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A kind of preparation method of environment-friendly disperse dye

An environmentally friendly technology for disperse dyes, applied in azo dyes, organic dyes, monoazo dyes, etc., can solve problems such as unsatisfactory effects

Active Publication Date: 2017-07-25
ZHEJIANG RUNTU INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These kinds of over-standard substances are often detected in disperse dyes with 2,6-dichloro-p-nitroaniline as the intermediate. In order to provide more environmentally friendly disperse dyes, it is necessary to add a complicated post-treatment process, and the effect is often not ideal.

Method used

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  • A kind of preparation method of environment-friendly disperse dye
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  • A kind of preparation method of environment-friendly disperse dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 100g of DMF and 135g of 2,6-dichloro-p-nitroaniline (industrial product) into a four-necked flask, stir and heat up to 110°C until 2,6-dichloro-p-nitroaniline is completely dissolved; then slowly Cool down to 60°C, add 250g of methanol, continue to cool down to about 10°C, stir for 0.5 hours and filter with suction, collect the mother liquor to recover DMF and methanol, wash the filter cake with water, and dry to obtain fine 2,6-dichloro-p-nitroaniline 126.8g, the yield is 93.92%.

[0020] Add 30g of 98% sulfuric acid and 47g of nitrosylsulfuric acid into a 250mL four-neck flask, cool down to below 20°C, slowly add 21g of the above-mentioned fine 2,6-dichloro-p-nitroaniline, and keep warm for 2-3 Hours, ready for use; slowly dilute the diazonium salt into ice, then dropwise add the coupling solution containing the structural formula [II] to carry out the coupling reaction, after the addition is completed, continue the heat preservation reaction for 4-6 hours, and th...

Embodiment 2

[0022] Add 100g of DMF and 110g of 2,6-dichloro-p-nitroaniline (industrial product) into a four-neck flask, stir and heat up to 100°C until 2,6-dichloro-p-nitroaniline is completely dissolved; then slowly Cool down to 60°C, add 250g of methanol, continue to cool down to about 10°C, stir for 0.5 hours and filter with suction, collect the mother liquor to recover DMF and methanol, wash the filter cake with water, and dry to obtain fine 2,6-dichloro-p-nitroaniline 101.6g, the yield is 92.36%.

[0023] Add 30g of 98% sulfuric acid and 47g of nitrosylsulfuric acid into a 250mL four-neck flask, cool down to below 20°C, slowly add 21g of the above-mentioned fine 2,6-dichloro-p-nitroaniline, and keep warm for 2-3 Hours, stand-by; Slowly drop the diazonium salt into the coupling solution containing the structural formula [Ⅲ] and the mixture of ice and water to carry out the coupling reaction. The reaction was carried out at ℃ for 1 hour, and the dye was obtained by suction filtration....

Embodiment 3

[0025] Add 100g of DMF and 135g of 2,6-dichloro-p-nitroaniline (industrial product) into a four-necked flask, stir and heat up to 110°C until 2,6-dichloro-p-nitroaniline is completely dissolved; then slowly Cool down to 60°C, add 200g of methanol, continue to cool down to about 10°C, stir for 0.5 hours and filter with suction, collect the mother liquor to recover DMF and methanol, wash the filter cake with water, and dry to obtain fine 2,6-dichloro-p-nitroaniline 127.7g, the yield is 94.59%.

[0026] Add 30g of 98% sulfuric acid and 47g of nitrosylsulfuric acid into a 250mL four-neck flask, cool down to below 20°C, slowly add 21g of the above-mentioned fine 2,6-dichloro-p-nitroaniline, and keep warm for 2-3 Hours, ready for use; slowly dilute the diazonium salt into ice, then dropwise add the coupling solution containing the structural formula [II] to carry out the coupling reaction, after the addition is completed, continue the heat preservation reaction for 4-6 hours, and th...

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Abstract

The invention discloses a method for preparing an environment-friendly disperse dye. The method comprises the following steps: a step (1) of performing crystallization purification on industrial grade 2,6-dichloro paranitroaniline by using dimethyl formamide (DMF) and methanol, and performing filtration, washing and drying to obtain high-quality 2,6-dichloro paranitroaniline; and causing the high-quality 2,6-dichloro paranitroaniline obtained in the step (1) and coupling component to undergo coupling reaction, so as to obtain the environment-friendly disperse dye. Through crystallization operation on 2,6-dichloro paranitroaniline, harmful substances in the final disperse dye are removed effectively, and the higher environmental protection standard is met.

Description

technical field [0001] The invention belongs to the field of preparation of disperse dyes, and in particular relates to a preparation method of environment-friendly disperse dyes. Background technique [0002] With the improvement of people's living standards, the requirements for the quality of disperse dyes are getting higher and higher. On the one hand, more and more disperse dyes with various bright colors and excellent fastness have been developed one after another; Hazardous substances producing adverse effects. [0003] Trichlorophenol (2,4,6-trichlorophenol), tetrachlorophenol (2,3,5,6-tetrachlorophenol, 2,3,4,6-tetrachlorophenol) and pentachlorophenol The substance will strongly irritate the skin of the human body and has certain carcinogenicity. These kinds of over-standard substances are often detected in disperse dyes with 2,6-dichloro-p-nitroaniline as the intermediate. In order to provide more environmentally friendly disperse dyes, it is necessary to add co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B29/08
CPCC09B29/0826C09B29/0829
Inventor 章文刚楼德强高立江陈伟东
Owner ZHEJIANG RUNTU INST