Method for preparing 1,4-dihydroxy anthraquinone

A technology of dihydroxyanthraquinone and boric acid, applied in the field of 1,4-dihydroxyanthraquinone synthesis, can solve the problems of waste of raw materials, high cost, environmental pollution, etc. The effect of good catalytic effect

Inactive Publication Date: 2015-09-23
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The traditional process uses boric acid as a catalyst. When the concentration of oleum is lower than a certain value, the reaction will be affected. In order to ensure the effective progress of the reaction, more sulfuric acid or oleum is often added, which not only increases the production cost, but also Excess raw materials are often discharged in the form of wastewater, which not only wastes resources, but also seriously pollutes the environment
[0007] The Chinese patent with publication number CN103664567A discloses a 1,4-dihydroxyanthraquinone production process using oleum as a solvent and a dehydrating agent and boric acid as a catalyst, which achieves a good yield, but the hair The mass ratio of nicotinic acid to p-chlorophenol is as high as 5.28, a large amount of raw materials are wasted, and the cost of post-treatment is also too high

Method used

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  • Method for preparing 1,4-dihydroxy anthraquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Boric acid was heated at 250°C for 10 hours to obtain boric acid dehydration compound; the boric anhydride in the boric acid dehydration compound was determined to be 99.3% and tetraboric acid 0.7% by elemental analysis;

[0028] In the condensation reactor, add oleum 350kg, phthalic anhydride 120kg, boric acid dehydration compound 40kg, p-chlorophenol 100kg (oleum: phthalic anhydride: metaboric acid: p-chlorophenol = 3.5: 1.2: 0.4: 1); oil bath Raise the temperature to 100°C for the material, precisely control the reaction temperature at 100~105°C, and keep it warm for 0.5 hours; press the material into a hydrolysis kettle with 300L of water, adjust the temperature to 50°C, keep it at 50°C for 0.1 hour, discharge the material, press filter, and wash with water To neutrality, blow dry to obtain 400.2kg of 1,4-hydroxyanthraquinone tide product, the moisture content is 54.2%, and the dry product is 183.3kg. Through liquid chromatography analysis, the content of 1,4-hydrox...

Embodiment 2

[0030] Boric acid was heated at 130°C for 2 hours to obtain boric acid dehydration compound; the content of metaboric acid in boric acid dehydration compound was 92.1% and tetraboric acid 7.9% according to elemental analysis.

[0031] In the condensation reaction kettle, add oleum 450kg, phthalic anhydride 150kg, boric acid dehydration compound 60kg, p-chlorophenol 100kg (oleum: phthalic anhydride: metaboric acid: p-chlorophenol = 4.5: 1.5: 0.6: 1); oil bath Raise the temperature to 250°C of the material, and keep it warm for 30 hours. Press the material into a hydrolysis kettle with 4500L of water, adjust the temperature to 105°C, keep it at 105~115°C for 4 hours, press filter, wash with water until neutral, and dry to obtain 1,4-hydroxyanthraquinone trendy product 507.1kg, tested moisture content 53.6%, converted to dry product 235.3kg, through liquid chromatography analysis, the content of 1,4-hydroxyanthraquinone reached 87.26%, dry product purity 81.43%, yield 89.5%.

Embodiment 3

[0033] Boric acid was heated at 220°C for 5 hours to obtain boric acid dehydration compound; the boric acid dehydration compound was determined to be 20.7% tetraboric acid and 79.3% boric anhydride in the boric acid dehydration compound.

[0034] In the condensation reactor, add oleum 400kg, phthalic anhydride 130kg, boric acid dehydration compound 50kg, p-chlorophenol 100kg (oleum: phthalic anhydride: boric acid dehydration compound: p-chlorophenol=4.0:1.3:0.5:1). Raise the temperature of the material in the oil bath to 190°C, and keep it warm for 15 hours; press the material into a hydrolysis kettle with 2000L of water, adjust the temperature to 100°C, keep it at 100-105°C for 4 hours, discharge the material, press filter, wash with water until neutral, Blow dry to obtain 413.6kg of 1,4-hydroxyanthraquinone tidal product, the detected moisture content is 55.3%, and the dry product is 184.9kg. Through liquid chromatography analysis, the content of 1,4-hydroxyanthraquinone rea...

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Abstract

The invention discloses a method for preparing 1,4-dihydroxy anthraquinone by taking a boric acid dehydration compound as a catalyst. The method comprises the following steps: (1) heating boric acid at 100-250 DEG C to prepare the boric acid dehydration compound; (2) adding fuming sulphuric acid, phthalic anhydride, the boric acid dehydration compound and parachlorophenol into a condensation kettle in sequence, and carrying out condensation reaction at 100-250 DEG C; (3) adding a proper amount of water and the materials in the condensation kettle into a hydrolysis kettle, carrying out hydrolysis reaction at 50-115 DEG C, discharging a reactant, filtering the reactant by pressing, washing and drying the reactant to prepare 1,4-dihydroxy anthraquinone. According to the method, the boric acid dehydration compound is used as the catalyst, so that the addition amount of the raw materials including fuming sulphuric acid and phthalic anhydride is reduced; the resource consumption can be reduced; the cost is reduced; the waste emission is reduced; the method is relatively environmentally-friendly and economical.

Description

technical field [0001] The invention relates to the technical field of 1,4-dihydroxyanthraquinone synthesis, in particular to a method for preparing 1,4-dihydroxyanthraquinone by using a boric acid dehydration compound as a catalyst. Background technique [0002] 1,4-Dihydroxyanthraquinone, commonly known as quinazine, is an important dye intermediate, which can be used in the production of disperse dyes, solvent dyes, acid dyes and vat dyes, etc. important raw material. [0003] The traditional production process of 1,4-dihydroxyanthraquinone mainly includes hydroquinone method and p-chlorophenol method: the hydroquinone method uses boric acid as a catalyst, and uses hydroquinone and phthalic anhydride to carry out ring closure reaction in sulfuric acid Generate 1,4-dihydroxyanthraquinone. The disadvantages of this process are the shortage of domestic hydroquinone, high price, severe carbonization of hydroquinone in the reaction process, low yield, high production cost, et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/34C07C46/00
CPCC07C46/00C07C2603/24
Inventor 王登兵吴传龙
Owner JIANGSU YABANG DYE
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