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Preparation method of modified solid acid catalyst and catalyst prepared by same

A solid acid catalyst and catalyst technology, applied in the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., can solve acid residues, increase esterification activity, and temperature sensitivity limits the space for esterification activity improvement, etc. problem, to achieve high esterification catalytic activity and water resistance improvement

Active Publication Date: 2012-04-25
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Strong acids and strong bases in the esterification catalysts currently used in industrial applications have good esterification activity, but we cannot ignore the pollution of strong acids and strong bases to the environment and the destructiveness to the components of bio-oil fuels
Ion exchange resin has certain esterification activity, but its sensitivity to temperature limits the room for improvement of esterification activity
Solid strong base catalyst has the characteristics of easy separation, but the esterification activity needs to be further improved, and there are still acid residue problems that need to be solved

Method used

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  • Preparation method of modified solid acid catalyst and catalyst prepared by same
  • Preparation method of modified solid acid catalyst and catalyst prepared by same
  • Preparation method of modified solid acid catalyst and catalyst prepared by same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Take 25.58g of tetra-n-butyl titanate and 20ml of ethanol in a 250ml beaker and stir evenly; take 20ml of ethanol, 1.04g of concentrated sulfuric acid and 4ml of distilled water, mix them evenly and put them in a separatory funnel, quickly drop them into the above beaker, Stir to obtain titanium sol. Aging the titanium sol at room temperature for 24 hours, drying at 110°C, and grinding through a 120-mesh sieve to obtain TiO 2 powder.

[0021] (2) According to SiO 2 with TiO 2 Weigh 4g SiO with a mass ratio of 2:3 2 , 6g TiO 2 , perform mechanical mixing, and add an appropriate amount of ethanol to continue stirring, stir and dry the above mixture to obtain a uniform SiO 2 with TiO 2 mixture, add 0.6g La 2 o 3 Powder, mixed evenly, impregnated with equal volume of sulfuric acid of 1 mol / L, stirred well and left for 5 hours, stirred and dried, transferred to muffle furnace for roasting at 400°C for 6 hours, the solid was naturally cooled, and the above solid w...

Embodiment 2

[0023] (1) Take 25.58g of tetra-n-butyl titanate and 20ml of ethanol in a 250ml beaker and stir evenly; take 20ml of ethanol, 1.04g of concentrated sulfuric acid and 4ml of distilled water, mix them evenly and put them in a separatory funnel, quickly drop them into the above beaker, Stir to obtain titanium sol; age the titanium sol at room temperature for 24 hours, dry at 110°C, and grind through a 120-mesh sieve to obtain TiO 2 powder.

[0024] (2) According to SiO 2 with TiO 2 Weigh 3g of SiO with a mass ratio of 3:7 2 , 7g TiO 2 , perform mechanical mixing, and add an appropriate amount of ethanol to continue stirring, stir and dry the above mixture to obtain a uniform SiO 2 with TiO 2 mixture, add 1g La 2 o 3 Powder, mixed evenly, impregnated with equal volume of sulfuric acid of 1 mol / L, stirred well and left for 5 hours, stirred and dried, transferred to muffle furnace for roasting at 400°C for 6 hours, the solid was naturally cooled, and the above solid was taken...

Embodiment 3

[0026] (1) Take 25.58g of tetra-n-butyl titanate, 20ml of ethanol in a 250ml beaker and stir evenly, take 20ml of ethanol, 1.04g of concentrated sulfuric acid and 4ml of distilled water, mix them evenly, put them in a separating funnel, and quickly drop them into the above beaker, Stir to obtain titanium sol; age the titanium sol at room temperature for 24 hours, dry at 110°C, and grind through a 120-mesh sieve to obtain TiO 2 powder.

[0027] (2) According to SiO 2 with TiO 2 Weigh 6g of SiO with a mass ratio of 6:4 2 powder, 4g TiO 2 Powder, mechanically mixed, and add an appropriate amount of ethanol to continue stirring, stir and dry the above mixture to obtain a uniform SiO 2 with TiO 2 mixture, add 0.8g La 2 o 3 The powder is impregnated with equal volume of sulfuric acid of 1 mol / L, stirred fully and left to stand for 5 hours, stirred and dried, transferred to a muffle furnace for roasting at 400°C for 6 hours, and the solid is cooled naturally. Carry out water ...

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Abstract

The invention discloses a preparation method of a modified solid acid catalyst, which comprises the following steps of: (1) preparing titanium dioxide of 120 meshes by utilizing the hydrolysis of tetrabutyl titanate; (2) dispersing the titanium dioxide and silicon dioxide into ethanol, stirring evenly and drying to obtain the mixture of the titanium dioxide and the silicon dioxide, wherein the mass ratio of the silicon dioxide to the titanium dioxide is 3:2 to 7; and (3) adding lanthanum oxide into the mixture of the titanium dioxide and the silicon dioxide, mixing evenly, carrying out isometric immersion by using 0.5 to 1.5mol / L of sulfuric acid, ageing, stirring, drying to obtain a solid, calcining for 2 to 8 hours under the condition of 350 to 450 DEG C, cooling the calcined solid, washing by using water until the pH value is 2 to 3 and then drying to obtain a catalyst La3+-SO42--TiO2-SiO2, wherein the mass of the lanthanum oxide is 4 to 15 percent of the total mass of the titaniumdioxide and the silicon dioxide. The catalyst has high esterification activity at a lower reaction temperature.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a preparation method of a modified solid acid catalyst and the prepared catalyst. Background technique [0002] With the increasing shortage of fossil fuels and the gradual implementation of the world's carbon dioxide emission reduction plan, China's demand for clean and renewable energy is gradually expanding. Biomass energy, as an important resource with zero carbon dioxide emissions, plays a pivotal role in the ranks of renewable new energy. As one of the important technologies for direct liquefaction of biomass at present, flash pyrolysis technology can realize the direct transformation of solid biomass waste into liquid bio-oil, and completes the first step in the utilization of biomass energy liquid fuel. However, the currently prepared liquid bio-oil is still far from the standards of gasoline and diesel power fuels produced by fossil fuels. The improvement o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053C07C69/14C07C67/08
Inventor 骆仲泱王树荣施正伦高翔余春江倪明江岑可法
Owner ZHEJIANG UNIV
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