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Preparation method of attapulgite-based solid acid catalyst for vegetable fat epoxidation

A technology of solid acid catalyst and vegetable oil, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, and fatty acid production. The effect of stability

Active Publication Date: 2014-03-26
盱眙凹土能源环保材料研发中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because peroxyphosphotungstic acid (salt) is easily soluble in water and other reaction systems where polar organic substances exist, it is difficult to recycle, resulting in high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Fully stir 10 g of attapulgite, 200 g of water, and 1 g of sodium hexametaphosphate, soak for 24 h; fully stir the soaked suspension at 80°C for 120 min, let it stand for 0.5 h, and absorb it by siphon method The supernatant is 10 cm; add water to the same position, repeat the above operations of settling, standing, and absorbing the supernatant; put the extracted supernatant in an oven to dry, crush, and pass through a 200-mesh sieve to obtain purified attapulgite ; Mix 5 g of the above-mentioned purified attapulgite, 1 g of acid and 15 ml of water, stir at 30°C for 180 min, filter, dry, grind, and pass through a 200-mesh sieve to obtain acid-modified attapulgite; Take 3 g of acid-modified attapulgite, heat it at 200°C for two hours, and then add 1.5 g of N-( β -Aminoethyl)- gamma -Aminopropyltrimethoxysilane, 98.5 g toluene, reflux for 24 hours, filter, grind, pass through a 200-mesh sieve, and vacuum-dry at 80°C for 3 hours to obtain organically modified attapul...

Embodiment 2

[0028] (1) Fully stir 15 g of attapulgite, 200 g of water, and 1 g of sodium hexametaphosphate, soak for 24 h; fully stir the soaked suspension at 80°C for 60 min, let it stand for 0.5 h, and absorb it by siphon method The supernatant is 10 cm; add water to the same position, repeat the above operations of settling, standing, and absorbing the supernatant; put the extracted supernatant in an oven to dry, crush, and pass through a 200-mesh sieve to obtain purified attapulgite ; Mix 10 g of the above-mentioned purified attapulgite, 5 g of acid and 50 ml of water, stir at a constant temperature of 60 ° C for 30 min, then filter, dry, grind, and pass through a 200-mesh sieve to obtain acid-modified attapulgite; Weigh 3 g of acid-modified attapulgite, keep it warm at 200°C for two hours, then add 8 g of γ-aminopropyltriethoxysilane and 92 g of toluene, reflux for 24 hours, filter, grind, pass through a 200-mesh sieve, and Vacuum drying at 80°C for 6 h to obtain organically modified...

Embodiment 3

[0032] (1) Fully stir 20 g of attapulgite, 100 g of water, and 0.1 g of sodium hexametaphosphate, and soak for 24 h; stir the soaked suspension at 60°C for 90 min while ultrasonically oscillating, let it stand for 0.5 h, and siphon Absorb the supernatant 10 cm by the method; add water to the same position, repeat the above operations of settling, standing, and absorbing the supernatant; put the extracted supernatant in an oven to dry, crush, and pass through a 200-mesh sieve to obtain purified concave-convex Attapulgite: Mix 10 g of the above-mentioned purified attapulgite, 2 g of acid and 50 ml of water, stir at 90°C for 180 min, filter, dry, grind, and pass through a 200-mesh sieve to obtain acid-modified attapulgite ; Weigh 3g of acid-modified attapulgite, heat at 200°C for two hours, add 4 g of cetyltrimethylammonium chloride, 96 g of toluene, reflux for 24 hours, filter, grind, pass through a 200-mesh sieve, and put in 80 ℃ vacuum drying for 3 h to obtain organically modi...

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Abstract

The invention discloses a preparation method of an attapulgite-based solid acid catalyst for vegetable fat epoxidation. The preparation method comprises the steps of synthesizing phosphotungstic acid peroxide serving as a catalyst for fat epoxidation; then performing purification, acid modification and organic modification on attapulgite; and finally, loading the phosphotungstic acid peroxide on the organically modified attapulgite serving as a carrier to obtain the load type solid acid catalyst. According to the preparation method, the performance of the phosphotungstic acid peroxide is improved, the repeated use of the phosphotungstic acid peroxide is realized, the application range of the attapulgite is expanded, and the additional value of the attapulgite is increased; the attapulgite-based solid acid catalyst has the characteristics of easiness in separation of the catalyst from products, zero pollution, no corrosion to equipment, simplicity in post-treatment of the products, reutilization, simple regeneration process and the like.

Description

technical field [0001] The invention relates to a solid acid catalyst used in the epoxidation reaction system of vegetable oils, in particular to a method for preparing organically modified attapulgite loaded peroxyphosphotungstic acid, which belongs to the utilization of attapulgite and the fixation of peroxyphosphotungstic acid technology field. Background technique [0002] Epoxy vegetable oil is a non-toxic and environmentally friendly plasticizer that was used earlier. It has very good plasticizing and thermal stabilization effects. It is widely used in plastics, coatings, new polymer materials, rubber and other industrial fields. It is an American drug The only additive approved by the Authority for use in food packaging materials. Epoxy vegetable oil is mainly prepared from vegetable oil through epoxidation reaction, and the preparation methods are mainly divided into solvent method and solvent-free method. The solvent method has disadvantages such as difficulty in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188C11C3/00
Inventor 陈新德张海荣杨娟杨会娟熊莲郭海军黄超林晓清
Owner 盱眙凹土能源环保材料研发中心
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