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Preparation method and applications of sulfydryl functionalized SBA molecular sieve

A molecular sieve and functionalization technology, which is applied in the field of preparation of modified SBA molecular sieves, can solve the problems of poor order degree and lower order degree of functionalized materials, and achieve good adsorption performance, improved performance and improved removal rate.

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 sulfydryl functionalized SBA molecular sieve
  • Preparation method and applications of sulfydryl functionalized SBA molecular sieve
  • Preparation method and applications of sulfydryl functionalized SBA molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] At 60°C, add 7.1g of F127 and 85.5g of deionized water into the reactor in turn, stir evenly, then add 79.2mL of 0.1mol / L hydrochloric acid solution, continue stirring, and slowly add 11g of ethyl orthosilicate dropwise (TEOS), the molar ratio of the obtained reaction mixture is SiO 2 : 90H 2 O: 0.01R: 0.15H + , the mixture was transferred to a crystallization kettle, heated to 80° C., and crystallized at a constant temperature for 30 h. The reacted mixture is separated, washed and dried at 100°C to obtain the original powder of SBA-16 molecular sieve. Take 5 g of the obtained SBA-16 molecular sieve powder and 0.0276 mol (3 g) of trimethylchlorosilane and stir for 3 h at 30 ° C, then mix the product with 0.0763 mol (15 g) of mercaptopropyltrimethoxysilane and 15 g of ethanol uniform, and stirred at 60°C for 4h, then mixed the product with 20g of methyl ether and stirred for 2h, filtered, washed and dried at 100°C and analyzed by BET, the specific surface area of ​​th...

Embodiment 2

[0042] 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 17.4g, the amount of water is changed to 108g, and the silicon source is changed to white carbon black (silicon dioxide content is 90wt% ), the dosage is 4g, the acid is changed to sulfuric acid, the dosage is 60mL, the crystallization temperature is changed to 90°C, the crystallization time is changed to 50h, the drying temperature is changed to 110°C, the passivating agent is changed to dimethyldichlorosilane, the dosage Change it to 0.0162mol (2.1g), change the passivation temperature to 50°C, change the passivation time to 5h, change the mercapto modifier to 3-(phenylmercapto)propyltrimethoxysilane, and change the dosage to 0.0364mol ( 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 dos...

Embodiment 3

[0045] The difference from Example 1 is that the feeding temperature is changed to 50°C, the stencil agent is changed to HMTA, the dosage is 0.08g, the amount of water is changed to 60g, and the silicon source is changed to silica sol (SW-25, silicon dioxide content 25wt%), the dosage is 5g, the acid source is changed to nitric acid, the dosage is 52.1mL, 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 was changed to 0.0049mol (1.25g), the passivation temperature was changed to 60°C, the passivation time was changed to 6h, the mercapto modifier was changed to ethanethiol, and the dosage was changed to 0.0804mol (5g). The 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 ether, the amount was changed to 10...

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Abstract

The invention relates to a sulfydryl 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 a sulfydryl modifier, carrying out amodification 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 extractionagent, extracting, removing the liquid phase, and drying the solid phase to obtain the sulfydryl functionalized SBA molecular sieve. According to the method of the invention, the pore channel structure and the crystallinity of the molecular sieve cannot be damaged, and the sulfydryl 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 a mercapto functionalized SBA molecular sieve. Background technique [0002] SBA molecular sieve is a mesoporous material with a pore size of 2-50nm. It has potential application prospects in the fields of catalysis, adsorption, separation, biological materials, energy and environment, especially in biological separation and functional materials. . From the research on the surface chemical properties of mesoporous materials, it can be known that the silanol groups on the surface and pores of mesoporous silica materials have certain chemical reactivity, which is the basis of chemical modification. People consciously carry out various modifications on the surface and pores of SBA-15 and SBA-16 molecular sieves to meet different requirements in practical applications. [0003] The organic functional modification of the inner and outer su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48B01J20/18
CPCC01B39/48B01J20/18C01P2002/72C01P2002/82C01P2006/12
Inventor 吴凯任行涛贾志光赵岚刘艳惠杨光
Owner CHINA PETROLEUM & CHEM CORP