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C@TiO2 solid acid catalyst in core-shell structure and preparation method thereof

A technology of solid acid catalyst and core-shell structure, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of harsh preparation conditions, difficult industrial application, and low acid density. Simple, stable performance, the effect of increasing acid strength

Active Publication Date: 2015-03-04
SANMING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many researchers have noticed this and vigorously developed solid acid catalysts. Although there are many types of solid acids that have been developed, they also have certain defects. The main problem is that the acid content is less, the acid density is lower, and the effect is better. The solid acid also has problems such as high cost or harsh preparation conditions, so that it is difficult for industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A core-shell structured CTiO 2 The preparation method of solid acid catalyst, concrete steps are:

[0019] (1) Dissolve 5g of starch in 100mL of water and stir until completely dissolved; then add 10mL of tetrabutyl titanate dropwise into the solution and stir evenly to obtain an emulsion; transfer the emulsion to polytetrafluoroethylene In an ethylene-lined stainless steel autoclave, react at 100°C for 24 hours, filter the product, wash with absolute ethanol, and dry at 50°C to obtain a powder; place the powder in a dry N 2 Under the atmosphere, pyrolyze at 200°C for 90 minutes to obtain a catalyst precursor with a core-shell structure;

[0020] (2) Grind the precursor into powder, hydrothermally sulfonate it with 1mol / L sulfuric acid at 200°C; then wash it with deionized water until no sulfate ion is detected; finally dry it at 50°C for 24 hours to obtain the nucleus Shell-structured CTiO 2 solid acid catalyst.

Embodiment 2

[0022] A core-shell structured CTiO 2 The preparation method of solid acid catalyst, concrete steps are:

[0023] (1) Dissolve 10g of sucrose in 150mL of water and stir until completely dissolved; then add 15mL of tetrabutyl titanate dropwise into the solution and stir evenly to obtain an emulsion; transfer the emulsion to PTFE In an ethylene-lined stainless steel autoclave, react at 200°C for 6 hours, filter the product, wash with absolute ethanol, and dry at 105°C to obtain a powder; place the powder in a dry N 2 Under the atmosphere, pyrolyze at 500°C for 60 minutes to obtain a catalyst precursor with a core-shell structure;

[0024] (2) Grind the precursor into powder, hydrothermally sulfonate it with 3mol / L sulfuric acid at 150°C; then wash it with deionized water until no sulfate ion can be detected; finally dry it at 105°C for 5 hours to obtain the nucleus Shell-structured CTiO 2 solid acid catalyst.

Embodiment 3

[0026] A core-shell structured CTiO 2 The preparation method of solid acid catalyst, concrete steps are:

[0027] (1) Dissolve 20g of cellulose in 200mL of water and stir until completely dissolved; then add 20mL of tetrabutyl titanate dropwise into the solution and stir evenly to obtain an emulsion; transfer the emulsion to polytetrafluoroethylene In a stainless steel autoclave lined with vinyl fluoride, react at 150°C for 13h, filter and wash the product, and dry at 75°C to obtain a powder; place the powder in a dry N 2 Under the atmosphere, pyrolyze at 350°C for 75 minutes to obtain a catalyst precursor with a core-shell structure;

[0028] (2) Grind the precursor into powder and hydrothermally sulfonate it with 5mol / L sulfuric acid at 100°C; then wash it with deionized water until no sulfate ion is detected; finally dry it at 75°C for 13 hours to obtain the nucleus Shell-structured CTiO 2 solid acid catalyst.

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Abstract

The invention belongs to the preparation field of catalysts, and in particular relates to a C@TiO2 solid acid catalyst in a core-shell structure and a preparation method of the C@TiO2 solid acid catalyst. The main preparation process is as follows: reacting biomass and tetrabutyl titanate serving as raw materials for 6-24 hours at 100-200 DEG C, drying and pyrolyzing the product to obtain a catalyst precursor in the core-shell structure, sulfonating the catalyst precursor through sulfuric acid, and drying to obtain the C@TiO2 solid acid catalyst in the core-shell structure. The catalyst has good catalysis activity and stability in acid alcohol esterification and transesterification. The raw material for the catalyst disclosed by the invention is cheap and easy to obtain, the performance is stable, and the large-scale production can be realized. Furthermore, the catalyst solves the common fault that the normal metallic oxide solid acid catalyst is easy to inactivate, and meanwhile, the acid density is increased, so that the acid strength is greatly prompted, the catalysis effect is good, and the catalyst is reusable and environmentally friendly.

Description

technical field [0001] The invention belongs to the field of preparation of catalysts, in particular to CTiO with a core-shell structure 2 Solid acid catalyst and its preparation method. Background technique [0002] In the chemical industry, many reactions need to be carried out under acid-catalyzed conditions, such as hydrocarbon cracking, alkyl isomerization, hydrolysis, alkyd esterification and transesterification. Traditional acid catalysts are mainly inorganic liquid acids, mainly HF, HCl, H 2 SO 4 、H 3 PO 4 etc., although the catalytic effect of these liquid acid catalysts is better, there are many weak points. For example, it is extremely easy to corrode equipment, endanger the safety of operators, can only be applied to batch processes, has poor product selectivity, and the separation steps from products are complicated. In addition, it will inevitably cause serious environmental pollution, especially in the environment where the "green chemical industry" is v...

Claims

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Application Information

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IPC IPC(8): B01J27/053C07C69/58C07C67/08
Inventor 牛玉李福颖王仁章杨金杯董国文
Owner SANMING UNIV
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