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Process of producing resorcinol by hydrolyzing m-phenylenediamine

A technology of m-phenylenediamine and resorcinol, which is applied in the field of resorcinol preparation, can solve the problems of oxidation, complex extraction process, lengthy production process, and low environmental friendliness, so as to reduce the generation of coke, The effect of high product yield and low environmental friendliness

Active Publication Date: 2014-06-11
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The sulfonation method uses benzene and sulfuric acid as raw materials, and the process includes steps such as sulfonation, neutralization, alkali fusion, and acidification. Strong alkali (such as sodium hydroxide) produces a large amount of inorganic salts (such as sodium sulfate, sodium sulfite) and waste liquid at the same time, and the degree of environmental friendliness is low; while the oxidation method is to first oxidize m-dicumyl into diperoxide dihydroperoxide Cumene is decomposed under acidic conditions to obtain resorcinol and by-product acetone. This method produces very little waste water and waste gas, less pollution, and lower cost, but the technical requirements are relatively high. Oxidation, extraction The process is relatively complicated, and at the same time restricted by the raw material of m-dicumene, industrial production has not yet achieved a breakthrough

Method used

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  • Process of producing resorcinol by hydrolyzing m-phenylenediamine
  • Process of producing resorcinol by hydrolyzing m-phenylenediamine

Examples

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Effect test

Embodiment 1

[0023] In a 5L autoclave equipped with stirring (heated by an electric heating coil), add 216.0g m-phenylenediamine, 350.0g hydrochloric acid (concentration 30%), 2200g water, 27.94g SO 4 2- / ZrO 2 -TiO 2 , The temperature of the feed liquid does not exceed 80°C. Stir for 30 minutes after the addition to make the materials evenly mixed. After airtight, heat to 200°C, pressure 1.8MPa, heat preservation reaction for 10 hours, after the reaction, cool down to room temperature 30°C; take out the reaction solution, filter, extract 4 times with 250.0g ether, distill off the solvent to obtain 175.0g of crude product, content It is 95.50%, obtains product 162.0g through distillation under 1.8KPa, and content is 99.38%.

Embodiment 2

[0025] In a 5L autoclave equipped with stirring (heated by an electric heating coil), add 220.8g m-phenylenediamine, 368.0g sulfuric acid (concentration 98%), 2600g water, 354.31g SO 4 2- / ZrO 2 -TiO 2 , The temperature of the feed liquid does not exceed 80°C. Stir for 30 minutes after the addition to make the materials evenly mixed. After airtight, heat to 220°C, pressure is 2.2MPa, heat preservation reaction for 8 hours, after the reaction, cool down to room temperature 30°C; take out the reaction solution, filter, extract 4 times with 400g ethyl acetate, distill off the solvent to obtain 185.0g of crude product, The content is 95.30%, and the product 178.0g is obtained through distillation at 2.0KPa, and the content is 99.40%.

Embodiment 3

[0027] In a 5L autoclave equipped with stirring (heated by an electric heating coil), add 426.0g m-phenylenediamine, 240.0g hydrochloric acid (concentration 30%), 2600g water, 40.0g SO 4 2- / TiO 2 -SnO 2 , The temperature of the feed liquid does not exceed 80°C. Stir for 30 minutes after the addition to make the materials evenly mixed. After airtight, heat to 200°C, pressure is 2MPa, heat preservation reaction for 4 hours, after the reaction, cool down to room temperature 30°C; take out the reaction solution, filter, extract 4 times with 500g isobutanol, distill off the solvent to obtain 295.0g of crude product, content It is 95.25%, obtains 281.0g of product through distillation at 1.9KPa, and content is 99.50%.

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Abstract

The invention relates to a process of producing resorcinol by hydrolyzing m-phenylenediamine. The process comprises the following steps: 1) adding m-phenylenediamine, an acid catalyst, a solid superacid catalyst and water in proportion into a high pressure hydrolysis reaction kettle, and uniformly mixing to obtain a mixed reaction liquid; 2) heating the reactor to hydrolyze m-phenylenediamine to obtain a resorcinol hydrolyzing reaction liquid; 3) carrying out filtration and solvent extraction on the hydrolyzing reaction liquid to obtain a resorcinol coarse product; and 4) carrying out reduced pressure distillation on the resorcinol coarse product to obtain a resorcinol finished product. The process provided by the invention is less in pollution, less in wastewater discharge, easy to control process condition and high in product yield.

Description

technical field [0001] The invention relates to a process for preparing resorcinol, more specifically, the invention relates to a method for preparing resorcinol by hydrolyzing m-phenylenediamine as a raw material. Background technique [0002] Resorcinol is commonly known as Resoxin, also known as 1,3-benzenediol, 1,3-dihydroxybenzene, etc. As an important organic intermediate, resorcinol is used in the fields of pesticides, dyes, paints, medicines, plastics, rubber, electronic chemicals, etc., and is mainly used in the preparation of adhesives for tire cords and adhesive resins for synthetic rubber. , high-performance adhesives for wood plywood, synthetic benzophenone UV absorbers, m-aminophenol, as preservatives, etc. At present, the industrialized synthesis of resorcinol mainly includes the sulfonation alkali fusion method using benzene as a raw material, and the oxidation method using m-dicumene as a raw material. [0003] 1. Benzene sulfonation alkali fusion method ...

Claims

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Application Information

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IPC IPC(8): C07C39/08C07C37/05
CPCC07C37/05C07C39/08
Inventor 陈苏汤文岐周振方张强
Owner NANJING UNIV OF TECH
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