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A kind of preparation method and application of cu/al-sba-15 bimetallic composite catalyst

An al-sba-15, bimetallic technology, applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problem of difficult formation, difficult matching of metal source and silicon source hydrolysis polymerization speed, and difficult formation etc. to achieve the effects of reducing raw material costs, improving hydrothermal stability, and saving solvents

Active Publication Date: 2022-08-05
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, many researchers have used it as a carrier to carry various active components and widely used in various catalytic fields. However, there are still problems in the process of synthesizing metal-doped SBA-15. To synthesize metal-doped SBA-15 15 Mesoporous molecular sieves, the process requires strong acidity, and metals mainly exist in the form of cations under acidic conditions, so it is difficult to form metal-oxygen-silicon (M-O-Si) bonds, followed by the hydrolysis of metal sources and silicon sources The polymerization rate is not easy to match, and even SBA-15 two-dimensional hexagonal ordered pores are difficult to form. Such problems have been extensively studied by many researchers in this field.

Method used

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  • A kind of preparation method and application of cu/al-sba-15 bimetallic composite catalyst
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  • A kind of preparation method and application of cu/al-sba-15 bimetallic composite catalyst

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Experimental program
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Effect test

Embodiment 2

[0037] A preparation method of a Cu / Al-SBA-15 bimetallic composite catalyst—mixing and stirring for 6 hours, crystallization at 120° C.; continuous stirring for 4 hours, drying at 80° C. for 8 hours, and drying for 8 hours. The following are specific implementations:

[0038] Take 0.6150g Al (NO 3 ) 3 ·9H 2 O, add it into a round-bottomed flask containing 80 mL of deionized water and stir until it is completely dissolved, and adjust the pH of the solution to 2; weigh 1 g of the prepared rod-shaped SBA-15 mesoporous molecular sieve, and add a solution containing an aluminum source. The mixture was continuously stirred at room temperature for 6 hours; the obtained mixed solution was transferred to a crystallization kettle lined with polytetrafluoroethylene, and the crystallization was continued at 120 ° C for 24 hours; the crystallized mixture was mixed with deionized water and absolute ethanol. After washing, drying, and then calcining at high temperature, in the process of h...

Embodiment 3

[0040] Example 3 (catalyst dosage 3.57wt%)

[0041] The compounds p-chlorothiophenol, iodobenzene, cesium carbonate (Cs 2 CO 3 ), Cu / Al-SBA-15 bimetallic composite catalyst and solvent dimethyl sulfoxide (DMSO), the molar ratio of compound p-chlorothiophenol and iodobenzene was 4:1, and the reaction was carried out under constant temperature stirring at 120 °C The reaction was re-refluxed and monitored by TCL.

[0042] Compounds A and B are 1.6 mmol and 0.4 mmol of p-chlorothiophenol and iodobenzene respectively. The dosage of Cu / Al-SBA-15 bimetallic composite catalyst is 3.57wt%. Cs 2 CO 3 The dosage is 2 mmol, and the dosage of solvent DMSO is 4 mL; after 2 hours of reaction, TCL monitors that the compound iodobenzene reacts completely, and the reaction ends, generating C target product 5-chloro-2-(phenylthio)phenol, which is subjected to gas-mass spectrometry (GC-MS) detected a yield of 25%.

Embodiment 4

[0043] Example 4 (catalyst dosage 7.14wt%)

[0044] The compounds p-chlorothiophenol, iodobenzene, cesium carbonate (Cs 2 CO 3 ), Cu / Al-SBA-15 bimetallic composite catalyst and solvent dimethyl sulfoxide (DMSO), the molar ratio of compound p-chlorothiophenol and iodobenzene was 4:1, and the reaction was carried out under constant temperature stirring at 120 °C The reaction was re-refluxed and monitored by TCL.

[0045] Compounds A and B are 1.6 mmol and 0.4 mmol of p-chlorothiophenol and iodobenzene respectively. The dosage of Cu / Al-SBA-15 bimetallic composite catalyst is 7.14 wt%. Cs 2 CO 3 The dosage is 2 mmol, and the dosage of solvent DMSO is 4 mL; after 2 hours of reaction, TCL monitors that the compound iodobenzene reacts completely, and the reaction ends, generating C target product 5-chloro-2-(phenylthio)phenol, which is subjected to gas-mass spectrometry (GC-MS) detected a yield of 51%.

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Abstract

The invention relates to a preparation method and application of a Cu / Al-SBA-15 bimetallic composite catalyst; a rod-shaped SBA-15 mesoporous molecular sieve is used as a supported substrate, and aluminum nitrate nonahydrate (Al(NO) is used as a loading substrate. 3 ) 3 ·9H 2 O) as the aluminum source, with copper nitrate trihydrate (Cu(NO) 3 ) 2 ·3H 2 O) is the copper source, with H 2 O is the synthesis solvent. First, adjust the pH value, stirring time, crystallization temperature and crystallization time of the mixed solution of aluminum source and rod-shaped SBA-15 to prepare the first immersion product Al / SBA-15; then adjust the mixing of copper nitrate solution and Al / SBA-15 The stirring time, drying temperature and drying time of the solution were used to prepare the secondary impregnation product Cu / Al-SBA-15 bimetallic composite catalyst. The present invention is a two-step impregnation loading process, no other solvent is used in the impregnation loading process, green and environmental protection, low production cost, simple and controllable process, ordered mesopores of the catalyst, good hydrothermal stability, and easy separation for application. Recycled and reused many times.

Description

technical field [0001] The invention relates to a preparation method and application of a Cu / Al-SBA-15 bimetallic composite catalyst. Background technique [0002] SBA-15 mesoporous molecular sieve has two-dimensional hexagonal structure ordered channels, larger pore volume, higher specific surface area and thicker pore wall. In recent years, many researchers have used it as a carrier to carry various active components and are widely used in various catalysis fields, but there are still problems in the process of synthesizing metal-doped SBA-15. 15 Mesoporous molecular sieve, the process requires strong acidity, and metals mainly exist in the form of cations under acidic conditions, so the metal-oxygen-silicon (M-O-Si) bond is difficult to form, followed by the hydrolysis of metal sources and silicon sources. The polymerization speed is not easy to match, and even SBA-15 two-dimensional hexagonal structure ordered pores are difficult to form. This kind of problem has been w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/04C07C319/14C07C323/20C07C1/24C07C15/54
CPCB01J29/044C07C319/14C07C1/24C07C323/20C07C15/54
Inventor 王龙罗享豪邓任远胡为民黄年玉
Owner CHINA THREE GORGES UNIV