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Preparation method of resorcinol

A technology of resorcinol and aminophenol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of low yield of diazotization reaction products, achieve less impurities, low risk factor, The simple effect of the three waste treatment process

Pending Publication Date: 2020-08-28
INNER MONGOLIA SHENG TANG INT MONGOLIAN MEDICINE RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process does not require high temperature and high pressure conditions, and is suitable for small-scale production of pharmaceutical companies; but the yield of diazotization reaction products is low

Method used

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  • Preparation method of resorcinol
  • Preparation method of resorcinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0103] (1) Preparation of m-aminophenol diazonium salt

[0104] Add water in the diazotization reaction tank, under stirring, slowly add concentrated sulfuric acid, control the temperature below 80°C, and prepare a sulfuric acid solution with a concentration of 30wt%. The resulting sulfuric acid solution was cooled to 25 °C. Add m-aminophenol thereto then, m-aminophenol: the vitriol oil: the mol ratio of sodium nitrite is 1:2.5:1.05. Stir for 15 minutes to dissolve m-aminophenol to form a mixed solution containing water, sulfuric acid and m-aminophenol. Then the mixed solution was cooled to -8°C for use.

[0105] Enter water in another preparation tank and add NaNO 2 , prepare 25wt% sodium nitrite aqueous solution. The sodium nitrite aqueous solution was cooled to 0°C.

[0106] The sodium nitrite aqueous solution of cooling is all dropped in the diazotization reaction tank, mixes with the above-mentioned cooling mixed solution, forms the diazotization reaction liquid, car...

Embodiment 2

[0131] (1) Preparation of m-aminophenol diazonium salt

[0132] Add water in the diazotization reaction tank, under stirring, slowly add concentrated sulfuric acid, control the temperature below 80°C, and prepare a sulfuric acid solution with a concentration of 30wt%. The resulting sulfuric acid solution was cooled to 25 °C. Then add m-aminophenol wherein, m-aminophenol: the vitriol oil: the mol ratio of sodium nitrite is 0.5:2:0.5. Stir for 15 minutes to dissolve m-aminophenol to form a mixed solution containing water, sulfuric acid and m-aminophenol. Then the mixed solution was cooled to -8°C for use.

[0133] Enter water in another preparation tank and add NaNO 2 , prepare 25wt% sodium nitrite aqueous solution. The sodium nitrite aqueous solution was cooled to 0°C.

[0134] The sodium nitrite aqueous solution of cooling is all dropped in the diazotization reaction tank, mixes with the above-mentioned cooling mixed solution, forms the diazotization reaction liquid, ca...

Embodiment 3

[0159] (1) Preparation of m-aminophenol diazonium salt

[0160] Add water in the diazotization reaction tank, under stirring, slowly add concentrated sulfuric acid, control the temperature below 80°C, and prepare a sulfuric acid solution with a concentration of 30wt%. The resulting sulfuric acid solution was cooled to 25 °C. Add m-aminophenol thereto then, m-aminophenol: the vitriol oil: the mol ratio of sodium nitrite is 1.5:3:1.5. Stir for 15 minutes to dissolve m-aminophenol to form a mixed solution containing water, sulfuric acid and m-aminophenol. Then the mixed solution was cooled to -8°C for use.

[0161] Enter water in another preparation tank and add NaNO 2 , prepare 25wt% sodium nitrite aqueous solution. The sodium nitrite aqueous solution was cooled to 0°C.

[0162] The sodium nitrite aqueous solution of cooling is all dropped in the diazotization reaction tank, mixes with the above-mentioned cooling mixed solution, forms the diazotization reaction liquid, ca...

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Abstract

The invention belongs to the field of chemical engineering, and particularly relates to a preparation method of resorcinol, which comprises: (1) carrying out a diazotization reaction on m-aminophenoland a sodium nitrite solution in a dilute solution of concentrated sulfuric acid to generate m-aminophenol diazonium salt, with the diazotization reaction temperature being 0 DEG C or below; (2) carrying out a hydrolysis reaction on the m-aminophenol diazonium salt in the presence of an organic solvent and water to obtain a resorcinol crude product, with the volume ratio of the water to the organic solvent being (0.5-1.5):(4-6); (3) carrying out post-treatment on the resorcinol crude product to obtain a product resorcinol, wherein the post-treatment step sequentially comprises: (i) an extraction stage; (ii) a vacuum distillation stage; (iii) a pickling stage; and (iv) refining, washing and drying stages. By using the method disclosed by the invention, the resorcinol yield can be greatly improved.

Description

technical field [0001] The disclosure belongs to the field of chemical industry, in particular to a method for preparing resorcinol. Background technique [0002] Resorcinol is a very important fine chemical raw material. Resorcinol and its related derivatives play an important role in the pharmaceutical industry, dye industry, plastic industry, rubber industry, chemicals and other industries. Various types of dyes can be synthesized from resorcinol, such as widely used azo dyes and fluorescent dyes; m-methyl adhesive resin synthesized from resorcinol can be used as an adhesive to bond ceramics, plastics, rubber, light metals , and textile fibers, wood and other materials; resorcinol can prepare a variety of drugs in the pharmaceutical and pesticide industries, such as anthelmintics, antiseptics, and drugs for treating tuberculosis; resorcinol has a certain bactericidal effect and can treat Dermatosis with fungal infections or as an intestinal disinfectant; also added to co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/045C07C39/08C07C37/70C07C245/20
CPCC07C37/045C07C245/20C07C37/685C07C39/08
Inventor 田志杰刘卫东
Owner INNER MONGOLIA SHENG TANG INT MONGOLIAN MEDICINE RES INST CO LTD
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