Carbon-based solid acid catalyst and preparation method thereof

A carbon-based solid acid and catalyst technology, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as poor dispersion, large catalyst particles, and full contact between unfavorable reactants and catalytic active centers and other problems, to achieve the effect of good dispersibility, strong surface hydrophobicity and good dispersibility

Inactive Publication Date: 2011-06-01
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods are direct carbonization of raw materials, resulting in large catalyst particles and poor dispersion in the liquid phase reaction system, which is not conducive to full contact between reactants and catalytic active centers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1, preparation of carbon-based solid acid catalyst and its catalytic effect in catalytic esterification reaction

[0028] 1) Put 9g of alumina in an aqueous sucrose solution containing 2.7g of sucrose (37.5% by mass of sucrose), stir and let stand for 45 minutes, evaporate to dryness in a water bath at 80°C to obtain a solid powder. The obtained solid powder was carbonized at 600° C. for 1 hour under the protection of nitrogen to obtain 9.3 g of black solid powder, namely carbon / alumina composite;

[0029] 2) Take 0.22g of p-aminobenzenesulfonic acid, dissolve it with 4ml of hydrochloric acid (1mol / L) and 30ml of deionized water, and place it in an ice-water bath at 0°C, then add 88mg of sodium nitrite, stir and let stand for 15 minutes Make it react fully, obtain the clear solution that contains 0.22g benzenesulfonic acid diazonium salt;

[0030] Take 6.7g of the black solid powder in step 1), add 40ml of deionized water, and place it in an ice-water bath a...

Embodiment 2

[0033] Embodiment 2, preparation of carbon-based solid acid catalyst and its catalytic effect in catalytic esterification reaction

[0034] 1) Put 6 g of titanium oxide in an aqueous sucrose solution containing 1.8 g of sucrose (the mass percentage of sucrose is 37.5%), stir and let stand for 45 minutes, evaporate to dryness in a water bath at 80° C. to obtain a solid powder. The obtained solid powder was carbonized at 500°C under the protection of nitrogen for 0.5 hours to obtain 6.2 g of black solid powder, namely carbon / titanium oxide composite;

[0035] The obtained 3g of carbon / titanium oxide composite was again placed in an aqueous sucrose solution (37.5% by mass of sucrose) containing 0.9g of sucrose, stirred and allowed to stand for 45 minutes, evaporated to dryness in a water bath at 80°C to obtain a solid powder. The obtained solid powder was carbonized at 500°C under the protection of nitrogen for 0.5 hours to obtain a black solid powder which is 3.1 g of carbon / tit...

Embodiment 3

[0039] Embodiment 3, preparation of carbon-based solid acid catalyst and its catalytic effect in catalytic esterification reaction

[0040] 1) Put 9g of silicon dioxide in an aqueous sucrose solution containing 2.7g of sucrose (37.5% by mass of sucrose), stir and let stand for 30 minutes, evaporate to dryness in a water bath at 80°C to obtain a solid powder. The obtained solid powder was carbonized at 800°C under the protection of nitrogen for 0.5 hours to obtain 9.3 g of black solid powder, namely carbon / silicon oxide composite;

[0041] 2) Take 6.7g of the black solid powder in step 1), add 40ml of deionized water, and place it in an ice-water bath at 3°C; add a clear solution containing 0.22g of benzenesulfonic acid diazonium salt (benzenesulfonic acid diazonium salt) under electromagnetic stirring The preparation method is the same as step 2 in Example 1) wherein the mass ratio of the carbon / alumina composite to benzenesulfonic acid diazonium salt is 31: 1), after continui...

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Abstract

The invention provides a carbon-based solid acid catalyst and a preparation method thereof. The method comprises the following steps of: 1) putting a metal oxide into organic matter aqueous solution for soaking, drying by distillation and carbonizing so as to obtain a carbon/oxide compound; 2) performing a sulfonation reaction on the carbon/oxide compound so as to obtain a sulfonated carbon/oxidecompound; and 3) reacting the sulfonated carbon/oxide compound with acid or alkali so as to obtain the carbon-based solid acid catalyst. The carbon-based solid acid catalyst prepared by the method has high dispersibility and hydrophobicity in a liquid phase reaction system and high catalytic activity in an esterification reaction of oleic acid and methanol.

Description

technical field [0001] The invention relates to a carbon-based solid acid catalyst and a preparation method thereof, belonging to the field of solid catalysts. Background technique [0002] Carbon-based solid acid catalysts have chemical inertness, surface hydrophobicity, good mechanical stability and thermal stability, and are ideal catalysts for liquid-phase reaction systems. [0003] Carbon-based solid acid catalysts were first proposed by Japanese scholar Hara et al. (Nature, 438, 178). They directly carbonized sugar compounds such as sucrose at high temperature, and then sulfonated them with concentrated sulfuric acid to obtain an amorphous carbon catalyst with sulfonic acid groups. This catalyst has good catalytic activity in liquid-phase reactions such as esterification, especially in the esterification of long-chain fatty acids involved in biodiesel production. 15 Higher catalytic activity. [0004] Chinese patent (publication number: CN1899691 A) discloses a prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C67/08C07C69/58
Inventor 朱月香耿靓王羽董会隗罡谢有畅
Owner PEKING UNIV
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