Unlock instant, AI-driven research and patent intelligence for your innovation.

Solid super acid-ionic liquid composite solid supported catalyst and preparation method thereof

A solid super acid, solid-supported catalyst technology, applied in the preparation of carboxylate, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. Reduce the specific surface area and other problems, to achieve the effect of the product can be reused, the acid strength is improved, and the preparation method is simple

Inactive Publication Date: 2014-03-12
DALIAN UNIV OF TECH
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of heteroatoms doped in these materials is relatively limited at present, mainly because too much doping will lead to the destruction of the mesoporous structure and a large decrease in specific surface area, but the acidity cannot meet the requirements if the doping amount is small. , so the acidity of this heteroatom-doped mesoporous material cannot meet the requirements of catalytic reactions

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Solid super acid-ionic liquid composite solid supported catalyst and preparation method thereof
  • Solid super acid-ionic liquid composite solid supported catalyst and preparation method thereof
  • Solid super acid-ionic liquid composite solid supported catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] I. Preparation of mesoporous silicon-zirconium carrier: 4g template agent P123 (EO 20 PO 70 EO 20 ) was dissolved in 125ml of 2mol / L HCl, stirred at 40°C to make the solution clear and transparent, then slowly added 9.346g (0.0045mol) TEOS (tetraethyl orthosilicate) dropwise, stirred for 4 hours, and then added 0.3863g (0.0009mol) Zr ( NO 3 ) 4 ·5H 2 O, stirred for 24h. Crystallized at 100°C for 48h. Take it out to cool down, adjust the pH to 8 with ammonia water, put it into an oven for crystallization at 100°C for 48 hours, vacuum filter, wash with deionized water until neutral, dry at 60°C for 12 hours, and roast at 600°C for 5 hours to obtain silicon zirconium The mesoporous carrier with a ratio of 5 is denoted as SZ-5.

[0042] II. The preparation of 1-propyl-triethoxysilyl-imidazolium chloride ionic liquid: in a three-necked flask, the same molar amount of 3-chloropropylethoxysilane and 1-methylimidazole, in N 2 Reflux at 80°C for 24h under atmosphere. ...

Embodiment 2

[0046] I. Preparation of mesoporous silicon-zirconium carrier: 4g template agent P123 (EO 20 PO 70 EO 20 ) was dissolved in 125ml of 2mol / L HCl, stirred at 40°C to make the solution clear and transparent, then slowly added 9.346g (0.0045mol) TEOS (tetraethyl orthosilicate) dropwise, stirred for 4 hours, and then added 0.4829g (0.001125mol) Zr ( NO 3 ) 4 ·5H 2 O, stirred for 24h. It was crystallized at the synthesis temperature of 100°C for 48h. Take it out to cool down, adjust the pH to 8 with ammonia water, put it into an oven for crystallization at 100°C for 48 hours, filter it with suction, wash, dry, and bake at 600°C for 5 hours to obtain a mesoporous carrier with a silicon-zirconium ratio of 4, which is denoted as SZ-4.

[0047] II. Preparation of 1-propyl-triethoxysilyl-imidazolium chloride ionic liquid: the same as the preparation method of the ionic liquid in Embodiment 1.

[0048] III. Catalyst precursor preparation: Take 1g of vacuum-dried carrier SZ-4 an...

Embodiment 3

[0051] I. Preparation of mesoporous silicon-zirconium carrier: 4g template agent P123 (EO 20 PO 70 EO 20 ) was dissolved in 125ml of 2mol / L HCl, stirred at 40°C to make the solution clear, then slowly added 9.346g (0.0045mol) TEOS (tetraethyl orthosilicate) dropwise, stirred for 4 hours, and then added 0.6439g (0.0015mol) Zr ( NO 3 ) 4 ·5H 2 O, stirred for 24h. Crystallized at a synthesis temperature of 100°C for 48h. Take it out to cool down, adjust the pH to 8 with ammonia water, put it into an oven for crystallization at 100°C for 48 hours, filter it with suction, wash, dry, and roast at 600°C for 5 hours to obtain a mesoporous carrier with a silicon-zirconium ratio of 3, which is denoted as SZ-3.

[0052] II. Preparation of 1-propyl-triethoxysilyl-imidazolium chloride ionic liquid: the same as the preparation method of the ionic liquid in Embodiment 1.

[0053] III. Catalyst precursor preparation: Take 1g of vacuum-dried carrier SZ-3 and disperse it in 30ml of et...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a preparation method and application of a mesoporous solid super acid-ionic liquid composite solid supported catalyst, belonging to the field of a preparation technology and application of the catalyst. The preparation method comprises the following steps of: preparing a mesoporous material doped with different contents of zirconium metal, immobilizing imidazolium-based ionic liquid on the surface of the mesoporous material by using a chemical bonding method, and using the ionic liquid for exchanging ions with H2SO4 to prepare the mesoporous solid super acid-ionic liquid composite solid supported catalyst. The catalyst has the advantages that the catalyst has high activity and selectivity on esterification reaction of acetic acid and ethanol at a lower temperature, a product is easy to separate and can be recycled, and the like.

Description

technical field [0001] The invention relates to a solid superacid-ionic liquid composite immobilized catalyst and a preparation method thereof, belonging to the field of catalyst preparation technology and application. Background technique [0002] As an important organic chemical intermediate, organic carboxylic acid ester has a wide range of industrial applications. Among them, ethyl acetate is widely used in the production process of acetate fiber, ethyl fiber, chlorinated rubber, vinyl resin, synthetic rubber, paint and paint. It is usually prepared by acetic acid and ethanol under acid catalysis, but the traditional liquid acid catalysts are mainly sulfuric acid, hydrofluoric acid and anhydrous aluminum trichloride, etc., which have high catalytic activity, but are highly corrosive, and the post-treatment is complicated. Serious environmental pollution and other shortcomings. Solid acid catalysts have the advantages of environmental friendliness, high selectivity, and...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/38C07C69/14C07C67/08
Inventor 纪敏罗群兴林丽利吕美横
Owner DALIAN UNIV OF TECH