane, filter after trichloroethane is completely evaporated, wash the filtered filter cake with hot water until the filtrate is color...

Embodiment 2

[0030] Put 38 g of isoviolanthrone wet cake (containing 40 wt.% moisture) and 22.8 g of 100% isoviolanthrone dry product into a container, add 30 g of water, 45.0 g of 98 wt.% sulfuric acid, grind and pulverize The fineness reached 30 μm, then 40 g of 1,2-dichloroethane was added, the temperature of the material was raised to 55 °C, and 180 mL of sodium hypochlorite solution (the content of available chlorine was 13 wt.%) was uniformly added within 16 h below the liquid surface, and then Continue to keep warm for 2 h, add 20 wt.% dilute soda ash solution to adjust pH = 7, raise the temperature to reflux, distill dichloroethane, dichloroethane is distilled and filtered, and the filtered filter cake is washed with hot water until the filtrate colorless. Then the filter cake is taken out and dried to obtain a bright red light product.

Embodiment 3

[0032] Put 45.6g of isoviolanthrone wet cake (containing 50 wt.% moisture) and 22.8 g of 100% isoviolanthrone dry product into a container, add 70 g of water, grind and pulverize to a fineness of 10 μm, and then add Tetrachloroethane 50 g, the material is heated up to 45 ~ 50 ℃. Then, within 20 hours, slowly inject 35 g of chlorine gas at the bottom of the liquid surface, keep it warm for 2 hours, add 20wt.% dilute soda ash solution to adjust the pH=7, raise the temperature to reflux, distill tetrachloroethane, and wait until the tetrachloroethane is completely evaporated After filtering, wash the filtered filter cake with hot water until the filtrate is colorless, then take out the filter cake and dry it to obtain a bright red product.

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Abstract

A preparation method of vat violet 1 belongs to the technical field of dye preparation. The preparation method comprises: adding isoviolanthrone, water and sulfuric acid to a container in sequence, performing grinding and pulverization, adding halogenated alkane to the ground mixture, adding a chloridizing agent below the liquid level, adjusting the pH value till the obtained solution is neutral,raising the temperature of the adjusted mixture till the mixture undergoes reflux, performing filtration till halogenated alkane is totally evaporated, cleaning the filtered cake with hot water till the filtrate is colourless, taking the filtered cake out, and drying the filtered cake to obtain vat violet 1. According to the technical scheme, defects that a large amount of solvent is hard to recycle and causes pollution due to a full-solution chlorination method are overcome. The synthesized vat violet 1 is a bright-colored red purple vat dye, is more bright gorgeous than a product sold in themarket, and is high in intensity of raw powder.

Description

technical field [0001] The invention belongs to the technical field of dye preparation, and in particular relates to a preparation method of isoviolanthrone dichloride. Background technique [0002] Isoviolanthrone dichloride, molecular formula C 24 h 14 Cl 2 o 2 , CAS: 1324-55-6, the trade name is Restored Brilliant Purple 2R. This product is mainly used for the dyeing of cotton, hemp and viscose fibers and the printing of their fabrics. It can also be used for processing organic pigments and as plastic colorants. Vat Brilliant Violet 2R is an extremely important product in vat dyes. It dyes cotton with bright blue-purple, high affinity, average level dyeing, good covering power to dead cotton, excellent fastness, and the fastness to sunlight reaches 6 grades. The other fastnesses are all in the 4-5 grade. It is often used in cotton dyeing and direct printing, and has a good affinity for silk and level dyeing, and is favored by the market. [0003] The existing pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/697C07C45/63C09B3/76
CPCC07C45/63C09B3/76C07C49/697
Inventor 李振奎任照堂李剑刘克伟徐宁刘会
Owner 江苏嘉利精细化工有限公司
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