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Synthesis method of environment-friendly solvent violet 13 with low toxicity and low harm

An environment-friendly solvent and synthesis method technology, applied in chemical instruments and methods, preparation of organic compounds, organic dyes, etc., can solve the problem of difficult control of competitive double condensation and hydrolysis side reactions, affecting reaction selectivity and color reproducibility It is very poor and other problems, and achieves the effects of safety improvement, product purity improvement and easy recovery

Inactive Publication Date: 2019-12-20
安徽清科瑞洁新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The quality of solvent violet 13 produced by this process is poor, and the reproducibility of color and light is very poor. The hue △E>0.5 accounts for about 50% of the total output. Some single batch products need to be refined by solvents to achieve qualified quality, resulting in Waste of resources and pollution to the environment; the reaction yield is low, about 81%, and the competitive double condensation and hydrolysis side reactions generated in the reaction process are not easy to control, which affects the reaction selectivity and then affects the product yield

Method used

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  • Synthesis method of environment-friendly solvent violet 13 with low toxicity and low harm
  • Synthesis method of environment-friendly solvent violet 13 with low toxicity and low harm

Examples

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preparation example Construction

[0022] A kind of synthetic method of low toxicity and low harm environment-friendly solvent violet 13 of the present invention comprises the following steps:

[0023] (a) add N-butylimidazole, auxiliary agent (for being selected from the mixture of one or more compositions in aluminum chloride, zinc chloride and barium chloride) in high-pressure reaction vessel, feed chlorine slowly again Ethane gas is reacted, until the pressure in the high-pressure reaction vessel does not drop, stop ventilating, continue to stir, remove excessive chloroethane under reduced pressure, obtain ionic liquid; The mass ratio of N-butylimidazole, chloroethane, auxiliary agent is 1:0.5~0.6:0.05;

[0024] (b) Raise the temperature of the ionic liquid to 75-85°C, then add 1,4-dihydroxyanthraquinone, 1,4-dihydroxyanthraquinone leuco, p-methylaniline into the high-pressure reaction vessel, and raise the temperature to 95- Condensation reaction was carried out at 105°C to obtain the first mixed solution...

Embodiment 1

[0029] This embodiment provides a method for synthesizing low-toxicity, low-hazard, and environment-friendly solvent violet 13, which comprises the following steps:

[0030] (a) Add 890 kilograms of N-butyl imidazoles and 44.5 kilograms of zinc chloride in the high-pressure reaction vessel, then slowly feed 485 kilograms of ethyl chloride gas to react until the pressure in the high-pressure reaction vessel does not drop and stop ventilation, continue to stir After 2 hours, excess ethyl chloride was removed under reduced pressure to obtain an ionic liquid;

[0031] (b) Warm up the ionic liquid to 80°C, then add 820 kg of 1,4-dihydroxyanthraquinone, 142 kg of 1,4-dihydroxyanthraquinone leuco, and 430 kg of p-methylaniline into the high-pressure reaction vessel, heating up to 100°C for condensation reaction to obtain the first mixed solution;

[0032] (c) Lower the temperature of the first mixed solution to 45°C, open the valve of the high-pressure reaction vessel, and discharge...

Embodiment 2

[0034] The present embodiment provides a kind of synthetic method of low toxicity, low harm and environment-friendly solvent violet 13, which is basically consistent with that in Example 1, except that the amount of p-methylaniline added in step (b) is 481 kilograms; finally After drying, pulverizing and packaging, 1196 kg of finished solvent violet 13 was obtained; the yield was 90.7%, the HPLC content was 95.87%, △E 0.467, △C 0.375 partial bright, pressure value 0.37.

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Abstract

The invention relates to a synthesis method of environment-friendly solvent violet 13 with low toxicity and low harm. The method comprises the following steps: (a), N-buthylimidazole and an auxiliaryare added to a high-pressure reaction container, chloroethane gas is slowly introduced for reaction, stirring is continued, and an ionic liquid is obtained; (b), the ionic liquid is heated to 75-85 DEG C, 1,4-dihydroxyanthraquinone, a 1,4-dihydroxyanthraquinone leuco body and methylaniline are added, the temperature is increased to 95-105 DEG C for a condensation reaction, and a first mixed solution is obtained; and (c), the first mixed solution is cooled to 40-50 DEG C and subjected to suction filtration, a filter cake and a filtrate are obtained, the filter cake is subjected to aftertreatment, and the solvent violet 13 is obtained. The synthesized ionic liquid is taken as the solvent, by means of model selection of organic cations in the ionic liquid, the condensation reaction is changedinto single condensation, product quality is improved to 95% or higher, yield reaches 90% or higher, production cost is greatly reduced, economic benefits are obvious, and pollution emissions are reduced; and for the obtained solvent violet 13 dye, delta E is smaller than 0.5, delta C represents partially colorful, and pressure value is smaller than 0.5.

Description

technical field [0001] The invention relates to a method for synthesizing a dye, in particular to a method for synthesizing low-toxicity, low-hazard, and environment-friendly solvent violet 13. Background technique [0002] Solvent Violet 13 is also known as Solvent Blue 90 and Disperse Blue 72. Its chemical name is 1-hydroxy-4-(p-toluidine)-anthraquinone, its English name is Solvent Violet 13, and its molecular formula is C 21 h 15 NO 3 , the molecular weight is 329.35, and the CAS number is 81-48-1. The appearance of this product is purple-black powder, insoluble in water, soluble in organic solvents such as benzene, chlorobenzene, xylene, DMF, etc., it appears dark green in concentrated sulfuric acid, and produces olive to red light blue precipitate after dilution. Solvent Violet 13 can be used in the coloring of various resin plastics, such as polyacrylic resin, ABS resin, polystyrene, plexiglass, polyester resin, polycarbonate, etc., to obtain red light blue; it has ...

Claims

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Application Information

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IPC IPC(8): C09B1/514C07C221/00C07C225/36
CPCC07C221/00C07C2603/24C09B1/5145C07C225/36
Inventor 周利霞张标来杨庆水刘镛
Owner 安徽清科瑞洁新材料有限公司
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