Preparation method of iron-containing MCM-41 molecular sieve membrane used for catalyzing phenol hydroxylation

A technology of MCM-41, catalyzing phenolic hydroxyl groups, applied in the field of mesoporous materials to achieve the effect of increasing catalytic activity

Inactive Publication Date: 2015-08-26
NANJING UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problems of separation of the catalyst and the reaction solution in the hydroxylation reaction of phenol, and provide a catalyst rich in active center iron, with uniform distribution of active centers and a high degree of mesoporous order for catalyzing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0020] Example 1: Combine 1.80g CTAB and 5.70g Na 2 SiO 3 ·9H 2 O is dissolved in water, the solution is slightly heated, after the solution is clear, it is recorded as solution A; then 0.41g of iron nitrate (Fe(NO 3 ) 3 ·9H 2 O) and 0.7g of tartaric acid dissolved in 10ml of deionized water, denoted as solution B; add solution B to solution A to form solution C (the material ratio is: silicon source: iron source: template agent: complexing agent = 1:0.05:0.25:0.25), stir vigorously for 2h at room temperature, then adjust the pH of the solution to 11 with 1mol / L dilute sulfuric acid solution, and transfer the synthesized sol to a polytetrafluoroethylene lining with a carrier aluminum sheet In the stainless steel high temperature and high pressure reactor, the first crystallization treatment, the crystallization treatment at 80 ℃ for 120 hours, and then the second crystallization treatment, the crystallization treatment at 100 ℃ for 72 hours, and finally the sample is washed, cent...

Example Embodiment

[0022] Example 2: According to the molar ratio of the materials: silicon source: iron source: template agent: complexing agent=1:0.01:0.1:0.1; the materials were weighed separately, and the iron source was selected as ferric chloride; other synthesis The steps are the same as in Example 1, and the synthesized mesoporous molecular sieve membrane is used for phenol hydroxylation (conditions are the same as in Example 1), and the catalytic reaction results are shown in Table 1.

Example Embodiment

[0023] Example 3: According to the molar ratio of each material: silicon source: iron source: template agent: complexing agent=1:0.1:0.5:0.6; the materials were weighed separately, and the iron source was selected as iron nitrate; other synthesis steps As in Example 1, the mixed solution was stirred for 4 hours, and the synthesized mesoporous molecular sieve membrane was used for phenol hydroxylation (conditions are the same as in Example 1), and the catalytic reaction results are shown in Table 1.

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Abstract

The invention relates to a preparation method of an iron-containing MCM-41 mesoporous molecular sieve membrane used in a process for preparing dihydroxybenzene through phenol hydroxylation. According to the invention, an in-situ hydrothermal synthesis method is adopted; the proportions of a silicon source, an iron source, a templating agent and a complexing agent are adjusted; and synthesis conditions are adjusted, such that the iron-containing mesoporous molecular sieve membrane with good catalytic performance is synthesized. Problems of the separation of catalyst and reaction liquid, poor reaction effect and the like are solved. The method has a good industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of an iron-containing MCM-41 mesoporous molecular sieve membrane used to catalyze phenol to produce hydroquinone, which belongs to the field of mesoporous materials. Background technique [0002] As an important chemical raw material and intermediate, hydroquinone is widely used in many fields such as spices, dyes, developers, inhibitors, medicines, pesticides and coatings. [0003] The traditional synthesis methods of hydroquinone, such as aniline oxidation method, ortho-chlorophenol hydrolysis, etc., in these methods, strong acids, strong bases, water-soluble metal ions and metal complexes are often used as catalysts, the process is complicated, and the equipment is seriously corroded , The amount of three wastes is large, and the pollution caused is quite serious. [0004] Oxidation of phenol with hydrogen peroxide has become the most important method for the synthesis of quinone due to its short synthe...

Claims

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Application Information

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IPC IPC(8): B01J29/88C07C37/60C07C39/08
CPCY02P20/52
Inventor 孔岩马红蕾席涛龙塞夫
Owner NANJING UNIV OF TECH
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