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Method for preparing mesoporous material with high hydrothermal stability by ZSM-5

A technology of mesoporous materials and thermal stability, applied in the direction of crystalline aluminosilicate zeolites, etc., can solve problems such as unsatisfactory long-range order, non-compliance with green chemistry, human and environmental toxicity, etc.

Active Publication Date: 2010-01-06
SHANGHAI NOVEL CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when using MCM-22 as the precursor, the mesoporous material obtained has a worm structure, and its long-range order is not ideal.
In addition, when synthesizing the precursors MCM-22 and UTM-1, hexamethyleneimine needs to be used as a template agent. This template agent is highly toxic and has a great poisonous effect on personnel and the environment. It does not comply with green chemistry. Based on the above-mentioned deficiencies of the original patent, it is necessary to choose other microporous molecular sieves as precursors

Method used

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  • Method for preparing mesoporous material with high hydrothermal stability by ZSM-5
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  • Method for preparing mesoporous material with high hydrothermal stability by ZSM-5

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Experimental program
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Effect test

Embodiment 1

[0017] Proportion by mass ZSM-5(SiO 2 / Al 2 o 3 Molar ratio = 300): cetyltrimethylammonium bromide: NaOH: H 2 O=1:2.3:4:95 Mix the materials to obtain a suspension, then place the resulting suspension in an oil bath environment, stir at 100°C for 6 hours, cool to room temperature and adjust to pH=9, then stirred at room temperature for 24 hours, finally the X-ray diffraction pattern (XRD) of the sample obtained after washing and drying is shown in figure 1 a.

Embodiment 2-5

[0019] In Example 1, after the mixture was cooled to room temperature, it was adjusted to pH=8-5 with 2 mol / L hydrochloric acid aqueous solution, then stirred at room temperature for 24 hours, and finally washed and dried to obtain the target sample (see Table 1).

[0020] Table 1 Example 2-5

[0021]

[0022] figure 1 It shows that the samples obtained in the range of pH=9-5 all have diffraction peaks at low angles, indicating that the product has a mesoporous structure. However, the pH value has a certain influence on the product structure. When the pH=9-7, the obtained material all appears four diffraction peaks, and the sine square ratio of the diffraction angle is sin 2 θ 1 : sin 2 θ 2 : sin 2 θ 3 : sin 2 θ 4 =1:3:4:7, indicating that the sample structure conforms to the two-dimensional hexagonal model, and is a mesoporous material with high long-range order. This is the first report on the synthesis of mesoporous materials from microporous molecular sieve ZSM...

Embodiment 6

[0024] Proportion by mass ZSM-5(SiO 2 / Al 2 o 3 =50):tetradecyltrimethylammonium bromide:NaOH:H 2 O=1:2.3:4:95 Mix the materials to obtain a suspension, then place the obtained suspension in an oil bath environment, stir at 100°C for 6 hours, and adjust it with 2 mol / liter aqueous hydrochloric acid solution after cooling to room temperature. To pH=7, then stirred at room temperature for 12 hours, finally after washing and drying, the X-ray diffraction pattern (XRD) of the obtained sample is shown in figure 2 A'.

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Abstract

The invention relates to a method for preparing a mesoporous material with high hydrothermal stability by ZSM-5, which is characterized by comprising the following steps: dissolving microporous molecular sieve ZSM-5 under the condition of the existence of a template agent R; adjusting a pH value of a system by a dilute acid aqueous solution; and after the solution is separated, dried and roasted, obtaining the mesoporous material with high hydrothermal stability and long-range order. After the material is roasted, the specific surface area of the material is 400 m<2> / g to 1,200 m<2> / g, and the pore volume is 0.1 cm<3> / g to 1.3 cm<3> / g. After being refluxed for 500 hours by boiling water, the material still maintains about 80 percent of specific surface area and pore volume.

Description

Technical field [0001] The field of the invention belongs to the field of synthesis and application of mesoporous materials, and the specific application fields are adsorption, catalysis, macromolecular reactions, nano-assembly, etc. Background technology [0002] Mesoporous silica molecular sieve has a large specific surface area, high thermal stability, ordered pore channels, and adjustable pore size. It has broad application prospects in adsorption, separation, catalytic conversion of macromolecules, and nano-assembly. It has attracted much attention since it was reported in 1992. focus on. However, compared with microporous molecular sieves, silica mesoporous materials have lower hydrothermal stability and are currently difficult to meet the stringent requirements of industrial catalytic cracking. In response to this situation, U.S. 20020128066, U.S. 20020128093, U.S. 20020128388, and CN01135624.3 reported the use of seed solutions of microporous molecular sieves instea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 刘子玉杨彬彬许宁韩红杰孙家香谈赟
Owner SHANGHAI NOVEL CHEM TECH
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