Preparation method of molecular sieve of silicon dioxide of media pores

A mesoporous silica and molecular sieve technology, applied in the direction of silica, silicon oxide, and aluminum phosphate with molecular sieve characteristics, to achieve the effects of easy industrial production, lower production costs, and simple processes

Inactive Publication Date: 2008-04-23
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] None of the above methods can adjust the molecular size of the template agent and control the sol-gel process by using the two-step hydrolysis polycondensation method, thereby effectively controlling the reaction time, adjusting the structure of the final product, and simplifying the reaction procedure.

Method used

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  • Preparation method of molecular sieve of silicon dioxide of media pores
  • Preparation method of molecular sieve of silicon dioxide of media pores
  • Preparation method of molecular sieve of silicon dioxide of media pores

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Dissolve 2.07g oxalic acid in 375g deionized water, add 1.75g ​​ammonium metavanadate, 0.99g ammonium molybdate, 0.04g ammonium dihydrogen phosphate, 0.2g sodium acetate, heat to dissolve, and dissolve 223g normal Ethyl silicate, 98.4g of cetyltrimethylammonium bromide and 276g of ethanol were mixed, stirred for 5 hours, added ammonia water to make the pH 12, stirred for 20 hours, the reaction temperature was 30°C, the mixture was filtered and used to remove Wash with ionic water until neutral, dry at room temperature, and bake at 500°C for 5 hours. XRD spectrum see figure 1. In the XRD spectrum, the 2θ corresponding to the d value of 1.0nm is 8.842°, and the 2θ corresponding to the d value of 1.8nm is 4.909°. In this embodiment, the d value corresponding to the strongest line is 3.97 nm, the d value corresponding to the second strongest line is 2.28 nm, and the d value corresponding to the second strongest line is 2.02 nm. TEM pictures and electron diffraction patte...

Embodiment 2

[0035] Dissolve 2.07g oxalic acid in 80g deionized water, add 1.75g ​​ammonium metavanadate, 0.99g ammonium molybdate, 0.04g ammonium dihydrogen phosphate, 0.03g cesium acetate, heat to dissolve, and dissolve 208g normal Ethyl silicate, 98.4g cetyltrimethylammonium bromide and 276g ethanol were mixed, stirred for 5 hours, added 20g sodium hydroxide, stirred for 80 hours, the reaction temperature was 18°C, the mixture was filtered, and deionized water was used to Wash until neutral, dry at room temperature and bake at 550°C for 4 hours. In this embodiment, the d value corresponding to the strongest line is 3.94 nm, and the d value corresponding to the second strongest line is 2.16 nm. BET surface area is 957m 2 / g, BJH pore size is 2.7nm.

Embodiment 3

[0037] Dissolve 9.46g oxalic acid in 375g deionized water, add 5.85g ammonium metavanadate, 4.2g ammonium molybdate, 0.2g ammonium dihydrogen phosphate, and dissolve 208g orthosilicate ethyl ester in 300g deionized water, 98.4g ten Mix hexaalkyltrimethylammonium bromide and 276g ethanol, stir for 0.5 hours, add 20g sodium hydroxide, stir for 1 hour, the reaction temperature is 18°C, filter the mixture, wash with deionized water until neutral, and dry at room temperature Then bake at 550°C for 3 hours. In this embodiment, the d value corresponding to the strongest line is 3.74 nm, and the d value corresponding to the second strongest line is 2.12 nm. BET surface area of ​​951m 2 / g, BJH pore size is 2.7nm.

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Abstract

A molecular sieve of mesoporous SiO2 features that the mole ratio of Si ions to doped ions is 1:X, where X=0-0.07, its BET specific surface area is at least 300 sq.m / g, and its pore diameter is 2-20 nm. Its preparing process includes proportionally mixing Si source, template agent, water, water-soluble cosolvent and doping ions, reacting respectively in acidic and alkaline conditions, filtering, drying and calcining.

Description

technical field [0001] The invention relates to inorganic porous materials, more specifically, to silicon-based mesoporous molecular sieves and a preparation method thereof. Background technique [0002] The sol-gel method is a commonly used chemical method for the preparation of new materials. Controlling the sol-gel process can control the microstructure of the final product, which embodies the idea of ​​molecular tailoring design and makes the preparation process easy to control. Starting from the sol reaction, the The prepared materials can be highly uniform at the molecular level. The two-step hydrolysis polycondensation method is to control the sol-gel speed by adjusting the pH of the reactants, so that the structure of the final product is more uniform. The sol-gel method is also widely used in the preparation of molecular sieves. [0003] Mesoporous molecular sieves were first synthesized by scientists from Mobil Corporation in the early 1990s. Due to their high sp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/02C01B37/06C01B33/113
Inventor 侯秀红曾埙
Owner SHANGHAI RES INST OF CHEM IND
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