A kind of method utilizing kaolin to synthesize highly stable ordered mesoporous material al-sba-15

An al-sba-15, high-stability technology, applied in chemical instruments and methods, molecular sieve compounds, molecular sieves and alkali exchange compounds, etc., can solve the problems of kaolin and other problems, achieve lower synthesis costs, loose operating conditions, high water content The effect of thermal stability

Inactive Publication Date: 2016-01-06
INNER MONGOLIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, research on the synthesis of molecular sieves using kaolin as raw materials mainly focuses on the preparation of 4A zeolite molecular sieves, Y-type zeolite molecular sieves, P-type zeolite molecular sieves, and ZSM-5 molecular sieves, etc., and a small number of ordered mesoporous materials MCM-41 is synthesized from kaolin as raw materials. related reports, but there is no report on the synthesis of SBA-15 from kaolin

Method used

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  • A kind of method utilizing kaolin to synthesize highly stable ordered mesoporous material al-sba-15
  • A kind of method utilizing kaolin to synthesize highly stable ordered mesoporous material al-sba-15
  • A kind of method utilizing kaolin to synthesize highly stable ordered mesoporous material al-sba-15

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Experimental program
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Effect test

Embodiment 1

[0032] Activate the kaolin by roasting at 800°C for 3 hours, weigh 12g of the roasted kaolin, leaching with 6mol / L hydrochloric acid for 4h, then filter and wash with deionized water until neutral and dry; dry the dried sample at 950°C Roast for 2 hours; then put it into 5mol / L NaOH alkali solution, and react for 3 hours under high temperature and high pressure (temperature is 160°C and pressure is 0.5MPa). After the reaction is completed, adjust the pH value to 12.0 with hydrochloric acid. Then it was added dropwise to the acid solution of surfactant P123, stirred and reacted at 40°C for 24h, hydrothermally reacted at 100°C for 24h, filtered, washed and dried, then roasted at 550°C in a muffle furnace for 6h to obtain high stability Ordered mesoporous material Al-SBA-15.

Embodiment 2

[0034] Activate the kaolin by roasting at 800°C for 3 hours, weigh 12 g of the roasted kaolin, treat it with a mixed acid with a volume ratio of 4 mol / L sulfuric acid and hydrochloric acid of 0.4 for 4 hours, then filter and wash with deionized water until neutral and dry; The dried sample was roasted at 950°C for 2h; then put into 5mol / L NaOH alkali solution, and reacted at high temperature and high pressure for 3h (temperature was 160°C, pressure was 0.5MPa), after the reaction was completed, the pH value was adjusted with hydrochloric acid In 12.0. Then it was added dropwise to the acid solution in the mixed surfactant (n(FSO-100) / n(P123)=5.5, the concentration of hydrochloric acid was 7.5mol / L), stirred at 40°C for 24h, and hydrothermally heated at 160°C After reacting for 48 hours, filtering, washing and drying, it was calcined in a muffle furnace at 550°C for 6 hours to obtain Al-SBA-15, an ordered mesoporous material with high stability.

Embodiment 3

[0036]Activate the kaolin by roasting at 700°C for 4 hours, weigh 12g of the roasted kaolin, leaching with 6mol / L hydrochloric acid for 4h, then filter and wash with deionized water until neutral and dry; dry the dried sample at 950°C Roast for 2 hours; then put it into 5mol / L NaOH alkali solution, react for 3 hours under high temperature and high pressure (temperature is 160°C, pressure is 0.5MPa), after the reaction is completed, adjust its pH value to 14.0 with hydrochloric acid. Then it was added dropwise to the acid solution in the mixed surfactant (n(FSO-100) / n(P123)=5.5, the concentration of hydrochloric acid was 7.5mol / L), stirred at 40°C for 24h, and hydrothermally heated at 160°C After reacting for 48 hours, filtering, washing and drying, it was calcined in a muffle furnace at 550°C for 6 hours to obtain Al-SBA-15, an ordered mesoporous material with high stability.

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Abstract

The invention discloses a method for synthesizing a high-stability ordered mesoporous material A1-SBA-15 by use of kaoline. The method comprises the following steps: by taking kaoline as a raw material, performing roasting and acid leaching treatment on kaoline, and then adding an alkaline solution with a certain concentration to the treated kaoline to have a reaction, thereby obtain silicon and aluminum sources; adjusting the pH value of the obtained silicon-aluminum source solution to a certain value, and then adding the silicon-aluminum source solution to a mixed solution of a triblock copolymer (P123), a fluorocarbon surfactant (FSO-100 or FS-31) and hydrochloric acid, stirring at 40 DEG C, then carrying out reaction under a hydrothermal condition for 12-72 hours, and finally, filtering, washing, drying and roasting to obtain the high-stability ordered mesoporous material A1-SBA-15. The ordered mesoporous material A1-SBA-15 is synthesized by use of the cheap natural mineral kaoline as the raw material; the preparation process is simple, the raw material is easy to get, and the operation conditions are lenient; the synthesized ordered mesoporous material has excellent hydrothermal stability and catalytic activity.

Description

technical field [0001] The invention relates to a method for synthesizing inorganic non-metallic materials, in particular to a method for synthesizing highly stable and ordered mesoporous material Al-SBA-15 by using kaolin. Background technique [0002] In 1992, Mobil Corporation developed a new class of molecular sieve materials - M41S series of ordered mesoporous materials. This development made molecular sieve materials the focus of scientists in the fields of chemistry, materials, and environmental protection. The advent of M41S mesoporous materials not only provides a new idea for the synthesis of ordered mesoporous structures for the scientific field, but also its large specific surface area and continuously adjustable pore size fill the gaps in the application of microporous materials. Subsequently, reports on the synthesis of ordered mesoporous materials continue to flow, and mesoporous materials with different compositions and structures have come out one after anot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/00C01B39/00
Inventor 杜春芳赵啟行刘志亮孙梦临
Owner INNER MONGOLIA UNIVERSITY
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