Preparation and applications of composite SBA-15 molecular sieve catalysts

A catalyst and reaction technology, applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problems of long synthesis route, large consumption of raw materials, serious environmental pollution, etc.

Inactive Publication Date: 2015-09-09
HARBIN UNIV OF COMMERCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the industrial synthesis of phenol from benzene has problems such as long synthetic routes, large consumption of raw materials, and serious environmental pollution. Therefore, it is very important to develop an environmentally friendly synthesis of phenol under mild conditions.

Method used

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  • Preparation and applications of composite SBA-15 molecular sieve catalysts
  • Preparation and applications of composite SBA-15 molecular sieve catalysts
  • Preparation and applications of composite SBA-15 molecular sieve catalysts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take the quantitative Na 2 HPO 4 ·12H 2 O was dissolved in distilled water and mixed with 10.6 g Na 2 CO 3 The aqueous solutions were mixed, stirred for a certain period of time, and 9.1 g of V was added slowly. 2 O 5 , heated to boiling, reacted for 30min, took 35.3g MoO 3 After being dissolved in distilled water, it was added to the above solution, heated at 90° C. for 30 min in a water bath, adjusted to pH value with 1:1 sulfuric acid, and cooled to room temperature with stirring. Add an appropriate amount of ether to extract and shake well, gradually add an appropriate amount of 1:1 sulfuric acid until layers appear, and the obtained red oily heteropolyether complex is in the middle layer. until it turns light yellow. Blow off the ether, dissolve the red solid in distilled water and place it in a vacuum desiccator. After the crystal film appears, put it in a refrigerator at 3°C ​​to 5°C for crystallization to obtain H 5 PMo 10 V 2 O 40 ·xH 2 O heteropoly...

Embodiment 2

[0023] The H obtained by the method of Example 1 5 PMo 10 V 2 O 40 SBA-15 molecular sieve catalyst supported by heteropoly acid, used in the reaction of benzene oxidation to phenol, with 20%, 40%, 60%, 80% H respectively 5 PMo 10 V 2 O 40 Heteropolyacids, examine different H 5 PMo 10 V 2 O 40 The effect of heteropolyacid loading on catalyst performance. The specific catalytic reaction is as follows: add benzene, 25mL glacial acetic acid and catalysts of different qualities into a 50mL three-neck flask, keep stirring, and then slowly add a certain amount of H dropwise. 2 O 2 (30%), the reaction was carried out in a water bath at a certain reaction temperature, a sample was taken every 0.5 h, and the reaction product was analyzed by high performance liquid chromatography.

[0024] The reaction products were analyzed on HPLC-Agilent1100 high performance liquid chromatography, using C8 column (4.6×150mm) type chromatographic column, programmable ultraviolet detector, N...

Embodiment 3

[0027] Prepare 60% H according to Example 1 5 PMo 10 V 2 O 40 The SBA-15 molecular sieve catalyst supported by the heteropolyacid was used to carry out the experiment of oxidizing phenol with benzene according to the catalytic reaction of Example 2. Change the reaction time to 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 6h, and investigate the effect of time on the reaction.

[0028] Reaction conditions: in benzene and H 2 O 2 The molar ratio of the catalyst was 1:1, the catalytic reaction temperature was 70 °C, the catalyst dosage was 0.20 g, and the H of the catalyst prepared by the sol-gel method 5 PMo 10 V 2 O 40 The load is 60%. The reaction results are: with the increase of reaction time, the selectivity of phenol gradually increases, and when the reaction time reaches 2h, H 5 PMo 10 V 2 O 40 The phenol selectivity of / SBA-15 catalyst reaches a maximum of 80.72%, compared to H 5 PMo 10 V 2 O 40 The selectivity of the Figure 5 ).

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Abstract

The present invention provides a class of heteropolyacid loaded mesoporous molecular sieve SBA-15 catalysts and a preparation method thereof, and applications of the catalysts in oxidation of benzene into phenol. According to the present invention, the catalyst adopts the mesoporous molecular sieve SBA-15 is adopted as the carrier, and the Keggin type heteropolyacid H5PMo10V2O40 is loaded on the mesoporous molecular sieve SBA-15 by using the sol-gel method to prepare the catalyst; and in the oxidation reaction of benzene into phenol, the loaded catalyst has characteristics of high selectivity and good catalyst recycling.

Description

technical field [0001] The invention relates to a preparation method of a heteropolyacid-supported mesoporous molecular sieve SBA-15 and its application in the oxidation of benzene to phenol. Background technique [0002] Phenol is an important organic chemical raw material, and it is the raw material for the synthesis of chemical products such as phenolic resin, bisphenol A, pentachlorophenol, salicylic acid, picric acid, caprolactam, adipic acid, phenolphthalein and ethoxyaniline. Intermediate. It is widely used in industries such as synthetic fibers, synthetic rubber, fragrances, plastics, dyes, pharmaceuticals, pesticides, coatings and oil refining. In addition, phenol can also be used directly as a chemical reagent, antiseptic and disinfectant. Especially in recent years, due to the rapid development of the automobile industry, electronic communication and construction industry, the demand for series products produced by phenol has accelerated, which has driven the in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/16B01J31/18C07C39/04C07C37/60
CPCY02P20/52Y02P20/582Y02P20/584
Inventor 刘蕊宋应金
Owner HARBIN UNIV OF COMMERCE
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