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Synthesis method of dye intermediate

The technology of a dye intermediate and a synthesis method, which is applied in the synthesis field of dye intermediates, can solve problems such as high risk, and achieve the effects of simple method, economic value, environmental protection and economic value.

Inactive Publication Date: 2019-05-28
海门市五洋化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the reaction conditions of this method involve high temperature and high pressure, which is very dangerous, and a large amount of chromium-containing waste acid is produced during the oxidation process, which brings many problems to the subsequent treatment.

Method used

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  • Synthesis method of dye intermediate
  • Synthesis method of dye intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The mass percentage concentration that is 4 parts of sodium nitrite is 40% sodium nitrite solution by weight, is added dropwise in the mass percentage concentration that is 1 part of hydrochloric acid and is 10% hydrochloric acid solution to produce nitrosyl chloride, stirs, simultaneously will generate The nitrosyl chloride passes through the mixture that the 1-nitro-2-methylanthraquinone of 1 part by weight and the sulfur trioxide mass percentage concentration of 2 parts are carried out in the mixture of oleum of 10% by weight, By controlling the drop rate of sodium nitrite solution, the reaction temperature of 1-nitro-2-methylanthraquinone was kept at 30°C, and reacted for 10 hours to obtain feed solution A; dilute feed solution A with 9 parts of water to obtain dilute feed Solution A, by controlling the drop rate of feed liquid A during the dilution process, the control temperature is maintained at 50°C; 1.2 parts of ferrous sulfate solution with a mass percentage co...

Embodiment 2

[0029] The mass percentage concentration that is 6 parts of sodium nitrite is 20% sodium nitrite solution by weight, is added dropwise in the mass percentage concentration that is 4 parts of hydrochloric acid and is 10% hydrochloric acid solution to produce nitrosyl chloride, stirs, simultaneously The nitrosyl chloride that generates is passed into the mixture of 1-nitro-2-methylanthraquinone and 3 parts of 4% oleum by weight to carry out oxidation reaction, by controlling the rate of addition of sodium nitrite solution to make 1 -The reaction temperature of nitro-2-methylanthraquinone is 10°C, react for 14 hours, and obtain feed liquid A; Drop rate, control temperature is 35 ℃; Add 3.8 parts of mass percent concentration in 8 parts of diluted feed liquid A and be 35% ferrous sulfate solution, reaction temperature is 80 ℃, and the reaction time is 3h, obtains feed liquid B, will The material solution B was diluted with 9 parts of water, filtered, washed with water until neutra...

Embodiment 3

[0031] The mass percent concentration that is 5 parts of sodium nitrite is 30% sodium nitrite solution by weight, is added dropwise in the hydrochloric acid solution that the mass percent concentration of 3 parts of hydrochloric acid is 10% to produce nitrosyl chloride, stirs, simultaneously will generate nitrosyl chloride Nitroyl chloride is passed into a mixture of 1 part of 1-nitro-2-methylanthraquinone and 2.5 parts of 8% fuming sulfuric acid for oxidation reaction, and the 1-nitro-2-methyl anthraquinone is oxidized by controlling the rate of addition of sodium nitrite solution. The reaction temperature of base anthraquinone is kept at 20°C, and the reaction is carried out for 12 hours to obtain the feed liquid A; the feed liquid A is diluted with 13 parts of water to obtain the diluted feed liquid A. At 45°C; add 2.5 parts of ferrous sulfate solution with a mass percent concentration of 30% in 8 parts of diluted feed liquid A, the reaction temperature is 90°C, and the reac...

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Abstract

The invention provides a synthesis method of a dye intermediate. The synthesis method includes the following steps that a sodium nitrite solution is dropwise added into a hydrochloric acid solution togenerate nitrosyl chloride, meanwhile, the generated nitrosyl chloride is introduced into a mixture of 1-nitro-2-methylanthraquinone and fuming sulfuric acid to be subjected to oxidation reaction, and thus a feed liquid A is obtained; the feed liquid A is diluted with water to obtain a diluted feed liquid A; a ferrous sulfate solution is added into the diluted feed liquid A for reduction ring-opening to obtain a feed liquid B; and the feed liquid B is diluted with water, filtered and washed to be neutral and then dried to obtain the dye intermediate. By means of the synthesis method, high temperature and high pressure do not need to be used as reaction conditions, reaction products are free of by-products such as chromium-containing waste acid, and the method is simple, convenient and environmentally friendly and has economic value.

Description

technical field [0001] The invention relates to a synthetic method of an intermediate, in particular to a synthetic method of a dye intermediate. Background technique [0002] 1-Amino-2-carboxyanthraquinone is an important intermediate for the synthesis of dyes Vat Red F3B and Vat Blue 64#, etc. Its chemical structure is as follows: [0003] [0004] The conventional synthetic route is to use 1-nitro-2-methylanthraquinone as a raw material, which is first oxidized to 1-nitro-2-carboxyanthraquinone with sodium dichromate under acidic conditions, and then oxidized in ammonia water under high temperature and pressure. Ammonolysis synthesis of 1-amino-2-carboxyanthraquinone, the conventional synthesis process is as follows: [0005] [0006] However, the reaction conditions of this method involve high temperature and high pressure, which is relatively dangerous, and a large amount of chromium-containing waste acid is produced during the oxidation process, which brings man...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/12C07C229/74
Inventor 陆春辉冯随意
Owner 海门市五洋化工有限公司
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