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Hydroquinone preparation method

A technology of hydroquinone and p-chlorophenol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low recovery rate of manganese resources, serious environmental pollution, and high equipment costs, and achieve recycling The effect of good application effect, low equipment investment and high production cost

Active Publication Date: 2015-05-20
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the consumption of raw materials is high, and a large amount of manganese sulfate, ammonium sulfate waste liquid and iron sludge are produced in the production process, which seriously pollutes the environment; the dilute sulfuric acid contained in the reaction feed liquid corrodes the equipment, and the equipment cost is high; in addition, the recycling rate of manganese resources Low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 106.6g of p-chlorophenol, 581.0g of 40% potassium hydroxide, KOH / ZrO into a 1L autoclave 2 Catalyst 10.7g, heated up after nitrogen replacement, controlled reaction temperature 215°C, reacted for 12 hours, recovered the catalyst by filtering the alkali solution, and acidified the filtrate to pH=2-3 with 430g of 35% concentrated hydrochloric acid. The conversion rate of p-chlorophenol is 98.5%, and the selectivity of hydroquinone is 87.1%.

Embodiment 2

[0030] Put 21.3g of p-chlorophenol, 493.9g of 10% potassium hydroxide, NaOH / ZrO into a 1L autoclave 2 Catalyst 3.0g, heat up after nitrogen replacement, control the reaction temperature at 210°C, react for 12 hours, and recover the catalyst by filtering the alkali solution, and acidify the filtrate with 93.0g of 35% concentrated hydrochloric acid to pH=2~3. The conversion rate of p-chlorophenol is 78.2%, and the selectivity of hydroquinone is 89.4%.

Embodiment 3

[0032] In a 1L autoclave, 79.9 g of p-chlorophenol, 522.9 g of 25% concentration potassium hydroxide, and Na 2 CO 3 / ZrO 2 Catalyst 9.7g, heat up after nitrogen replacement, control the reaction temperature at 220°C, react for 8 hours, and recover the catalyst by filtering the alkali solution, and acidify the filtrate to pH=2-3 with 245.3g of 35% concentrated hydrochloric acid. The conversion rate of p-chlorophenol is 82.4%, and the selectivity of hydroquinone is 90.1%.

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PUM

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Abstract

The present invention relates to a hydroquinone preparation method, especially to a method for preparing hydroquinone by adopting a supported solid alkali as a catalyst and carrying out an alkaline hydrolysis reaction on p-chlorophenol and a potassium hydroxide solution. According to the present invention, the supported solid alkali is adopted as the catalyst, the p-chlorophenol and the potassium hydroxide solution are subjected to an alkaline hydrolysis reaction at a certain temperature, the alkaline hydrolysis solution is filtered to recover the catalyst so as to be applied indiscriminately, the filtrate is acidified with hydrochloric acid to achieve the pH value of 2-3, the reaction product is extracted with methyl isobutyl ketone, and the raw material content and the product content in the raffinate are less than 0.05%.

Description

technical field [0001] The invention relates to a method for preparing hydroquinone, in particular to a method for preparing hydroquinone through alkaline hydrolysis reaction of p-chlorophenol and potassium hydroxide solution by using a loaded solid base as a catalyst. Background technique [0002] Hydroquinone is mainly used as a photographic imaging agent, a drug raw material, a polymerization inhibitor added during monomer storage and transportation, a rubber antioxidant, an azo dye, an anthraquinone dye, a stabilizer, an antioxidant, etc. [0003] There are more than ten production methods of hydroquinone, among which the main ones that have been industrialized are aniline oxidation, dicumyl peroxidation, bisphenol A, and phenol hydrogen peroxide hydroxylation. [0004] Aniline oxidation is the earliest production method of hydroquinone. The production process usually includes a two-step reaction, that is, aniline is oxidized to p-benzoquinone by manganese dioxide (or s...

Claims

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Application Information

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IPC IPC(8): C07C39/08C07C37/02
CPCC07C37/02C07C39/08
Inventor 程晓曦顾克军徐林顾志强丁克鸿黄杰军张晓谕缪荣荣
Owner JIANGSU YANGNONG CHEM GROUP
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