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Super-strong acid mesoporous material synthesized in one pot and preparing method

An acid-mesoporous, super-strong technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of catalyst preparation steps and long cycle, and achieve good catalytic activity and short cycle , the effect of fewer steps

Inactive Publication Date: 2007-08-29
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the zirconium-containing mesoporous materials synthesized by this method need to be impregnated with sulfuric acid to have super acidity, so the preparation steps of the catalyst are more and the cycle is longer.

Method used

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  • Super-strong acid mesoporous material synthesized in one pot and preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0016] First, 4.4gZr(NO 3 ) 4 ·3H 2 O and 1.63gCTAB were dissolved in 40ml and 15ml of ethanol solution respectively, after dissolving, mixed and stirred for 1h, counted as A; at the same time, 1gP123 was dissolved in 10ml 1mol / LH 2 SO 4 and 30ml of 2mol / L HCl, stirred at 40°C for 3h, until P123 was completely dissolved, then added 2.3ml of TEOS, continued to stir for 2.5h, counted as B;

[0017] Then put A in a 100ml reaction kettle with a polytetrafluoroethylene liner, pre-crystallize at 110°C for 3.5h, then take it out, cool to room temperature, stir at room temperature for 0.5h, add B, continue Stir for 3 hours, put in a kettle, crystallize at 100°C for 48 hours, count as C;

[0018] Finally, cool C, wash, filter with suction, dry at room temperature, and roast at 600°C for 3 hours to obtain SO 4 2- / ZrO 2 -SiO 2 The superacid mesoporous material has good crystallinity by XRD analysis.

Embodiment approach 2

[0020] First, 4.4gZr(NO 3 ) 4 ·3H 2 O and 1.63gCTAB were dissolved in 40ml and 15ml of ethanol solution respectively, after dissolving, mixed and stirred for 1h, counted as A; at the same time, 1gP123 was dissolved in 20ml 1mol / LH 2 SO 4 and 20ml of 2mol / L HCl, stir at 40°C for 4h, until P123 is completely dissolved, add 2.3ml of TEOS, continue to stir for 2h, count as B;

[0021] Then put A in a 100ml reaction kettle with a polytetrafluoroethylene liner, pre-crystallize at 110°C for 4h, then take it out, cool to room temperature, stir at room temperature for 0.5h, add B, and continue stirring 3h, put in a kettle, crystallize at 95°C for 48h, counted as C;

[0022] Finally, cool C, wash, suction filter, dry at room temperature, and roast at 610°C for 2.5h to obtain SO 4 2 / ZrO 2 -SiO 2 The crystallinity of the superacid mesoporous material is more than twice that of the sample obtained in the first embodiment through XRD analysis.

Embodiment approach 3

[0024] First, 4.4gZr(NO 3 ) 4 ·3H 2 O and 1.63gCTAB were dissolved in 40ml and 15ml of ethanol solution respectively, after dissolving, mixed and stirred for 1h, counted as A; at the same time, 1gP123 was dissolved in 30ml 1mol / LH 2 SO4 and 10ml of 2mol / L HCl, stir at 38°C for 3.5h, until P123 is completely dissolved, add 2.3ml of TEOS, continue to stir for 3h, count as B;

[0025] Then put A in a 100ml reaction kettle with a polytetrafluoroethylene liner, pre-crystallize at 115°C for 3h, then take it out, cool to room temperature, stir at room temperature for 0.5h, add B, and continue stirring 3h, put in a kettle, crystallize at 100°C for 46h, count as C;

[0026] Finally, cool C, wash, filter with suction, dry at room temperature, and roast at 590°C for 3.5h to obtain SO 4 2- / ZrO 2 -SiO 2 Superacid mesoporous materials. According to XRD analysis, its crystallinity is more than double that of the sample obtained in Embodiment 1.

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Abstract

The invention relates to a one-pot synthesis super acid mesoporous material and preparation method, specifically involved a SO42- / ZrO2-SiO2 super acid mesoporous material and preparation method. Its characteristic lie in Zr(NO3)4 . 3H2O and CTAB were separately dissolved in ethanol solution, mix stirring, calculated as A; At the same time, the mixture of concentration 1mol / LH2SO4 and 2 mol / LHCl into Polyoxyethylene - polyoxypropylene - Polyoxyethylene triblock copolymer, and add to silicate lipid mixing make it uniform, calculated as B; put A into reaction kettle loaded with Teflon-lined, heating 3-4h under the 95-100degree centigrade, and after its removal, after cooling joined into B, the mixture evenly loaded into reaction kettle, at 95 ~ 100 degree centigrade crystallization 45 ~ 48 h, it would complete after washing filtrating roasting to remove template. The method prepared super acid mesoporous materials has short synthesis lead time, and have structured mesoporous structure, good thermal stability, and it demonstrated a positive catalytic activity in positive pentane isomerization reaction, it will become the important catalytic material of fine chemical,petrochemical and other aspects.

Description

1. Technical field [0001] The one-pot synthesized superacid mesoporous material of the present invention and its preparation method are a kind of synthesis method about inorganic porous catalytic materials, belonging to the field of fine chemical industry, more specifically, a simple SO 4 2- / ZrO 2 -SiO 2 Synthesis method of superacid mesoporous materials. 2. Technical Background [0002] Since 1992, Mobil first successfully synthesized the new M41S series mesoporous SiO with adjustable pore size in the range of 2-10nm by using alkyl quaternary ammonium salt cationic surfactant as template agent. 2 Since then, the research on mesoporous materials has rapidly become a hot spot in the world. This type of material has the characteristics of large specific surface area, narrow pore size distribution and strong adsorption capacity. Especially in recent years, with the continuous innovation of technology, molecular sieve series such as SBA and HMS have emerged, and their therm...

Claims

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Application Information

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IPC IPC(8): B01J27/053
Inventor 李瑞丰李福祥周梅梅于峰梁栋王琰谢克昌
Owner TAIYUAN UNIV OF TECH
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