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Preparation method and applications of amino-functionalized SBA molecular sieve

A technology of amino functionalization and molecular sieves, which is applied in the field of preparation of modified SBA molecular sieves, can solve the problems of reduced order degree and poor order degree of functionalized materials, and achieve the effect of improving performance

Pending 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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  • Preparation method and applications of amino-functionalized SBA molecular sieve
  • Preparation method and applications of amino-functionalized SBA molecular sieve
  • Preparation method and applications of amino-functionalized SBA molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] At 60°C, add 3.5g of F127 and 76g of deionized water into the reactor in turn, stir well, then add 53mL of 0.1mol / L hydrochloric acid solution, continue stirring, and slowly add 11g of ethyl orthosilicate (TEOS ), the molar ratio of the obtained reaction mixture is SiO 2 : 80H 2 O: 0.005R: 0.1H + , the mixture was transferred to a crystallization kettle, heated to 90° C., and crystallized at a constant temperature for 40 h. The reacted mixture is separated, washed and dried at 100°C to obtain the original powder of SBA-16 molecular sieve. Take 5g of the obtained SBA-16 molecular sieve powder and 0.0276mol (3g) of trimethylchlorosilane and stir for 4h at 40°C, then mix the product with 0.0587mol (15g) of 3-(phenylamino)propyltrimethoxy Mix base silane and 15g of ethanol uniformly, and stir at 60°C for 4h, then mix the product with 20g of methyl ether and stir for 2h, filter, wash and dry at 100°C and analyze by BET, The specific surface area of ​​the resulting produc...

Embodiment 2

[0037] The difference from Example 1 is that the feeding temperature is changed to 40°C, the template agent is changed to F108, the consumption is 10.9g, the amount of water is changed to 135g, and the silicon source is changed to white carbon black (silicon dioxide content is 90wt% ), the dosage is 5g, the acid is changed to sulfuric acid, the dosage is 112mL, the crystallization temperature is changed to 100°C, the crystallization time is changed to 50h, the drying temperature is changed to 110°C, the passivating agent is changed to dimethyldichlorosilane, and the dosage Change it to 0.0162mol (2.1g), change the passivation temperature to 50°C, change the passivation time to 5h, change the amino modifier to 3-aminopropyltriethoxysilane, and change the dosage to 0.0451mol (10g), The modification temperature was changed to 80°C, the modification time was changed to 5h, the amount of ethanol was changed to 10g, the extraction agent was changed to diethyl ether, the dosage was ch...

Embodiment 3

[0040] The difference from Example 1 is that the feeding temperature is changed to 50°C, the template agent is changed to HMTA, the dosage is 0.15g, the amount of water is changed to 82.5g, and the silicon source is changed to silica sol (SW-25, silicon dioxide The content is 25wt%), the dosage is 10g, the acid source is changed to nitric acid, the dosage is 83mL, the crystallization temperature is changed to 110°C, the crystallization time is changed to 60h, the drying temperature is changed to 120°C, and the passivating agent is changed to diphenyl Dichlorosilane, the dosage is changed to 0.0049mol (1.25g), the passivation temperature is changed to 60°C, the passivation time is changed to 6h, the amino modifier is changed to 3-aminopropyltrimethoxysilane, and the dosage is changed to 0.0278mol (5g), the modification temperature was changed to 90°C, the modification time was changed to 6h, the amount of ethanol was changed to 5g, the extraction agent was changed to diethyl eth...

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Abstract

The invention relates to an amino-functionalized SBA molecular sieve preparation method, which comprises: S1, providing SBA molecular sieve raw powder, wherein preferably an organic template agent, water, a silicon source and an acid are mixed to form a gel, the gel-formed mixture is subjected to hydrothermal crystallization, solid-liquid separation is performed, and the separated solid phase is washed and dried to provide the SBA molecular sieve raw powder; S2, mixing the SBA molecular sieve raw powder and a passivator, carrying out passivation, adding an amino modifier, carrying out a modification reaction, performing solid-liquid separation on the product, and washing and drying the separated solid sample; and S3, mixing the dried product obtained in the step S2 and an extraction agent,extracting, removing the liquid phase, and drying the solid phase to obtain the amino-functionalized SBA molecular sieve. According to the method of the invention, the pore channel structure and thecrystallinity of the molecular sieve cannot be damaged, and the amino can be uniformly grafted in the molecular sieve pore channels.

Description

technical field [0001] The invention provides a method for preparing a modified SBA molecular sieve, in particular to a method for preparing an amino-functionalized SBA molecular sieve and its application. Background technique [0002] Since Mobil Corporation successfully synthesized regular MCM-41 for the first time in 1992, mesoporous materials have shown many potential applications in adsorbents, catalysts and catalyst supports. In 1998, for the first time, Zhao Dongyuan successfully synthesized new mesoporous materials SBA-15 and SBA-16, which have larger specific surface area, regular pore size distribution, thicker pore walls and better thermal stability than M41S molecular sieves. This material has shown greater application value in catalysts. Compared with conventional M41S series molecular sieves, the three-dimensional channels can make it easier for reactants to enter the interior of the molecular sieve for reaction without causing blockage of the molecular sieve ...

Claims

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Application Information

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IPC IPC(8): C01B39/04C01B39/02B01J20/18
CPCC01B39/04C01B39/026B01J20/186C01P2002/72C01P2002/82C01P2006/12
Inventor 吴凯任行涛贾志光赵岚刘艳惠杨光
Owner CHINA PETROLEUM & CHEM CORP