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Organic functional group functionalized MCM molecular sieve preparation method

A technology of organic functional groups and molecular sieves, which is applied in the direction of molecular sieve catalysts, molecular sieve compounds, chemical instruments and methods, etc., can solve the problems of poor order degree and reduced order degree of functional materials, and achieve reduced yield, reduced production cost, The effect of saving process

Active Publication Date: 2019-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the functionalized materials prepared by the co-condensation method usually have the disadvantage of poor order, and the order will decrease with the increase of the amount of organic groups introduced.

Method used

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  • Organic functional group functionalized MCM molecular sieve preparation method
  • Organic functional group functionalized MCM molecular sieve preparation method
  • Organic functional group functionalized MCM molecular sieve preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Under the condition of 30°C, 2.1g of cetyltrimethylammonium bromide (CTAB) and 83g of deionized water were successively added into the reactor, stirred evenly, and then 12g of tetraethylorthosilicate (TEOS ), finally adding 4.6g NaOH to adjust the pH of the solution is 10~11, and the molar ratio of the obtained reaction mixture is SiO 2 : 80H 2 O: 0.1R: 2OH - , the mixture was transferred to a crystallization kettle, heated to 110° C., and crystallized at a constant temperature for 72 hours. After the crystallization is complete, when the temperature drops to room temperature, add 6.2g of metasilicate to the mother liquor after crystallization, stir and mix for 1 hour, and measure that the content of CTAB drops to 700ppm, then the reacted mixture is separated, washed, and heated at 100°C Drying under low temperature can get the original powder of MCM-41 molecular sieve. Take 5g of the obtained MCM-41 molecular sieve powder and 0.0193mol (2.1g) trimethylchlorosilane a...

Embodiment 2

[0038] The difference from Example 1 is that the feeding temperature is changed to 40°C, the template agent is changed to cetyltrimethylammonium chloride (CTAC), the dosage is 9.5g, the amount of water is changed to 121.6g, and the silicon source Sodium silicate was changed to 12g, the amount of NaOH was changed to 11.8g, the crystallization temperature was changed to 140°C, the crystallization time was changed to 108h, the weak acid was changed to sulfurous acid, and the dosage was 10.8g, and the measured CTAC content was reduced to 500ppm, the drying temperature was changed to 140°C, the passivating agent was changed to dimethyldichlorosilane, the dosage was changed to 0.0043mol (0.56g), the passivation temperature was changed to 90°C, the passivation time was changed to 10h, and the organic functional group was modified The agent was changed to ethynyltrimethylsilane, the dosage was changed to 0.0510mol (5g), the modification temperature was changed to 120°C, the modificatio...

Embodiment 3

[0040] The difference from Example 1 is that the feeding temperature is changed to 50°C, the stencil agent is changed to cetyltrimethylammonium chloride (CTAC), the consumption is 7.4g, the amount of water is changed to 165.9g, and the amount of TEOS The amount is changed to 16g, the alkali source is changed to ammonia water, the dosage is 10.7g, the crystallization temperature is changed to 130°C, the crystallization time is changed to 90h, the weak acid is changed to formic acid, the dosage is 16g, the measured CTAC content is reduced to 150ppm, and the drying temperature Change to 120°C, change the passivation agent to diphenyldichlorosilane, change the dosage to 0.0049mol (1.25g), change the passivation temperature to 60°C, change the passivation time to 5h, and change the organic functional group modifier to six Methyl disiloxane, the amount was changed to 0.0617mol (10g), the modification temperature was changed to 90°C, the modification time was changed to 6h, the amount...

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Abstract

The invention discloses an organic functional group functionalized MCM molecular sieve preparation method, which comprises: S1, mixing an organic template agent, water, a silicon source and an alkalisource to form a gel, and carrying out hydrothermal crystallization on the gel mixture to obtain a crystallization liquid mother liquor; S2, mixing the crystallization liquid mother liquor and a weakly acidic substance, carrying out solid-liquid separation on the product, and washing and drying the separated solid phase to obtain MCM molecular sieve raw powder; and S3, mixing the MCM molecular sieve raw powder and a passivator, carrying out passivation, adding an organic functional group modifier, carrying out a modification reaction, carrying out solid-liquid separation on the product, and washing and drying the separated solid sample to obtain the organic functional group functionalized MCM molecular sieve. According to the invention, the organic functional groups of the molecular sieveprepared by the method are uniformly dispersed in the pore channels of the molecular sieve.

Description

technical field [0001] The invention provides a method for preparing a modified molecular sieve, in particular to a method for preparing an organic functional group functionalized MCM molecular sieve. Background technique [0002] Since the mesoporous molecular sieve MCM-41 was synthesized in the early 1990s, due to its special properties and structure, it has become the most studied type of mesoporous silicon-based materials. Its remarkable characteristics are: regular hexagonal pore structure, narrow pore size distribution, extremely high specific surface area, thick pore wall, adjustable pore size, high chemical stability and hydrothermal stability. Organofunctionalization of mesoporous materials has attracted extensive attention from researchers in materials, physics, chemistry and other disciplines in the past decade. This type of material has the complementary characteristics of mesoporous materials and organic groups: the organic groups provide the desired surface pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03C01B37/00
CPCB01J29/0308C01B37/005
Inventor 吴凯任行涛项迎春贾志光赵岚刘艳惠杨光
Owner CHINA PETROLEUM & CHEM CORP