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Preparation method of supported solid acid catalyst for hydrolysis of m-phenylenediamine

A technology of solid acid catalyst and m-phenylenediamine, which is applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., and can solve the problems of high equipment material requirements, tedious follow-up treatment process, and corrosive reaction system Strong and other problems, to achieve the effect of inhibiting coking of polymerization, excellent chemical stability, and easy control of loading capacity

Active Publication Date: 2017-10-20
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional m-phenylenediamine hydrolysis method usually uses inorganic acids such as sulfuric acid, hydrochloric acid, and phosphoric acid as the acid catalyst for the hydrolysis reaction of aromatic amines. The disadvantages are large acid consumption, tedious follow-up treatment process, and strong corrosion of the reaction system, which affects the equipment material. Higher requirements, increased investment in equipment

Method used

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  • Preparation method of supported solid acid catalyst for hydrolysis of m-phenylenediamine

Examples

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Embodiment 1

[0018] Example 1: A method for preparing a supported solid acid catalyst for the hydrolysis of m-phenylenediamine, which specifically includes the following steps:

[0019] (1) Using a hydrochloric acid solution with a mass concentration of 20%, the contrast surface area is 1200m 2 / g of nutshell charcoal powder is heated and refluxed. The washed charcoal powder is washed with deionized water until the pH remains unchanged, and then added with a 20% mass concentration nitric acid solution for heating and refluxing. The heating temperature is 65°C and the reflux time is 10h , The treated activated carbon powder is washed with deionized water until the pH remains unchanged, and dried in vacuum for use;

[0020] (2) Prepare 100g of phosphotungstic acid solution with a mass concentration of 10%, add 20g of charcoal powder from the husk obtained in step (1), stir and immerse for 15h at low speed, and filter and depressurize the carbon-supported heteropolyacid catalyst after immersion Af...

Embodiment 2

[0022] Embodiment 2: A preparation method of a supported solid acid catalyst for the hydrolysis of m-phenylenediamine, which specifically includes the following steps:

[0023] (1) Using a sulfuric acid solution with a mass concentration of 40%, the contrast surface area is 1800m 2 / g of husk charcoal powder is heated and refluxed. The washed charcoal powder is washed with deionized water until the pH remains unchanged, and then 30% hydrogen peroxide is added for heating and reflux treatment. The heating temperature is 80℃, and the reflux time is 5h. The treated activated carbon powder is washed with deionized water until the pH remains unchanged, and dried in vacuum for use;

[0024] (2) Prepare 90g of phosphomolybdic acid solution with 25% mass concentration, add 35g of nutshell charcoal powder obtained by step (1), stir and immerse for 30h at low speed, after immersion, the carbon-supported heteropolyacid catalyst is filtered and decompressed After drying, it is transferred to a...

Embodiment 3

[0028] Example 3: A preparation method of a supported solid acid catalyst for the hydrolysis of m-phenylenediamine, which specifically includes the following steps:

[0029] (1) Using 30% hydrochloric acid solution, the contrast surface area is 1500m 2 / g of husk charcoal powder is heated and refluxed. The washed charcoal powder is washed with deionized water until the pH remains unchanged, and then a 30% mass concentration ammonium persulfate solution is added for heating and reflux treatment. The heating temperature is 72℃, and the reflux time For 8 hours, the treated activated carbon powder is washed with deionized water until the pH does not change, and vacuum dried for use;

[0030] (2) Prepare 200 g of phosphotungstic acid solution with a mass concentration of 15%, add about 80 g of the charcoal powder from the husk obtained in step (1), stir and immerse for 22 hours at low speed, and after the end of immersion, the carbon-supported heteropoly acid catalyst is filtered and red...

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Abstract

The invention relates to the technical field of production of m-phenylenediamine and in particular relates to a preparation method of a supported solid acid catalyst for hydrolysis of m-phenylenediamine. The preparation method of the supported solid acid catalyst for hydrolysis of m-phenylenediamine is characterized by comprising the following steps: heating, refluxing and washing activated carbon powder by adopting an acid solution, and washing with deionized water until the pH value is invariable; adding a pretreatment agent for heating and refluxing, washing the treated activated carbon powder with deionized water until the pH value is invariable, and performing vacuum drying for later use; adding heteropolyacid impregnation liquid into the activated carbon powder, filtering the carbon powder subjected to complete impregnation, performing reduced pressure drying, and curing at a high temperature, thereby obtaining the product. The method disclosed by the invention is simple in steps, the prepared catalyst is easily controllable in active ingredient capacity, high in catalytic activity, high in stability and long in service life; and the product is applied to a reaction for preparing resorcinol and m-aminophenol through hydrolysis of m-phenylenediamine, high conversion ratio and yield can be obtained, and polymerized coke and other side reactions can be effectively controlled.

Description

(1) Technical field [0001] The invention relates to the technical field of m-phenylenediamine production, in particular to a method for preparing a supported solid acid catalyst for the hydrolysis of m-phenylenediamine. (2) Background technology [0002] Resorcinol is an important fine organic chemical raw material, widely used in agriculture, dyes, coatings, medicine, plastics, rubber, electronic chemicals and other fields. At present, the main preparation methods of resorcinol are sulfonated alkali fusion method, m-dicumene oxidation method and m-phenylenediamine hydrolysis method. Compared with the first two production methods, the m-phenylenediamine hydrolysis method has been widely studied and adopted due to its convenient source of raw materials, simple process flow, mature technology and less pollution, showing a good application prospect. [0003] The traditional m-phenylenediamine hydrolysis method usually uses sulfuric acid, hydrochloric acid, phosphoric acid and other i...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J27/188B01J27/19B01J35/10C07C37/05C07C39/08
CPCC07C37/05B01J27/188B01J27/19B01J35/618B01J35/638B01J35/647C07C39/08
Inventor 丁军委于文龙于世涛刘仕伟
Owner QINGDAO UNIV OF SCI & TECH
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