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Preparation method of polydivinylbenzene-ionic liquid-polyacid catalysts and application thereof

A technology of polydivinylbenzene and divinylbenzene is applied in the field of catalyst preparation to achieve the effects of high-efficiency catalytic activity and high catalytic activity

Active Publication Date: 2014-04-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, the main problem limiting the application of polyacids as homogeneous catalysts is the recovery and recycling of catalysts.

Method used

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  • Preparation method of polydivinylbenzene-ionic liquid-polyacid catalysts and application thereof
  • Preparation method of polydivinylbenzene-ionic liquid-polyacid catalysts and application thereof
  • Preparation method of polydivinylbenzene-ionic liquid-polyacid catalysts and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1. Add 2.0g of divinylbenzene (PDVB) and 0.5g of 1-vinylimidazole (VIM) to 30ml of ethyl acetate solution containing 0.08g of azobisisobutyronitrile, and stir at room temperature for 2 hours. Keep the temperature in a polytetrafluoroethylene-substrated pressure reaction vessel at a constant temperature for 32 hours in Celsius, and remove the solvent by rotary evaporation under reduced pressure after the reaction is completed to obtain PDVB-VIM;

[0021] 2. Dissolve 1g of the product of step 1 in 30ml of toluene, then add 4g of 1,3-propane sultone (PS), stir at room temperature for 10 hours, filter the product, wash with ether, and remove excess 1,3- Propane sultone was washed and dried in vacuum at 80°C for 12 hours to form PDVB-VIM-PS;

[0022] 3. Add 1.5g of the product in step 2 to 50ml of toluene solution containing 5.76g of phosphotungstic acid (HPW), stir at room temperature for 32 hours, and evaporate the solvent on a rotary evaporator to form polydivinylbenzene-...

Embodiment 2

[0024] 1. Add 2.0g divinylbenzene (PDVB) and 0.7g 4-vinylpyridine (VPY) to 30ml ethyl acetate solution containing 0.08g azobisisobutyronitrile, stir at room temperature for 3 hours, Keep the temperature in a polytetrafluoroethylene-substrated pressure reaction vessel at 100°C for 24 hours, and remove the solvent by rotary evaporation under reduced pressure after the reaction is over to obtain PDVB-VPY;

[0025] 2. Dissolve 1g of the product of step 1 in 30ml of toluene, then add 4g of 1,3-propane sultone (PS), stir at room temperature for 10 hours, filter the product, wash with ether, and remove excess 1,3- Propane sultone was washed and dried in vacuum at 60°C for 12 hours to form PDVB-VPY-PS;

[0026] 3. Add 1.5 g of the product in step 2 to 50 ml of aqueous solution containing 6.2 g of silicotungstic acid, stir at room temperature for 32 hours, and evaporate the solvent to dryness on a rotary evaporator to form polydivinylbenzene-ionic liquid-polyacid Catalyst PDVB-VPY-HPW...

Embodiment 1

[0028] The catalytic reaction is carried out in a simple glass reactor with magnetic stirring. Weigh 0.05g of the catalyst prepared in Example 1, 7.5mmol of lauric acid, and methanol solutions of different molar ratios, add them into a round bottom flask, and reflux at 65°C for 3h. Do not add catalyst, according to acid: alcohol = 1:6 to do a blank test, for comparison. Use n-hexane as a solvent, methyl tridecanoate as an internal standard, gas chromatography for quantitative analysis, and calculate the yield of the reaction.

[0029] Catalytic results such as figure 2 Shown, the productive rate of blank reaction is only 2.89%, from figure 2 It can be seen that the PDVB-VIM-PS-HPW prepared in Example 1 is used as a catalyst, and when the alcohol: the acid molar ratio reaches 6:1, the productive rate reaches 91.17%, and the catalytic effect is quite obvious; when the alcohol: the acid molar ratio reaches At 10:1 or greater, the yield is close to 99%, with no significant ch...

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Abstract

The invention discloses a preparation method of polydivinylbenzene-ionic liquid-polyacid catalysts and an application thereof, and belongs to the technical field of catalyst preparation. Through polymerization reaction, an ionic liquid is loaded on polydivinylbenzene in a covalent combination manner, and then polyacid is combined with the ionic liquid in an electrostatic interaction effect to form a heterogeneous catalyst capable of efficiently catalyzing a long-chain fatty acid esterification reaction; and the potential application is to catalyze and prepare biodiesel. The catalyst has the advantages that an earlier stage processing is not needed before using, the catalyst can be used repeatedly, reaction containers are not corroded, and the catalytic activity is high and the like.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation method and application of a polydivinylbenzene-supported ionic liquid-polyacid catalyst. This catalyst can efficiently catalyze the esterification reaction of long-chain fatty acids, and has potential application in the future to the production of biodiesel. Background technique [0002] As a functional polymer material, polydivinylbenzene (PDVB) has good adsorption and hydrophobic properties for various organic substances, and is widely used in the separation and purification of organic substances, industrial wastewater treatment, catalyst carriers, etc. According to literature reports, PDVB has a strong adsorption effect on oils and esters, and its contact angle on water molecules can exceed 150 degrees, which is a type of superhydrophobic material. [0003] Polyacid compounds are a class of multimetal oxides containing V, Mo, W and other ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/16B01J31/18C07C69/22C07C67/08C11C3/04C10L1/02
Inventor 宋宇飞李文虎
Owner BEIJING UNIV OF CHEM TECH
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