Novel process for producing 1,4-dihydroxy anthraquinone

A technology of dihydroxyanthraquinone and new process is applied in the field of p-chlorophenol production, which can solve the problems of high labor intensity, long process time, unstable product quality, etc. The effect of production cost and labor intensity

Inactive Publication Date: 2014-03-26
PENGZE XINGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, whether it is the hydroquinone route or the p-chlorophenol route, a large amount of water must be used for multiple washings during the product separation process, resulti

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1: Add 200ml of oleum and 35g of boric acid into a three-necked flask equipped with a stirring blade and a thermometer, slowly raise the temperature to 110°C, keep it warm for 30-60 minutes, then add 95g of phthalic anhydride, and the temperature will be reduced by the heat released by the reaction. When the temperature rises to about 130°C, start to add 75 grams of p-chlorophenol several times in batches, and complete the addition within 4 hours. The temperature of the whole feeding process is controlled at 130-150°C. After adding p-chlorophenol, the temperature was raised to 200-205°C and kept for 5 hours. Pour the reaction product into 8 times the volume of water for hydrolysis, control the temperature above 100°C and stir for 30 minutes, add 200ml of toluene to the hydrolyzate, drain the lower layer of waste acid after standing, add 100ml of 90°C to the upper layer extract Wash with hot water, drain the washing wastewater after standing still, heat and steam...

example 2

[0011] Example 2: Add 200ml of oleum and 45 grams of boric acid into a three-necked flask equipped with a stirring blade and a thermometer, slowly heat up to 110°C, keep warm for 30 to 60 minutes, then add 95 grams of phthalic anhydride, and raise the temperature by the heat released by the reaction. When the temperature reaches about 130°C, start to add 75 grams of p-chlorophenol several times in batches, and complete the addition within 4 hours. The temperature of the whole feeding process is controlled at 130-150°C. After the addition, the temperature was raised to 200-205°C for 5 hours. Pour the reaction product into 8 times the volume of water for hydrolysis, control the temperature above 100°C and stir for 30 minutes, add 200ml of toluene to the hydrolyzate, drain the lower layer of waste acid after standing, add 100ml of 90°C to the upper layer extract Wash with hot water, drain the washing wastewater after standing still, heat and steam the toluene, the residue in the ...

example 3

[0012] Example 3: Add 4000kg of fuming sulfuric acid and 350kg of boric acid into a 5000L reactor, slowly raise the temperature to 110°C, keep it warm for 30-60 minutes, then add 950kg of phthalic anhydride, and the temperature will rise to about 130°C by the heat released by the reaction. Begin to add 750kg of p-chlorophenol in batches several times, and finish adding within 4 hours. The temperature of the whole addition process is controlled at 130-150°C. After adding p-chlorophenol, the temperature was raised to 200-205°C and kept for 5 hours. Put the reaction product into a hydrolysis kettle pre-added with 12000kg of water, control the temperature above 100°C and stir for 30 minutes, add 2000 L of toluene to the hydrolysis kettle, drain the lower layer of waste acid after standing still, and then add 1000 L Wash with hot water above 90°C, drain the washing wastewater after standing still, pump the extract into the toluene still, and recycle the evaporated toluene. After t...

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PUM

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Abstract

The invention discloses a novel process for producing 1,4-dihydroxy anthraquinone, and relates to the technical field of chemical production. The technological process is as follows: firstly, co-heating and dehydrating fuming sulphuric acid and boric acid for 30-60 minutes, adding phthalic anhydride, heating up to 130 DEG C, adding parachlorophenol into the reaction system for multiple times in batches, heating up to 200-205 DEG C after adding the parachlorophenol, continuously reacting for 5-10 hours, slowly putting a reactant in 8 times by volume of water for hydrolysis after the reaction is finished, controlling the hydrolysis temperature at 100-130 DEG C, extracting the product to an organic phase by use of a solvent after hydrolysis, discharging the lower-layer waste acid, washing the upper-layer extracting solution by use of hot water, distilling the solvent for cycle use, and carrying out high-vacuum distillation and sublimation to obtain high-quality 1,4-dihydroxy anthraquinone. The novel process disclosed by the invention is used for improving the product yield and reducing the production cost by regulating process conditions such as raw material feeding ratio, feeding method, feeding temperature and the like on the premise of ensuring the product yield and the product quality.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a new process for producing 1,4-dihydroxyanthraquinone by p-chlorophenol method. Background technique [0002] 1,4-dihydroxyanthraquinone, commonly known as quinazine, can be used as smoke dyes, pigments and solvent dyes, and can also be used as disperse dyes in transfer printing process. In addition, 1,4-dihydroxyanthraquinone is an important intermediate in the synthesis of aminoanthraquinone, which can be used to synthesize 1,4-diaminoanthraquinone, 1-hydroxy-4-substituted aminoanthraquinone, 1,4-disubstituted amino Anthraquinone, or introducing a substituent at the β-position to obtain a series of red and blue dyes, is widely used in the synthesis of disperse dyes, acid dyes, reactive dyes, and vat dyes, and plays an important role in the dye industry. The anthraquinone dyes synthesized therefrom are one of the most important types in the anthraquinone dye family...

Claims

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Application Information

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IPC IPC(8): C07C50/34C07C46/00C09B1/04
CPCC07C46/00C09B1/04
Inventor 缪玉群赵新良
Owner PENGZE XINGDA CHEM
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