Composite mesoporous molecular sieve solid superacid and preparation method thereof

A mesoporous molecular sieve and solid superacid technology, which is applied in the preparation of carboxylate esters, molecular sieve catalysts, and organic compounds, can solve the problems of low density of solid superacid acid centers, short service life of catalysts, and low catalytic activity. Achieve uniform distribution of active centers, mild preparation conditions, and high catalytic activity

Inactive Publication Date: 2016-03-16
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although solid superacids have many advantages, there are still deficiencies in the application process: ①Compared with traditional acid catalysts, solid superacids have lower acid center density, lower activity, and smaller specific surface area, so the reaction reaches equilibrium under the same conditions. long; ②The acid strength of different solid superacids varies greatly, and the adaptability to different reaction systems is different; ③SO 4 2- It is easy to lose, so the service life of the catalyst is short; ④ In the organic reaction, there is a p

Method used

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  • Composite mesoporous molecular sieve solid superacid and preparation method thereof
  • Composite mesoporous molecular sieve solid superacid and preparation method thereof
  • Composite mesoporous molecular sieve solid superacid and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0042] TiO 2 The effect of loading rate on the catalytic activity of solid super acid:

[0043] At room temperature, add 1g of each MAS-5 mesoporous molecular sieve into a beaker containing 5-20ml of sol, magnetically stir for 30 minutes, and then sonicate for 40 minutes; ensure that the inner surface of the MAS-5 mesoporous molecular sieve is in full contact with the sol; Pressure distillation, evaporate the solvent, and vacuum-dry at 70℃ and 0.09MPa vacuum degree for 4h; take it out and grind it into powder with agate, and calcinate in a muffle furnace at 500℃ for 3h;

[0044] Take 1g of loaded TiO 2 MAS-5 molecular sieve is placed in a watch glass, and 2mol / L H 2 SO 4 Add 3.8g of the solution dropwise to the watch glass where the molecular sieve is placed. Stir slowly with a glass rod, and it is creamy. After stirring, put it in a vacuum drying oven at 70℃ and dry for 4h; after grinding it into powder, place it in a muffle furnace Calcined at 450°C for 4 hours to obtain a solid ...

Embodiment 2

[0054] TiO 2 Calcination temperature for doped 37.5%TiO 2 The effect of solid super acid on catalytic activity:

[0055] Same operation as in Example 1, but its TiO 2 The calcination temperatures were 475°C, 500°C, and 530°C, respectively, and the activity evaluation results of the obtained new composite mesoporous molecular sieve solid superacid are shown in Table 2.

[0056] Table 2TiO 2 Effect of calcination temperature on catalytic activity of catalyst

[0057]

[0058] It can be seen from Table 2 that TiO 2 When the calcination temperature is 500℃, the catalyst activity is ideal.

Embodiment 3

[0060] Impregnated H 2 SO 4 The influence of solution concentration on the catalytic activity of solid super acid:

[0061] Same operation as in Example 1, but the impregnated H 2 SO 4 The solution concentrations were 1 mol / L, 2 mol / L, and 3 mol / L, and the activity evaluation results of the obtained composite mesoporous molecular sieve solid super acid are shown in Table 3.

[0062] Table 3 The influence of impregnated sulfuric acid concentration on the catalytic activity of the catalyst

[0063]

[0064] It can be seen from Table 3 that H 2 SO 4 Solution immersion concentration 2mol / L, SO 4 2- When the loading rate is 35.23%, the catalytic activity of the obtained catalyst is ideal.

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Abstract

The invention relates to a composite mesoporous molecular sieve solid superacid and a preparation method thereof. According to the method, a home-made mesoporous molecular sieve is used as a carrier, a sol-gel method and an impregnation method are adopted to dope TiO2 and load SO4<2-> to obtain the novel molecular sieve loaded oxide solid superacid SO4<2->/TiO2/MAS-5 which is used as a catalyst to prepare propylene glycol monomethyl ether acetate (PMA) by taking propylene glycol monomethyl ether (PM) and acetic acid (HAc) as materials for esterification reaction so as to achieve probe reaction, thus optimizing the formula and loading conditions of TiO2 and SO4<2->. Compared with existing SO4<2->/TiO2 solid superacid catalysts, the catalyst disclosed by the invention has the advantages of high acid strength, high catalytic activity, large specific surface area, long service life and good stability, and has wide industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of a novel solid superacid, in particular to a composite mesoporous molecular sieve solid superacid and a preparation method thereof. Background technique [0002] Acid catalysis has important applications in chemical reactions. Early acid catalysts were liquid acids such as sulfuric acid and phosphoric acid. Although this kind of acid catalyst has quite high catalytic activity at lower temperature, it is not suitable for acid-catalyzed reaction at higher temperature. At the same time, there are many problems such as easy corrosion of equipment, environmental pollution, and difficulty in catalyst post-treatment. Since 1979, Japanese scientists Hino et al. reported the first M x o y Since the solid superacid, people's research on the solid superacid has been deepening. Solid super acid is a new type of green catalytic material, which can replace the traditional liquid acid catalyst and has good catalytic...

Claims

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Application Information

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IPC IPC(8): B01J29/70C07C67/08C07C69/16
CPCB01J29/7049C07C67/08C07C69/16
Inventor 王红星柯艺聪邱挺叶长燊李玲黄智贤杨臣王晓达杨金杯陈锦溢
Owner FUZHOU UNIVERSITY
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