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Acid-base bifunctional solid catalyst and preparation method thereof

A solid catalyst, acid-base dual function technology, used in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. The activity needs to be further improved, the yield of 5-HMF is not ideal, etc., to achieve the effect of improving catalytic reaction activity, improving regeneration performance, and enhancing thermal stability

Inactive Publication Date: 2017-01-11
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, for the multifunctional solid catalysts emerging in this research field, the catalytic activity needs to be further improved, mainly because the conversion rate of the reaction substrate is not high, the yield of 5-HMF is not ideal, and the target requirements for industrial production are still far away.

Method used

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  • Acid-base bifunctional solid catalyst and preparation method thereof
  • Acid-base bifunctional solid catalyst and preparation method thereof
  • Acid-base bifunctional solid catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Preparation of acid-base bifunctional solid catalyst

[0035] 0.2 g of dried silicon-based mesoporous molecular sieve SBA-15 was dispersed in 10 mL of n-hexane, and 1.0 g of zirconium n-propoxide was added dropwise to the mixed system under stirring. After the reaction system was hydrolyzed at 50°C for 6h, the resulting product was washed 3-5 times with distilled water, collected by centrifugation and vacuum-dried at 40°C to obtain a single-layer zirconia product (1ML-ZrO 2 @SBA-15).

[0036] 0.2g 1ML-ZrO obtained in the previous step 2 @SBA-15 was redispersed in 10mL of n-hexane, and 0.6g of zirconium n-propoxide was added dropwise to the mixed system under the condition of stirring. After the reaction system was hydrolyzed at 50°C for 6h, the resulting product was washed 3-5 times with distilled water, collected by centrifugation and vacuum-dried at 40°C to obtain a two-layer zirconia product (2ML-ZrO 2 @SBA-15).

[0037] 0.2g of 2ML-ZrO obtained in the previo...

Embodiment 2

[0054] (1) Preparation of acid-base bifunctional solid catalyst

[0055] 5.0 g of dried silicon-based mesoporous molecular sieve SBA-15 was dispersed in 300 mL of n-hexane, and 25 g of zirconium n-propoxide was added dropwise to the mixed system under stirring. After the reaction system was hydrolyzed at 80°C for 30h, the resulting product was washed 3-5 times with distilled water, collected by centrifugation and vacuum-dried at 80°C to obtain a single-layer zirconia product (1ML-ZrO 2 @SBA-15).

[0056] 5.0g 1ML-ZrO obtained in the previous step 2 @SBA-15 was redispersed in 300mL of n-hexane, and 15g of zirconium n-propoxide was added dropwise to the mixed system under stirring conditions. After the reaction system was hydrolyzed at 80°C for 30h, the resulting product was washed 3-5 times with distilled water, collected by centrifugation and vacuum-dried at 80°C to obtain a two-layer zirconia product (2ML-ZrO 2 @SBA-15).

[0057] 1.0g of 2ML-ZrO obtained in the previous s...

Embodiment 3

[0065] (1) Preparation of acid-base bifunctional solid catalyst

[0066] 10 g of dried silicon-based mesoporous molecular sieve SBA-15 was dispersed in 600 mL of n-hexane, and 58.5 g of zirconium n-propoxide was added dropwise to the mixing system under stirring. After the reaction system was hydrolyzed at 120°C for 48h, the resulting product was washed 3-5 times with distilled water, collected by centrifugation and vacuum-dried at 120°C to obtain a single-layer zirconia product (1ML-ZrO 2 @SBA-15).

[0067] 10g of 1ML-ZrO obtained in the previous step 2 @SBA-15 was redispersed in 600mL of n-hexane, and 28.5g of zirconium n-propoxide was added dropwise to the mixed system under the condition of stirring. After the reaction system was hydrolyzed at 120°C for 48h, the resulting product was washed 3-5 times with distilled water, collected by centrifugation and vacuum-dried at 120°C to obtain a SBA-15 loaded two-layer zirconia product (2ML-ZrO 2 @SBA-15).

[0068] 1.8g of 2ML-...

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Abstract

The invention belongs to the field of heterogeneous catalysts, and particularly provides an acid-base bifunctional solid catalyst and a preparation method thereof. The method comprises the steps that a silica-based mesoporous molecular sieve SBA-15 is selected as a carrier, ZrO2 / SO4<2-> type solid superacid is loaded, obtained solid superacid is subsequently grafted with an acidic -SO3H group and a basic -NH2 group through a silane coupling reaction, and the acid-base bifunctional solid catalyst is obtained. The defects that in the reaction field of preparing 5-hydroxymethylfurfural (5-HMF) from cellulose, the activity is not high, and the selectivity is poor are overcome, and the preparation method of the acid-base bifunctional heterogeneous solid catalyst with a large specific surface area is provided.

Description

technical field [0001] The invention relates to the field of solid catalysts, in particular to a solid catalyst with acid-base dual functions and high catalytic activity and a preparation method thereof. Background technique [0002] In recent years, as the development and utilization of fossil energy such as coal and oil face more and more cost and environmental problems, more and more attention has been paid to the development of new energy. In addition to solar energy, etc., bio-energy has also shown an increasingly important role. Among them, cellulose, as the most widely distributed and abundant macromolecular polysaccharide biomass resource in nature, is an ideal renewable raw material to replace traditional fossil fuels in the production of carbon-based chemicals. 5-Hydroxymethylfurfural (5-HMF) is an important fine chemical raw material, which can be further prepared into high value-added fuels, polymer materials, pharmaceutical products, etc. through oxidation, hyd...

Claims

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Application Information

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IPC IPC(8): B01J31/38C07D307/46
CPCC07D307/46B01J31/38B01J35/50B01J35/647B01J35/615
Inventor 张云雷陈瑶李春香闫永胜王凯
Owner JIANGSU UNIV
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