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Waste discharge-free preparation method for 1,4-dihydroxy-anthraquinone

A dihydroxyanthraquinone and waste discharge technology, which is applied in the preparation of organic compounds, quinone preparation, chemical instruments and methods, etc., can solve a large number of waste acids, waste gas, pollutants and other problems, and achieve the effect of saving production costs

Inactive Publication Date: 2016-03-02
甘肃金缘泰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problem that a large amount of waste acid and exhaust gas pollutants are produced during the preparation and production of 1,4-dihydroxyanthraquinone in the above-mentioned prior art, the present invention provides a 1,4-dihydroxyanthraquinone without waste discharge preparation method

Method used

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  • Waste discharge-free preparation method for 1,4-dihydroxy-anthraquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Such as figure 1 Process flow shown, at 5m 3 In the condensation reactor, add p-chlorophenol 600kg, 20% oleum 2000kg, phthalic anhydride 1000kg and boric anhydride 230kg (wherein, the mass ratio of p-chlorophenol, oleum, phthalic anhydride and boric anhydride is 0.6:2.0:1.0:0.23 ), then the oil bath was heated up to 200°C, kept warm for condensation reaction for 30h, pressed into a hydrolysis kettle with 10000L of water, adjusted the temperature to 100°C, kept warm and hydrolyzed for 4h, discharged and press-filtered, and the filter cake was washed with water until neutral. After drying, 900 kg of 1,4-dihydroxyanthraquinone was obtained. The detected moisture content was 0.2wt%, and the toluene insoluble matter was 0.3wt%. Through liquid chromatography analysis, the content of 1,4-dihydroxyanthraquinone reached 97.3wt%.

[0054] Discharging is added in the sulfuric acid solution that pressure filtration obtains, light-burned magnesia (88wt%) 1100kg is carried out react...

Embodiment 2

[0058] Such as figure 1 Process flow shown, at 5m 3 In the condensation reactor, add p-chlorophenol 700kg, 20% oleum 2500kg, phthalic anhydride 1100kg and boric anhydride 300kg (wherein, the mass ratio of p-chlorophenol, oleum, phthalic anhydride and boric anhydride is 0.7:2.5:1.1:0.30 ), then the oil bath was heated up to 195°C, kept warm for condensation reaction for 35 hours, pressed into a hydrolysis kettle with 12000L of water, adjusted the temperature to 95°C, kept warm for 5 hours, and discharged for pressure filtration, and the filter cake was washed with water until neutral. After drying, 1000 kg of 1,4-dihydroxyanthraquinone was obtained. The detected moisture content was 0.18wt%, and the toluene insoluble matter was 0.4wt%. Through liquid chromatography analysis, the content of 1,4-dihydroxyanthraquinone reached 96.5wt%.

[0059] Add light-burned magnesia (85wt%) 1250kg to the sulfuric acid solution obtained by pressure filtration and react at 90°C for 0.5h (wherei...

Embodiment 3

[0063] Such as figure 1 Process flow shown, at 5m 3 In the condensation reactor, add p-chlorophenol 650kg, 20% oleum 2200kg, phthalic anhydride 1000kg and boric anhydride 250kg (wherein, the mass ratio of p-chlorophenol, oleum, phthalic anhydride and boric anhydride is 0.65:2.2:1.0:0.25 ), then the oil bath was heated up to 205°C, kept warm for condensation reaction for 25h, pressed into a hydrolysis kettle with 11000L of water, adjusted the temperature to 105°C, kept warm for 3h, and discharged for pressure filtration, and the filter cake was washed with water until neutral. After drying, 950 kg of 1,4-dihydroxyanthraquinone was obtained. The detected moisture content was 0.22wt%, and the toluene insoluble matter was 0.3wt%. Through liquid chromatography analysis, the content of 1,4-dihydroxyanthraquinone reached 97.1wt%.

[0064] Discharge is added in the sulfuric acid solution that obtains through pressure filtration, light-burned magnesia (95wt%) 1400kg is carried out rea...

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Abstract

The invention provides a waste discharge-free preparation method for 1,4-dihydroxy-anthraquinone. The method comprises the following steps of: (1) by taking parachlorophenol, fuming sulphuric acid, phthalic anhydride and boric anhydride as raw materials, carrying out a condensation reaction and a hydrolysis reaction to obtain a solution, filtering the solution to obtain a filter cake, and drying the filter cake to obtain 1,4-dihydroxy-anthraquinone; (2) adding light calcined magnesia into a filtrate obtained by filtering the solution to react, then extracting boric acid by virtue of cooling and air floatation, and recycling boric anhydride prepared from boric acid through the reaction as the raw material; (3) evaporating, crystallizing and calcining the residual liquid, from which the boric acid has been extracted by virtue of cooling and air flotation, to obtain anhydrous magnesium sulfate; and (4) preparing anhydrous calcium chloride by using HCl gas generated in the process of the step (1). In the whole production process, no waste acids and exhaust gas are discharged, and the prepared product can be sold as the raw material, so that the preparation method is a clean production process, and the prepared boric anhydride is recycled, and therefore, the production cost is lowered.

Description

technical field [0001] The invention belongs to the field of clean production of fine chemicals, and relates to a preparation method of 1,4-dihydroxyanthraquinone, in particular to a preparation method of 1,4-dihydroxyanthraquinone without waste discharge. Background technique [0002] 1,4-Dihydroxyanthraquinone is an important dye intermediate, which can be used to synthesize and analyze Blue R, Disperse Blue SW, Acid Anthraquinone Violet SG, Acid Anthraquinone Green G, Lake Purple 3BL, Lake Purple 4BL and Prayan blue variety of dyes. It can also further synthesize dye intermediate 1,4-diaminoanthraquinone, and it can also make disperse brown GL and dyes. The main raw materials of 1,4-dihydroxyanthraquinone are p-chlorophenol, oleum, phthalic anhydride, and boric acid. The sulfuric acid in the raw materials is used as a solvent and dehydrating agent, and boric acid is used as a catalyst. The two themselves do not enter the product, and are finally diluted with water. It b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/00C07C50/34C01F11/28C01F5/40
CPCC01F5/40C01F11/28C07C46/00C07C50/34
Inventor 赵红林
Owner 甘肃金缘泰新材料有限公司