Immobilized ionic liquid catalyst, and preparation method and application thereof

An ionic liquid and catalyst technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as poor stability and difficult catalyst separation, and achieve favorable dispersion, improved catalytic efficiency and recycling. efficiency, and the preparation method is simple and easy to implement

Active Publication Date: 2018-02-16
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The object of the present invention is to provide a kind of immobilized ionic liquid catalyst, catalyze methanol and trioxane to synthesize polyoxymethylene dimethyl ether with low polymerization degree with this catalyst, can solve the problem that catalyst separation is difficult, poor stability, can improve polyoxymethylene again. The reactivity and selectivity of the target product in the synthesis of dimethyl ether

Method used

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  • Immobilized ionic liquid catalyst, and preparation method and application thereof
  • Immobilized ionic liquid catalyst, and preparation method and application thereof
  • Immobilized ionic liquid catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 0.98g SBA-16, 0.5g 1-sulfonic acid butyl-3-methylimidazolium methanesulfonate, add to a single-necked flask containing 35ml methanol, N 2 The reaction was refluxed at 68° C. for 24 h under atmosphere. Remove solvent methanol by rotary evaporation, then add 4mmol octyltrimethoxysilane and 10ml dichloromethane, N 2The reaction was carried out at 40°C for 24h under the atmosphere. The reaction product was washed and vacuum-dried to obtain catalyst a.

[0034] Add 12.1448g of paraformaldehyde, 6.7303g of methanol, 0.4788g of catalyst a in a 100ml autoclave, and fill with N 2 To the pressure of 1.8MPa, slowly heated to 95 ° C, stirred for 1h. The reaction product was cooled to room temperature, and analyzed by gas chromatography for PODE 3-8 The relative percentage content is 30.48%, and the conversion rate of paraformaldehyde is 64.43%.

Embodiment 2

[0036] Weigh 1.3g SBA-16, 0.64g 1-sulfonic acid butyl-3-methylimidazolium p-toluenesulfonate, add to a single-necked flask containing 30ml methanol, N 2 The reaction was refluxed at 65° C. for 24 h under atmosphere. Rotary evaporation removes solvent methanol, then adds 5mmol dodecyltrimethoxysilane and 15ml dichloromethane, N 2 The reaction was carried out at 40°C for 24h under the atmosphere. The reaction product was washed and vacuum-dried to obtain catalyst b.

[0037] Add 11.8807g of paraformaldehyde, 6.3344g of methanol, 0.5367g of catalyst b in a 100ml autoclave, and fill with N 2 To the pressure of 1.7MPa, slowly heated to 100 ° C, stirring the reaction for 1h. The reaction product was cooled to room temperature, and analyzed by gas chromatography for PODE 3-8 The relative percentage content is 44.62%, and the conversion rate of paraformaldehyde is 82.18%.

Embodiment 3

[0039] Weigh 1.64g SBA-16, 0.71g 1-sulfonic acid butyl-3-methylimidazolium trifluoromethanesulfonate, add to a single-necked flask containing 30ml methanol, N 2 The reaction was refluxed at 65° C. for 24 h under atmosphere. Remove solvent methanol by rotary evaporation, then add 5mmol octyltrimethoxysilane and 15ml dichloromethane, N 2 The reaction was carried out at 40°C for 24h under the atmosphere. The reaction product was washed and vacuum-dried to obtain catalyst c.

[0040] Add 8.9220g of paraformaldehyde, 6.3344g of methanol, 0.4973g of catalyst c in sequence in a 100ml autoclave, and fill with N 2 To the pressure of 1.9MPa, slowly heated to 90 ° C, stirring the reaction for 0.75h. The reaction product was cooled to room temperature, and analyzed by gas chromatography for PODE 3-8 The relative percentage content is 49.95%, and the conversion rate of paraformaldehyde is 85.85%.

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Abstract

The invention discloses an immobilized ionic liquid catalyst. The immobilized ionic liquid catalyst is formed by taking a mesoporous molecular sieve SBA-16 as a carrier, taking a 1-butyl-3-methylimidazole sulfonate ionic liquid as an active component and packaging the ionic liquid in the pore cage of the SBA-16 molecular sieve, wherein the mass ratio of the 1-butyl-3-methylimidazole sulfonate ionic liquid to the mesoporous molecular sieve SBA-16 is (1-5):10. When being used for catalyzing the synthesis of polyoxymethylene dimethyl ether through a reaction of methanol and trioxymethylene, the catalyst disclosed by the invention can solve the problems of difficult catalyst separation and poor stability, can be recycled for multiple times, and can improve the reaction activity of the synthesis reaction of the polyoxymethylene dimethyl ether and the selectivity of the target product.

Description

technical field [0001] The invention belongs to the technical field of ionic liquid catalysis, and relates to a solid-supported ionic liquid catalyst, in particular to an ionic liquid catalyst for synthesizing polyoxymethylene dimethyl ether with a low polymerization degree from methanol and paraformaldehyde. Background technique [0002] With the continuous development of the economy, the number of diesel-powered vehicles continues to increase, and the demand for diesel fuel has risen sharply, while the limited resources of diesel fuel are decreasing day by day, so there is a trend of insufficient supply of diesel fuel and rising prices. In addition, the alkane molecular weight of the diesel component is relatively large, resulting in a low combustion rate and poor combustion performance, which not only increases fuel consumption, but also deepens the pollution of the exhaust gas to the air. Therefore, reducing the energy consumption and pollutant emission of diesel vehicle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C41/56C07C43/30
CPCB01J31/0285B01J31/0292B01J31/0295C07C41/56C07C43/30
Inventor 李瑞丰张朝峰李静张桐露杨耀宗
Owner TAIYUAN UNIV OF TECH
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