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Immobilized ionic liquid catalyst, and preparation method and application thereof

A technology of ionic liquid and acidic ionic liquid, which is applied in the field of catalytic synthesis of biodiesel, can solve the problems of weak acidity or alkalinity, limited application, and no catalytic activity, etc., and achieve high mass transfer rate, high catalytic activity, and good heat transfer performance Effect

Inactive Publication Date: 2016-06-08
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mesoporous molecular sieve itself has very weak acidity or alkalinity, and has almost no catalytic activity, which greatly limits its application in research fields and industries.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Dissolve 4.0 g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123, Mw=5800) in 80 mL of H 2 O, add dropwise 2mL 2mol / L HCl solution. Add 0.8g Fe(NO 3 ) 3 9H 2 O and 10g of tetraethyl orthosilicate, aged at 100°C for 24h. After filtering, washing, drying, and roasting at 500°C for 8h, 3.35g of Fe-SBA-15 was obtained, wherein the mass fraction of Fe in Fe-SBA-15 was 3.6%.

[0022] Weigh 2.2mmol ionic liquid 1-(3-sulfopropyl)-3-trimethoxysilylpropyl-imidazole dihydrogen phosphate and 3gFe-SBA-15 into 50mL toluene, N 2 Reflux at 120°C for 24h under protection. After suction filtration, washing and vacuum drying, 3.59 g of immobilized ionic liquid catalyst was obtained, wherein the immobilized amount of acidic ionic liquid was 0.5 mmol / g Fe-SBA-15.

[0023] Add 0.1 mol of oleic acid and 0.8 mol of methanol into a three-necked flask, add 0.71 g of immobilized ionic liquid catalyst, stir and react at a constant temperature at 70°C for 4...

Embodiment 2

[0025] Dissolve 4.0 g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123, Mw=5800) in 120 mL of H 2 O, add dropwise 1.5mL 2mol / L HCl solution. Add 0.4g Fe(NO 3 ) 3 9H 2 O and 40g tetraethyl orthosilicate, aged at 80°C for 48h. After filtering, washing, drying, and roasting at 600°C for 6h, 13.28g of Fe-SBA-15 was obtained, wherein the mass fraction of Fe in Fe-SBA-15 was 0.5%.

[0026] Weigh 4.3mmol ionic liquid 1-(3-sulfonic acid butyl)-3-trimethoxysilylpropyl-imidazolium bisulfate and 2gFe-SBA-15 and join in containing 60mL toluene, N 2 Reflux at 100°C for 48h under protection. After suction filtration, washing and vacuum drying, 2.76 g of immobilized ionic liquid catalyst was obtained, wherein the immobilized amount of acidic ionic liquid was 1.5 mmol / g.

[0027] Add 0.1 mol of oleic acid and 0.2 mol of butanol into a three-necked flask, add 1.42 g of immobilized ionic liquid catalyst, stir and react at a constant temperature of 100°...

Embodiment 3

[0029] Dissolve 4.0 g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123, Mw=5800) in 100 mL of H 2 In O, add 2.5mL of 1mol / L HCl solution dropwise. Add 0.6g Fe(NO 3 ) 3 9H 2 O and 15g tetraethyl orthosilicate, aged at 90°C for 36h. After filtering, washing, drying, and roasting at 500°C for 8h, 5.24g of Fe-SBA-15 was obtained, wherein the mass fraction of Fe in Fe-SBA-15 was 1.9%.

[0030] Weigh 4.1mmol ionic liquid 1-(3-sulfopropyl)-3-triethoxysilylpropyl-imidazole bisulfate and 4gFe-SBA-15 into 80mL toluene, N 2Reflux at 110°C for 36h under protection. After suction filtration, washing and vacuum drying, 5.28 g of immobilized ionic liquid catalyst was obtained, wherein the immobilized amount of acidic ionic liquid was 0.9 mmol / g.

[0031] Add 0.1mol oleic acid and 0.6mol ethanol into a three-necked flask, add 2.84g of immobilized ionic liquid catalyst, stir and react at a constant temperature at 90°C for 4 hours, the conversion rate ...

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PUM

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Abstract

The invention discloses an immobilized ionic liquid catalyst, and a preparation method and an application thereof. The method is characterized in that an acidic ionic liquid is immobilized to the surface of a Fe-doped meso-porous material SBA-15 which is Fe-SBA-15 through a bonding grafting technology; the immobilization capacity of the acidic ionic liquid on the Fe-SBA-15 is 0.5-1.5mmol / g; and the doping mass fraction of Fe in the Fe-SBA-15 is 0.5-3.6%. The prepared catalyst simultaneously has Lewis acidity and Bronsted acidity. The catalyst has the advantages of high catalysis activity, low corrosion, mild reaction conditions, easy separation and recovery, and reusability in a reaction for synthesizing biodiesel through esterifying oleic acid and short chain alcohol.

Description

technical field [0001] The invention relates to a solid-supported ionic liquid catalyst, a preparation method and application thereof, and belongs to the field of catalytic biodiesel synthesis. Background technique [0002] With the rapid development of the national economy, petrochemical energy is increasingly exhausted, and the future development of human beings has been severely tested. The excessive use of petrochemical resources has caused serious environmental pollution problems. It has become an inevitable trend to develop renewable energy and resources to replace the gradually depleted petrochemical resources. As a renewable energy source, biodiesel has the advantages of high energy density, high cetane number, biodegradability, less pollutant emission, and renewable raw materials, so it is highly valued by countries all over the world. [0003] Currently, there are two ways to synthesize biodiesel, transesterification and esterification. The transesterification me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J29/035C07C67/08C07C69/58
CPCC07C67/08B01J29/0356B01J31/0292B01J2231/49C07C69/58Y02E50/10
Inventor 管国锋万辉王磊张林
Owner NANJING UNIV OF TECH
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