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Method for preparing ordered mesoporous material by utilizing bentonite

A technology of mesoporous materials and bentonite, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of low specific surface area of ​​Al-MCM-41, high concentration of surfactant, less amount of bentonite, etc., to achieve low price, Raw materials are easy to obtain and the pores are uniform

Inactive Publication Date: 2010-02-10
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In recent years, bentonite has been used by researchers in the synthesis of highly stable mesoporous molecular sieves. For example, Zhou et al. used natural clay, ethyl orthosilicate, and aluminum isopropoxide as raw materials at room temperature. Methylammonium bromide is used as a template to synthesize a highly stable mesoporous molecular sieve containing B acid sites; however, using organoaluminum as a raw material is not only costly but also highly toxic (Chinese Chemistry Letters, 2005, 16: 261-264); Liu Jianfen et al. used natural montmorillonite and silica gel as raw materials and hexadecyltrimethylammonium bromide as a template to synthesize highly stable Al-MCM-41 in situ on montmorillonite. The pure reagent silicon source is needed, the surfactant concentration required for the reaction is higher, and the energy consumption is time-consuming, the specific surface area of ​​the obtained Al-MCM-41 is not high (Journal of Inorganic Materials, 2003, 18: 867-871) ; Tang Yajing and others synthesized high-stability mesoporous molecular sieves with bentonite, sodium silicate and aluminum chloride as raw materials by microwave method, but the use amount of sodium silicate and aluminum chloride is relatively large, and the amount of bentonite is less (nanotechnology and Precision Engineering, 2008, 6: 185-189)

Method used

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  • Method for preparing ordered mesoporous material by utilizing bentonite
  • Method for preparing ordered mesoporous material by utilizing bentonite

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Mix 15g of bentonite raw material passing through a 200-mesh sieve with NaOH solid at a mass ratio of 1:1.25, roast at 600°C for 2h, add 300mL of deionized water after natural cooling, let stand for 16h, and then leaching 80mL of supernatant liquid gradually Add dropwise into the solution of cetyltrimethylammonium bromide, continue to stir, adjust the pH value of the mixed solution to 11 with hydrochloric acid, transfer the mixed solution to the reaction kettle for 24 hours at 110°C to crystallize for 24 hours to obtain the precursor, the precursor After suction filtration, washing, drying for 4 hours, calcination at 540°C for 6 hours, and natural cooling to room temperature, the ordered mesoporous material Al-MCM-41 was obtained with a silicon-aluminum ratio of 13.72. The specific surface area of ​​the prepared Al-MCM-41 can be as high as 840m 2 g -1 , the pore volume can reach 1.04cm 3 g -1 .

Embodiment 2

[0020] Mix 15g of bentonite raw material passed through a 200-mesh sieve with NaOH solid at a mass ratio of 1:1, roast at 600°C for 2h, add 300mL of deionized water after natural cooling, let stand for 12h, and then leaching 80mL of supernatant Add dropwise into the tetradecyltrimethylammonium chloride solution, continue to stir, adjust the pH value of the mixed solution to 9 with hydrochloric acid, and transfer the mixed solution to a reaction kettle for 24 hours at 160°C to obtain a precursor. After suction filtration, washing, drying for 4 hours, calcination at 540°C for 6 hours, and natural cooling to room temperature, the ordered mesoporous material Al-MCM-41 was obtained with a silicon-aluminum ratio of 32.66. The specific surface area of ​​the prepared Al-MCM-41 can be as high as 1000m 2 g -1 above, the pore volume can reach 1.00cm 3 g -1 above.

Embodiment 3

[0022] Mix 15g of bentonite raw material passing through a 200-mesh sieve and NaOH solid at a mass ratio of 1:1.5, roast at 600°C for 2h, add 300mL of deionized water after natural cooling, let stand for 20h, and then leaching 80mL of supernatant liquid one by one Add dropwise into the solution of octadecyltrimethylammonium bromide, continue to stir, and adjust the pH value of the mixed solution to 9 with hydrochloric acid. After 30 minutes, transfer the mixed solution to a reaction kettle for crystallization at 130°C for 24 hours to obtain a precursor. The body was filtered, washed, dried for 4 hours, calcined at 540°C for 6 hours, and naturally cooled to room temperature to obtain an ordered mesoporous material Al-MCM-41 with a silicon-aluminum ratio of 22.69. The specific surface area of ​​the prepared Al-MCM-41 can be as high as 721m 2 g -1 , the pore volume can reach 0.88cm 3 g -1 .

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Abstract

The invention relates to a method for preparing ordered mesoporous material by utilizing bentonite. Bentonite material and alkali with the weight ratio of 1: 0.5-2 are mixed and roasted for activation, a sample after roasting is stirred and leached in deionized water at common temperature, leaching solution is the synthesized material, the leaching solution is dripped in surfactant solution, the pH value of the solution is adjusted to 7-13, the solution is put in a reaction kettle for crystallization at 100-180 DEG C, filtered, washed, dried and roasted at 500-600 DEG C to obtain white power,i.e. the ordered mesoporous material. The method has simple preparation process, cheap and easily available raw material, low concentration of organic material and difficult initiation of environmentpollution. The specific surface area of the prepared ordered mesoporous material has a maximum of over 1000m<2>*g<-1>, the pore volume can reach over 1.00cm<3>*g<-1>, and the distribution of pore diameters is centralized.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials, in particular to a method for preparing ordered mesoporous materials by using bentonite. Background technique [0002] In 1992, Beck et al. of Mobil Corporation synthesized M41S ordered mesoporous material with organosilicon source. Because of its ordered pore structure, large specific surface area, and adjustable pore size, it quickly became one of the hot spots in the field of catalytic materials research. First, it can exert its good adsorption and separation functions in the fields of catalysis, medicine, and petroleum industry (Journal of American Chemical Society, 1992, 114, 10834-10843). With the advancement of synthesis technology, there are continuous innovations from silicon species to templates, from synthesis methods to synthesis conditions. [0003] The preparation of mesoporous silicon materials using self-assembled surfactants as templates has attracted widespread i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 杨华明邓月华欧阳静
Owner CENT SOUTH UNIV
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