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Bisamide chain organosilicon quaternary ammonium salt compound and preparation and application thereof

A technology of organosilicon quaternary ammonium salt and bisamide chain, which is applied in the field of surfactant and its preparation, can solve the problems of poor hydrothermal stability of molecular sieve and single structure of mesoporous molecular sieve, and achieves the improvement of pore volume and specific surface area, wide application The effect of uniform foreground and pore size distribution

Inactive Publication Date: 2015-04-22
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 Problems to be solved by quaternary ammonium cationic surfactants

Method used

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  • Bisamide chain organosilicon quaternary ammonium salt compound and preparation and application thereof
  • Bisamide chain organosilicon quaternary ammonium salt compound and preparation and application thereof
  • Bisamide chain organosilicon quaternary ammonium salt compound and preparation and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Bisamide chain organosilicon quaternary ammonium compound, its chemical structural formula is:

[0033]

[0034] where X - for I - , m is 6, n=3.

[0035] Preparation method: Add 7.6g of capric acid and 2.9g of N,N-bis(3-aminopropyl)methylamine into a 250mL three-necked flask, and then add 50mL of toluene. The temperature was raised to 140°C and the reaction was stirred for 17h. After the reaction was complete, cool down and evaporate toluene to dryness. Add 60 mL of n-hexane for recrystallization, and filter to obtain 9.3 g of white powder tertiary amine intermediate.

[0036] Add 0.7g of the above-mentioned intermediate and 0.72g of 3-iodopropyltrimethoxysilane into a 50mL round-bottomed flask, slowly heat to 100°C, and react for 36h. 0.83 g of the above-mentioned bisamide chain organosilicon quaternary ammonium salt compound.

Embodiment 2

[0038] Bisamide chain organosilicon quaternary ammonium compound, its chemical structural formula is:

[0039]

[0040] where X - for I - , m is 8, n=3.

[0041] Preparation method: Add 11.2g of lauric acid and 2.9g of N,N-bis(3-aminopropyl)methylamine into a 250mL three-necked flask, and then add 70mL of xylene. The temperature was raised to 165°C and the reaction was stirred for 10h. After the reaction was complete, cool down and evaporate xylene to dryness. 85 mL of n-hexane was added for recrystallization, and 10.5 g of a white solid tertiary amine intermediate was obtained by filtration.

[0042]Add 1.3g of the above-mentioned intermediate and 1.16g of 3-iodopropyltrimethoxysilane into a 50mL round-bottomed flask, slowly heat to 120°C, and react for 72h. 1.74 g of the above bisamide chain organic silicon quaternary ammonium salt compound was obtained.

Embodiment 3

[0044] Synthesis of multi-level porous MFI structure zeolite molecular sieve: Add 0.163g aluminum isopropoxide, 8.13g tetrapropylammonium hydroxide, 8.33g tetrapropylammonium hydroxide and 60mL deionized water into a three-necked flask, stir for 30min, and wait for the dissolution to complete Then, 0.74 g of the bisamide chain organosilicon quaternary ammonium salt in Example 1 was added into the reaction flask in batches, and the stirring was continued at room temperature for 2 h. After the stirring was completed, the mixed solution in the reaction bottle was poured into a polytetrafluoro-lined stainless steel reaction kettle, and hydrothermally crystallized at 150° C. for 3 days. Cool, filter with suction, and wash repeatedly with deionized water until the pH is about 7. The product was dried at 100°C for 4h, and then calcined in a muffle furnace at 600°C for 5h. That is, the multi-level porous MFI structure zeolite molecular sieve, its BET surface area is 401.52m 2 g -1 ...

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Abstract

The invention relates to a bisamide chain organosilicon quaternary ammonium salt compound and preparation and application of the bisamide chain organosilicon quaternary ammonium salt compound and. The chemical structural formula (please see the formula in the specification) is provided, wherein X- is C1- or Br- or I-, m is any integer ranging from one to eighteen, and n is any integer ranging from one to five; the preparation comprises the steps of firstly, mixing N, N-double methylamine (3- aminopropyl) and fatty acid; secondly, adding solvent and performing temperature reaction to obtain a tertiary amine intermediate; finally, mixing the tertiary amine intermediate and halogen alkyl trimethoxysilane and performing temperature reaction; thirdly, the double amide chain organosilicon quaternary ammonium salt compound is obtained. The bisamide chain organosilicon quaternary ammonium salt compound can be applied to the preparation of hierarchical zeolite. The hierarchical zeolite prepared by the bisamide chain organosilicon quaternary ammonium salt compound can improve the pore volume and specific surface area of zeolite molecular sieve, effectively regulate the pore diameter and pore volume of hierarchical porous molecular sieve through changing the number of carbon atoms of double amide group chain, and further regulate and control the morphology of the hierarchical zeolite through the molar ratio of silicon dioxide in mother-liquid of quaternary ammonium cation surface active agents and the zeolite molecular sieve.

Description

technical field [0001] The invention belongs to the field of surfactants and their preparation, in particular to a bisamide chain organic silicon quaternary ammonium compound and its preparation 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 is increasing. The petrochemical industry urgent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18B01F17/18B01F17/54C01B39/04C01B39/40C09K23/18C09K23/54
Inventor 刘栋良赵飞
Owner DONGHUA UNIV
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