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Synthesis method of 1,4-diaminoanthraquinone and leuco body thereof

A technology of diaminoanthraquinone and synthesis method, which is applied in the field of synthesis of 1,4-diaminoanthraquinone and its leuco body, can solve the problems of high ammonia nitrogen wastewater and low product purity, reduce cost pressure, and improve product quality. Quality, cost reduction effects

Inactive Publication Date: 2020-05-01
常州悦朋科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the defects of high ammonia nitrogen wastewater and low product purity in the production process of 1,4-diaminoanthraquinone in the prior art, and provide a kind of 1,4-diaminoanthraquinone and its leuco synthesis method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 90g of 90% sodium hydroxide, 116g of 32% sodium hydroxide, 89g of 1,4-dihydroxyanthraquinone and 215g of 20% ammonia water into a 1L autoclave. Close the autoclave and start stirring. After stirring for 30 minutes, the temperature was raised to 92° C., and the temperature was kept at 0.4 MPa for 4 hours. Cool down to 50°C, filter after pressure relief, wash with hot water until the filtrate pH is 7-8, and dry. 81.4 g of the product was obtained, the total amount of 1,4-diaminoanthraquinone and its leuco was 96% as detected by HPLC, and the calculated molar yield was 88%.

Embodiment 2

[0013] Add 108g of 90% sodium hydroxide, 139g of 32% sodium hydroxide, 89g of 1,4-dihydroxyanthraquinone and 215g of 20% ammonia water into a 1L autoclave. Close the autoclave, start stirring, stir for 30 minutes, then raise the temperature to 95°C, keep the temperature for 4 hours, and the pressure is 0.6MPa. Cool down to 50°C, filter after pressure relief, wash with hot water until the filtrate pH is 7-8, and dry. 85 g of the product was obtained, the total amount of 1,4-diaminoanthraquinone and its leuco was 97% as detected by HPLC, and the calculated molar yield was 93%.

Embodiment 3

[0015] Add 81g of 90% sodium hydroxide, 105g of 32% sodium hydroxide, 89g of 1,4-dihydroxyanthraquinone and 215g of 20% ammonia water into a 1L autoclave. Close the autoclave and start stirring. After stirring for 30 minutes, the temperature is raised to 88° C., and the temperature is kept at 0.3 MPa for 4 hours. Cool down to 50°C, filter after pressure relief, wash with hot water until the filtrate pH is 7-8, and dry. 80 g of the product was obtained, and the total amount of 1,4-diaminoanthraquinone and its leuco was 94% as detected by HPLC, and the calculated molar yield was 86%.

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PUM

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Abstract

The invention discloses a synthesis method of 1,4-diaminoanthraquinone and a leuco body thereof. The synthesis method comprises the following steps: adding 1,4-dihydroxyanthraquinone, sodium hydroxide, sodium hydrosulfite and an ammonia water solution into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, carrying out uniform stirring, carrying out heating to 85-95 DEG C,carrying out a heat preservation reaction for several hours, performing cooling to 40-50 DEG C, carrying out pressure relief and discharging, conducing washing with hot water until a pH value is 7-8,and carrying out drying. During feeding, sodium hydroxide is added to be matched with sodium hydrosulfite for use, so the reduction effect of sodium hydrosulfite is brought into full play; and cost pressure caused by three-waste treatment is reduced while product quality is improved. The purity of the obtained 1,4-diaminoanthraquinone and the leuco body thereof is increased from 90% to 95%, the yield is increased from 80% to 88%, obtained ammonia-nitrogen wastewater is halved, and treatment cost of the ammonia-nitrogen wastewater is reduced; and the method does not use an organic solvent, reduces the use amount of ammonia water, and lowers the cost of recovering and treating the organic solvent.

Description

technical field [0001] The invention relates to a synthesis method of 1,4-diaminoanthraquinone and its leuco body. Background technique [0002] 1,4-Diaminoanthraquinone is an important fine chemical intermediate, which can be used in the synthesis of various dyes such as disperse violet 28, and the market demand is tight. Due to the increasingly stringent national environmental protection policies, the cost of high COD organic wastewater and high ammonia nitrogen wastewater treatment limits the large-scale production of traditional processes, and the purity of 1,4-diaminoanthraquinone produced by traditional processes is too low, only 88%. about. Contents of the invention [0003] The technical problem to be solved by the present invention is to overcome the defects of high ammonia nitrogen wastewater and low product purity in the production process of 1,4-diaminoanthraquinone in the prior art, and provide a kind of 1,4-diaminoanthraquinone and its leuco synthetic metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C225/34C07C221/00
CPCC07C221/00C07C225/34
Inventor 吴建中邹小冬
Owner 常州悦朋科技有限公司