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Process for preparing SBA-15 surfical sulfonic group modified mesoporous molecular sieve

A technology of mesoporous molecular sieves and surface sulfonic acid groups, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of complex preparation process, high catalyst cost, and long preparation cycle, and achieve convenient production , simple operation, mild reaction conditions

Inactive Publication Date: 2006-02-22
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the post-synthesis method is often used in the synthesis process of organic acid-modified mesoporous materials. Although the organic-inorganic hybrid materials prepared by the post-synthesis method can completely maintain the structure of the molecular sieve, the distribution of the modified groups is uneven, and most of them are located at the pores. The inner surface and the outer surface are not evenly distributed on the surface of the pore, and the preparation process is relatively complicated. Many chemical raw materials are required in the modification process, resulting in high catalyst cost and long preparation cycle, which is not suitable for the industrialization of catalysts.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve 1 g of P123 in 97.58 g of deionized water, and stir at room temperature for 2 hours; add 25.53 g of concentrated hydrochloric acid (37%), heat up to 40° C., and stir for 60 minutes; dropwise add 8.11 g of TEOS, and stir for 45 minutes; Add 0.40g MPTMS and 4.18g H 2 o 2 (30%), H 2 o 2 It can oxidize mercapto group to sulfonic acid group, stir at 40°C for 20 hours, put it into a 150ml stainless steel autoclave lined with polytetrafluoroethylene, crystallize at 100°C for 24 hours, take it out for suction filtration, washing, and drying Afterwards, the synthesized molecular sieve powder was washed with absolute ethanol solution for 24 hours to remove the template agent P123 to obtain a mesoporous molecular sieve modified with sulfonic acid groups on the surface of SBA-15. The acid content, specific surface area and pore size of mesoporous molecular sieves are shown in Table 1

Embodiment 2

[0022] Dissolve 1 g of P 123 in 97.58 g of deionized water, and stir at room temperature for 4 hours; add 12.76 g of concentrated sulfuric acid (50%), heat up to 70°C, and stir for 30 minutes; dropwise add 7.69 g of TEOS, and stir for 45 minutes; Then add 0.81g MPTMS and 8.37g H 2 o 2 (30%), stirred at 70°C for 15 hours, then put into 150ml stainless steel autoclave with polytetrafluoroethylene liner, statically crystallized at 120°C for 48 hours, took it out for suction filtration, washed, dried with anhydrous The synthesized raw powder molecular sieve was washed with ethanol solution for 24 hours, and the template agent P123 was removed to obtain the mesoporous molecular sieve modified by SBA-15 surface sulfonic acid groups. The acid content, specific surface area and pore size of mesoporous molecular sieves are shown in Table 1

Embodiment 3

[0024] Dissolve 4 g of P123 in 195.16 g of deionized water, and stir at room temperature for 2 hours; add 25.53 g of concentrated hydrochloric acid (37%), heat up to 40° C., and stir for 60 minutes; dropwise add 7.26 g of TEOS, and stir for 90 minutes; Add 1.21g MPTMS and 12.56g H 2 o 2 (30%), after stirring for 20 hours at 40°C, put it into a 150ml stainless steel autoclave with a polytetrafluoroethylene liner, statically crystallize it at 100°C for 24 hours, take it out and carry out suction filtration, washing, and dry it with anhydrous The synthesized raw powder molecular sieve was washed with ethanol solution for 48 hours, and the template agent P123 was removed to obtain the mesoporous molecular sieve modified by SBA-15 surface sulfonic acid groups. The acid content, specific surface area and pore size of mesoporous molecular sieves are shown in Table 1

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Abstract

Disclosed is a method for preparation of molecular sieve modified by SBA- 15 surface sulfuric acid group, which contains the step: with polymer of the polyethylene glycol- polyglycerol- polyethylene glycol as the template agent, 3-mercaptopropyl-trimethoxysilane condensing ethyl orthosilicate in a acid condition, and by the oxidization of hydroperoxide, the molecular sieve modified by propanesulfonic acid being synthesized. The method for preparation is simple, the operation is easy, and the reaction condition is mild; the acid containing and the structure of the molecular can be regulated and controlled by regulating the matching of materials and processing parameter, the acid quantity being among 0.48- 1.15mmolH+ / g, specific surface being among 445- 680m2 / g, and the pore diameter being among 5.47- 7.58nm.

Description

technical field [0001] The invention belongs to a method for preparing mesoporous molecular sieves, in particular to a method for preparing mesoporous molecular sieves modified with sulfonic acid groups on the surface of SBA-15 Background technique [0002] In recent years, inorganic materials functionalized with organic groups have attracted increasing interest, mainly because such organic-inorganic hybrid materials can tune their catalytic and adsorption properties by designing organic acid functional groups in the pores ( Fowler C.E. et al. Chemistry Communication, 1997, 1769). At present, most researches focus on SiO 2 The surface of the carrier is functionalized, and the organic functional group is connected to the inorganic matrix through the O-Si-C bond. The synthesis method is mainly divided into a post-synthesis method and a one-step synthesis method. The post-synthesis method (also called surface grafting method) is to generate organic-inorganic hybrid materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/00
Inventor 孙予罕魏伟郑岩苏小威
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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