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Method for preparing resorcinol

A technology of resorcinol and m-aminophenol, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as harsh conditions, complex processes, and high equipment requirements, and achieve mild reaction conditions and process Easy technology and good product quality

Inactive Publication Date: 2016-05-25
浙江精进药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the sulfonated alkali fusion method uses benzene as raw material, adds fuming sulfuric acid to react, and then uses sodium hydroxide for alkali fusion, then dissolves in water, and produces with acid acidification, mainly including four processes of sulfonation, neutralization, alkali fusion and acidification , although the sulfonated alkali fusion method has the characteristics of simple investment, low investment and sufficient supply of raw materials, but the production efficiency is low, the energy consumption is large, the three wastes are generated, the treatment cost is high, and the environmental pollution such as waste water and waste is serious
The m-dicumene oxidat

Method used

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  • Method for preparing resorcinol

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Effect test

Embodiment 1

[0029] Add 211g of sulfuric acid (2.15mol) with a mass concentration of 98% into a 2L reaction flask containing 800g of water while stirring, cool to 30°C, add 110g (1.01mol) of m-aminophenol, and stir to dissolve. Cool to -5°C, add dropwise a solution composed of 73.6g (1.07mol) sodium nitrite and 200g water, and the reaction is exothermic. During the dropping process, the dropping speed is controlled, so that the temperature of the system is controlled at -5°C to 5°C. After the dropwise addition, the temperature was raised to 40° C., and the temperature was kept for 2 hours. At this time, bubbles no longer emerged (remarks: the bubbles were nitrogen, and when bubbles still emerged, it indicated that the diazonium salt had not been decomposed), and the obtained Hydroquinone aqueous solution (ie, decomposition reaction solution). Cool the reaction solution to 15°C and keep it warm for 30 minutes. Filter, extract the filtrate with 600g*2 ethyl acetate, combine the ethyl aceta...

Embodiment 2

[0031] Add 153g of 98% sulfuric acid (1.56mol) into a 2L reaction flask containing 800g of water while stirring, cool to 30°C, add 110g (1.01mol) of m-aminophenol, and stir to dissolve. Cool to -5°C, add dropwise a solution composed of 73.6g (1.07mol) sodium nitrite and 200g water, and the reaction is exothermic. During the dropping process, the dropping speed is controlled, so that the temperature of the system is controlled at -5°C to 5°C. After the dropwise addition, the temperature was raised to 60° C., and the temperature was kept for 2 hours. At this time, no bubbles emerged, and an aqueous solution of resorcinol was obtained. Cool the reaction solution to 15°C and keep it warm for 30 minutes. Filter, extract the filtrate with 600g*2 ethyl acetate, combine the ethyl acetate extracts, wash with 100g saturated brine, and separate the layers. Concentrate the ethyl acetate layer under reduced pressure (concentrate under vacuum -0.08MPa, 50°C until no liquid drops out), dis...

Embodiment 3

[0033] Add 240g of sulfuric acid (2.45mol) with a mass concentration of 98% into a 2L reaction flask containing 800g of water while stirring, cool to 30°C, add 110g (1.01mol) of m-aminophenol, and stir to dissolve. Cool to -5°C, add dropwise a solution composed of 75.9g (1.10mol) sodium nitrite and 200g water, and the reaction is exothermic. During the dropping process, the dropping speed is controlled, so that the temperature of the system is controlled at -5°C to 5°C. After the dropwise addition, the temperature was raised to 40° C., and the temperature was kept for 2 hours. At this time, no bubbles emerged, and an aqueous solution of resorcinol was obtained. Cool the reaction solution to 15°C and keep it warm for 30 minutes. Filter, extract the filtrate with 600g*2 methyl tert-butyl ether, combine the methyl tert-butyl ether extract, wash with 100g saturated brine, and separate the layers. Concentrate the methyl tert-butyl ether layer under reduced pressure (concentrate i...

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Abstract

The invention discloses a method for preparing resorcinol. The method is characterized by comprising the following steps: adding m-aminophenol into a sulfuric acid solution, dropwisely adding a sodium nitrate water solution at -10-0 DEG C, and carrying out thermal-insulation reaction on the obtained diazonium-salt-containing reaction solution at 20-80 DEG C for 2-2.5 hours, thereby implementing decomposition of diazotization salts; and cooling the obtained decomposition reaction solution, filtering, extracting the filtrate by using an organic solvent, removing an organic solvent from the obtained extraction layer, and distilling to obtain the resorcinol. The method has the advantages of mild reaction conditions, low facility requests and the like; the technique is easy to master; and the product quality conforms to the standard requirements.

Description

technical field [0001] The invention belongs to the technical field of preparation of resorcinol compounds. Background technique [0002] Resorcinol is mainly used in rubber adhesives, synthetic resins, dyes, preservatives, medicine and analytical reagents, etc. Resorcinol is similar to phenol and cresol, and forms condensation polymers with formaldehyde, which can be used to make viscose yarn And tire cord binder for nylon, preparation of wood glue, used for bonding vinyl materials and metals, resorcinol is an intermediate of many azo dyes and fur dyes, and is also a pharmaceutical intermediate p-nitrogen Raw material of salicylic acid. Resorcinol has a bactericidal effect and can be used as a preservative, added to cosmetics and dermatological drug pastes and ointments. At present, the synthesis methods of resorcinol mainly include benzene sulfonation alkali fusion method, m-dicumyl oxidation method, and m-phenylenediamine method. Among them, the sulfonated alkali fusio...

Claims

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Application Information

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IPC IPC(8): C07C37/045C07C37/72C07C37/74C07C39/08C07C245/20
CPCC07C37/045C07C37/72C07C37/74C07C245/20C07C39/08
Inventor 王亚斌赵金浩王晖许重阳秋小龙
Owner 浙江精进药业有限公司
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