Preparation method of attapulgite/polymerized ionic liquid composite catalyst

A technology for polymerizing ionic liquids and attapulgite clays, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. Requirements and other issues, to achieve the effect of improved catalytic esterification efficiency, low preparation cost, and reduced material cost

Active Publication Date: 2015-03-11
常熟紫金知识产权服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this patent (ZL200710308594.2), there is only one ionic liquid at a grafting site on the surface of attapulgite, which does not meet the strong acidic requirements of the catalytic esterification reaction, and the ionic liquid selected is imidazolium chloride, It belongs to non-strongly acidic ionic liquid, the purpose is mainly to increase the compatibility of attapulgite with various organic solvents, not as a catalyst for esterification reaction

Method used

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  • Preparation method of attapulgite/polymerized ionic liquid composite catalyst
  • Preparation method of attapulgite/polymerized ionic liquid composite catalyst
  • Preparation method of attapulgite/polymerized ionic liquid composite catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1: prepare composite catalyst according to the following steps:

[0029] ①In a 500mL beaker, 8.0g of attapulgite clay was dispersed in 300mL of deionized water, and ultrasonically treated at room temperature at 50Hz for 6 h; the supernatant was centrifuged, and the obtained solid was dried at 105 °C to constant weight , crushed to 200 mesh; soak the crushed attapulgite clay in 1.5 mol / L hydrochloric acid aqueous solution at room temperature for 8 h, and then wash it with deionized water until neutral; centrifuge to separate the solid matter, and put the solid matter in Vacuum-dried at 50°C for 48 h, crushed through 200 mesh to obtain about 3.5 g of purified attapulgite clay (1);

[0030]②Put 3.0 g of purified attapulgite clay in a 250 mL flask, add 1.0 mL of distilled water and 50.0 mL of toluene successively, and drop in 1.0 mL of γ-(methacryloyloxy)propyltrimethoxysilane under magnetic stirring. React in ultrasonic waves at 30°C for 30 minutes; react in a ...

Embodiment 2

[0033] Embodiment 2: prepare composite catalyst according to the following steps:

[0034] ①In a 500mL beaker, 8.0g of attapulgite clay was dispersed in 300mL of deionized water, and ultrasonically treated at room temperature at 50Hz for 6 h; the supernatant was centrifuged, and the obtained solid was dried at 105 °C to constant weight , crushed to 200 mesh; soak the crushed attapulgite clay in 1.5 mol / L hydrochloric acid aqueous solution at room temperature for 8 h, and then wash it with deionized water until neutral; centrifuge to separate the solid matter, and put the solid matter in Vacuum-dried at 50°C for 48 h, crushed through 200 mesh to obtain about 3.5 g of purified attapulgite clay (1);

[0035] ②Put 3.0 g of purified attapulgite clay in a 250 mL flask, add 1.5 mL of distilled water and 100.0 mL of toluene successively, and drop in 3.0 mL of γ-(methacryloyloxy)propyltrimethoxysilane under magnetic stirring. React in ultrasonic waves at 50°C for 50 minutes; react in ...

Embodiment 3

[0038] Embodiment 3: prepare composite catalyst according to the following steps:

[0039] ①In a 500mL beaker, 8.0g of attapulgite clay was dispersed in 300mL of deionized water, and ultrasonically treated at room temperature at 50Hz for 6 h; the supernatant was centrifuged, and the obtained solid was dried at 105 °C to constant weight , crushed to 200 mesh; soak the crushed attapulgite clay in 1.5 mol / L hydrochloric acid aqueous solution at room temperature for 8 h, and then wash it with deionized water until neutral; centrifuge to separate the solid matter, and put the solid matter in Vacuum-dried at 50°C for 48 h, crushed through 200 mesh to obtain about 3.5 g of purified attapulgite clay (1);

[0040] ②Put 3.0 g of purified attapulgite clay in a 250 mL flask, add 1.0 mL of distilled water and 50.0 mL of toluene successively, add 1.0 mL of vinyltriethoxysilane dropwise under magnetic stirring, and react in ultrasonic waves at 30°C for 30 Minutes; reacted for 3 hours in a m...

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Abstract

The invention discloses a preparation method of an attapulgite/polymerized ionic liquid composite catalyst for esterification reactions. The preparation method comprises the following steps: carrying out reactions between a silane coupling agent containing double bonds and attapulgite to obtain modified attapulgite with vinyl active functional groups on the surface; because modified attapulgite can be polymerized with the strong acidic ionic liquid monomers under the protection of inert gas, subjecting the modified attapulgite to graft polymerization through a solution polymerization method so as to obtain the attapulgite/polymerized ionic liquid composite catalyst with high density strong acid sites. The provided preparation method has the advantages of low raw material cost, low production cost, and wide application prospect. The composite catalyst has an excellent catalytic activity on esterification reactions. In the esterification reactions of glycerol trioleate and methanol, the oleic acid conversion rate can reach 90% or more in the presence of the provided composite catalyst. Compared to the catalyst made of pure ionic liquid, the using amount of ionic liquid is reduced by 70% or more, and the oleic acid conversion rate is reduced by 7% or less.

Description

technical field [0001] The invention relates to a method for preparing an attapulgite clay / polymerized ionic liquid composite catalyst, in particular to a method for polymerizing and immobilizing a strongly acidic double bond-containing ionic liquid on the surface of attapulgite clay to obtain a functional composite material with catalytic esterification performance method. Background technique [0002] Biodiesel is a long-chain fatty acid methyl ester produced by transesterification of animal and vegetable oils and methanol. It is a high-quality substitute for petroleum diesel. At present, its main industrial preparation method is the transesterification process, and most of the catalysts use strong acid and strong alkali. There are problems such as serious equipment corrosion, complicated subsequent separation procedures, and large amounts of industrial wastewater and waste residues. As a new type of environment-friendly liquid catalyst, ionic liquid has the characteristi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/10C08F292/00
Inventor 李梅生赵宜江周守勇张文裴宇航褚效中薛爱莲
Owner 常熟紫金知识产权服务有限公司
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