Diester-based fat chain organosilane quaternary ammonium salt compound and preparation method and application thereof

An organosilane and quaternary ammonium salt technology, applied in the field of quaternary ammonium salt compounds and their preparation, can solve the problems of poor hydrothermal stability of molecular sieves and single structure of mesoporous molecular sieves, improve internal diffusion limitation, increase pore volume and The effect of specific surface area, macropore volume and specific surface area

Inactive Publication Date: 2016-06-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the mesoporous molecular sieve synthesized by using long-chain alkyl quaternary ammonium salt type cationic surfactant as a template has a single structure, and the pore wall is thin, and the hydrothermal stability of the synthesized molecular sieve is poor, so these problems are the development of new The problem to be solved by quaternary ammonium cationic surfactants (Davis.OrderedPorousMaterialsForEmergingApplications[J].Nature,2002,417(40):813-821)

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  • Diester-based fat chain organosilane quaternary ammonium salt compound and preparation method and application thereof
  • Diester-based fat chain organosilane quaternary ammonium salt compound and preparation method and application thereof
  • Diester-based fat chain organosilane quaternary ammonium salt compound and preparation method and application thereof

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Embodiment 1

[0035] The diester-based aliphatic chain organosilane quaternary ammonium compound of the present embodiment has a chemical structural formula of:

[0036] where X - for I - , m=3, n=6.

[0037] Preparation method: Add 15.63g of capric acid and 3.57g of N-methyldiethanolamine into a 250mL three-necked flask, and then add 150mL of toluene. The temperature was raised to 150°C and the reaction was stirred for 17h. After the reaction was complete, cool down and evaporate toluene to dryness. Then add 120mL of dichloromethane to dissolve, wash with alkali, wash with water, evaporate the dichloromethane to dryness, separate and purify by column chromatography, and obtain the above-mentioned light yellow diester chain intermediate product.

[0038]Add 1.10g of the above-mentioned intermediate and 0.94g of 3-iodopropyltrimethoxysilane into a 50mL round bottom flask, slowly heat to 100°C, and react for 12h. The mixed solvent was washed twice to obtain the above-mentioned diester-...

Embodiment 2

[0040] The diester-based aliphatic chain organosilane quaternary ammonium compound of the present embodiment has a chemical structural formula of:

[0041] where X - for I - , m=3, n=8.

[0042] Preparation method: Add 15.63g of lauric acid and 3.57g of N-methyldiethanolamine into a 250mL three-necked flask, and then add 150mL of toluene. The temperature was raised to 150°C and the reaction was stirred for 19h. After the reaction was complete, cool down and evaporate toluene to dryness. Then add 120mL of dichloromethane to dissolve, wash with alkali, wash with water, evaporate the dichloromethane to dryness, separate and purify by column chromatography, and obtain the above-mentioned light yellow diester chain intermediate product.

[0043] Add 1.21g of the above-mentioned intermediate and 0.94g of 3-iodopropyltrimethoxysilane into a 50mL round-bottomed flask, slowly heat to 100°C, and react for 12h. The mixed solvent was washed three times to obtain the above-mentioned...

Embodiment 3

[0045] Diester-based aliphatic chain organosilane quaternary ammonium compound, its chemical structural formula is:

[0046] where X - for I - , m=3, n=10.

[0047] Preparation method: Add 17.81g of myristic acid and 3.57g of N-methyldiethanolamine into a 250mL three-necked flask, and then add 150mL of toluene. The temperature was raised to 150°C and the reaction was stirred for 19h. After the reaction was complete, cool down and evaporate toluene to dryness. Then add 120mL of dichloromethane to dissolve, wash with alkali, wash with water, evaporate the dichloromethane to dryness, separate and purify by column chromatography, and obtain the above-mentioned light yellow diester chain intermediate product.

[0048] Add 1.35g of the above-mentioned intermediate and 0.94g of 3-iodopropyltrimethoxysilane into a 50mL round-bottomed flask, slowly heat to 100°C, and react for 12h. The mixed solvent was washed 5 times to obtain the above-mentioned diester-based aliphatic chain o...

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Abstract

The invention relates to a diester-based fat chain organosilane quaternary ammonium salt compound and a preparation method and application thereof. The structural formula of the compound can be found in description, wherein m is an arbitrary integer from 2 to 9, n is an arbitrary integer from 1 to 19, and X is Cl, Br or I. The preparation method includes the steps that N-methyldiethanolamine and fatty acid are subjected to a reaction for 1-24 hours at the temperature of 100-200 DEG C, a dichloromethane solution is added, washing, drying and column chromatography are conducted, and a diester-based fat chain midbody is obtained; then the diester-based fat chain midbody and halogen alkyl trimethoxy silane react for 1-24 hours at the temperature of 80-150 DEG C, cooling and washing are conducted, and the diester-based fat chain organosilane quaternary ammonium salt compound is obtained. The organosilane quaternary ammonium salt compound is applied to preparation of a ZSM-5 zeolite molecular sieve containing mesoporous. By the application of the quaternary ammonium salt compound, the pore volume and specific area of the ZSM-5 zeolite molecular sieve containing mesoporous are remarkably raised, and internal diffusion limit is improved; a specific template agent stabilizing framework is adopted so that the obtained molecular sieve can be applicable to a macromolecules reaction.

Description

technical field [0001] The invention belongs to the field of quaternary ammonium salt compounds and their preparation, in particular to a diester-based aliphatic chain organosilane quaternary ammonium salt compound and its preparation method and application. Background technique [0002] Zeolite molecular sieves are widely used as catalysts in petrochemical and fine chemical industries. Because of their unique adsorption and separation functions, they are also widely used in engineering and technical fields such as ion exchange, adsorption and separation, and environmental protection. However, traditional zeolite molecular sieves are mostly microporous (pore size less than 2nm), which is difficult to catalyze chemical reactions of macromolecules, so the application of microporous zeolite molecular sieves in the field of macromolecular catalysis is limited. Especially in today's global petroleum resources are becoming less and less, and the content of heavy oil in petroleum i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C01B39/40
CPCC01B39/40C07F7/1804
Inventor 刘栋良王一江
Owner DONGHUA UNIV
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