Dual-pore distribution silica synthesis method

A dual-pore distribution and synthesis method technology, applied in the direction of silicon oxide, silicon dioxide, etc., can solve the problems of harsh synthesis conditions and high cost, and achieve the effects of simple synthesis method, large pore volume, and flexible operation

Active Publication Date: 2010-07-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This invention uses organosilicon compound as the silicon source, uses special surfactant, the synthesis conditions are harsh, and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0023] Bi-porous silica was synthesized using tetraethyl orthosilicate as the silicon source and a mixture of glucose and cetyltrimethylammonium bromide (CTAB) as the template.

[0024] With 8.59g ethyl orthosilicate (Sinopharm Chemical Reagent Co., Ltd., SiO 2 Mass content 28.0%), 1.98g glucose (Sinopharm Chemical Reagent Co., Ltd., analytically pure) and 1.47gCTAB (Sinopharm Chemical Reagent Co., Ltd., mass content 99.0%) were added to 36ml of water, stirred at room temperature for 3 hours, with concentration 10% by weight of dilute hydrochloric acid solution to adjust the pH value to 4.0, stirred for 6 hours, aged at 40°C for 96 hours, filtered the resulting mixture, washed with deionized water, dried at 100°C, and calcined at 600°C for 6 hours to obtain a double-pore Distributed silica, its properties are shown in Table 1.

Embodiment 2

[0026] Silica with biporous distribution was synthesized using sodium silicate as silicon source and mixture of glucose and cetyltrimethylammonium bromide (CTAB) as template.

[0027] 11.78g sodium silicate (Na 2 SiO 3 9H 2 O, Sinopharm Chemical Reagent Co., Ltd., Na 2 O mass content 19.3~22.8%), 1.98g glucose (Sinopharm Chemical Reagent Co., Ltd., analytically pure) and 1.47g CTAB (Sinopharm Chemical Reagent Co., Ltd., mass content 99.0%) were added to 36ml of water, stirred at room temperature for 0.5 hour, adjust the pH value to 12.0 with a concentration of 10% by weight dilute sodium hydroxide solution, then stir for 3 hours, stop stirring, and age at 80° C. for 48 hours; the resulting mixture is filtered, washed with deionized water, and dried at 120° C. , and then calcined at 640°C for 3 hours to obtain biporous silicon oxide, whose properties are shown in Table 1.

Embodiment 3

[0029] Ethyl orthosilicate (Sinopharm Chemical Reagent Co., Ltd., SiO 2 The mass content is 28.0%) as a silicon source, and the mixture of sucrose and polyoxyethylene-polyoxypropylene-polyoxyethylene (P123) is a template agent for synthesizing double-hole distributed silicon oxide.

[0030] With 8.59g ethyl orthosilicate (Sinopharm Chemical Reagent Co., Ltd., SiO 2Mass content 28.0%), 1.98g sucrose (Sinopharm Group Chemical Reagent Co., Ltd., analytically pure) and 3.72g P123 (Nanjing Weier Chemical Co., Ltd., molecular weight: 5650) were added to 36ml of water, stirred at room temperature for 4 hours, with concentration Adjust the pH value to 6.0 for a 10% by weight dilute hydrochloric acid solution, then stir for 6 hours, stop stirring, age at 60°C for 72 hours, filter the resulting mixture, wash with deionized water, dry at 120°C, and then bake at 600°C for 6 Hours, the biporous distributed silica was obtained, and its properties are shown in Table 1.

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Abstract

A dual-pore distribution silica synthesis method includes that water, silicon source and template agent are mixed, and the pH value of the mixture is regulated to 4-12, the mixture is aged for 0.5-4 days at the temperature of 40-120 DEG C, and then the mixture is filtered, rinsed, dried and roasted; the template agent is the mixture of sugar and surfactant, the weight ratio of sugar and surfactant of the template agent is 0.5-2, the molar ratio of silicon and water is 1:30-1:200, the molar ratio of silicon and template agent is 1:0.005-2. The portable pore diameter of the pore with smaller pore diameter of the dual-pore distribution silicon-aluminum material is 2-10 nm, the portable pore diameter of the pore with larger pore diameter is 10-25nm, the specific area is 400-750 m2/g, and the pore volume is 0.8-1.5cm3/g. The dual-pore distribution silicon-aluminum material can be used as absorbent and catalyst, or used as the carriers of absorbent and catalyst.

Description

technical field [0001] The invention relates to a method for synthesizing silicon oxide. Background technique [0002] Using new synthetic routes to prepare materials with special properties and new structures is a hot spot in the field of materials at home and abroad. In 1992, researchers at Mobile Corporation first used C n h 2n+1 N(CH 3 ) 3 M41S series mesoporous molecular sieves were synthesized with Br(n>6) cationic surfactants as templates. Because of their high specific surface area, large pore volume, narrow pore distribution and adjustable pore , separation and new catalytic materials have potential industrial application prospects. The pore size of this mesoporous molecular sieve has a single-valued distribution, and the preparation of catalytic cracking catalysts for macromolecule cracking often requires a reasonable configuration of two-stage pores or multi-stage pores. [0003] CN1304871A discloses a double hole molecular sieve, the specific surface are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
Inventor 许本静田辉平朱玉霞陆友保龙军
Owner CHINA PETROLEUM & CHEM CORP
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