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Method for preparing functional amido silicon dioxide

A silicon dioxide and functionalization technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of complex requirements for reaction instruments and equipment, cumbersome operation, etc., and achieve easy operation and preparation methods Simple, mild preparation conditions

Inactive Publication Date: 2007-10-24
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has complex requirements on reaction instruments and equipment, and the operation is cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] 5.0 g of chloropropyltrimethoxysilane was added to 30 g of cyclohexane to prepare a solution, and 3.0 g of silica was added to it after ultrasonic wave (operating frequency 50 KHz) dispersed uniformly, and sealed. The working frequency of this reaction system was 50KHz ultrasonic oscillation for 1 hour. The samples were extracted with toluene for 8 hours and vacuum dried at 100°C for 8 hours. That is to get Cl / SiO 2 . Then 1.0g of tetrahydropyrrole was added to 30g of cyclohexane solution, and the working frequency was 50KHz ultrasonic wave to disperse uniformly, and then the above 3.0gCl / SiO 2 Immerse in it and seal. The working frequency of this reaction system was 50KHz ultrasonic oscillation for 0.5 hours. The samples were extracted with toluene for 8 hours and vacuum dried at 100°C for 8 hours. That is to obtain tetrahydropyrrole functionalized silica (tetrahydropyrrole / SiO 2 ). The mass percentage content of C, H, N elements of the sample was determined by ...

Embodiment 2

[0013] 5.0 g of chloropropyltrimethoxysilane was added to 33 g of cyclohexane to prepare a solution, 3.3 g of silica was added to it after ultrasonic wave (working frequency 40KHz) dispersed uniformly, and sealed. The reaction system was oscillated with ultrasonic waves (working frequency 40KHz) for 1.3 hours. The samples were extracted with toluene for 9 hours and vacuum dried at 95°C for 9 hours. That is to get Cl / SiO 2 . Then 1.5g of hexahydropyridine was added to 30g of cyclohexane solution, and the above 3.3g of Cl / SiO was dispersed uniformly by ultrasonic wave (working frequency 40KHz). 2 Immerse in it and seal. The reaction system was oscillated with ultrasonic waves (working frequency 40KHz) for 0.7 hours, the samples were extracted with toluene for 9 hours, and vacuum dried at 95°C for 9 hours. That is to obtain hexahydropyridine functionalized silica (hexahydropyridine / SiO 2 ). The mass percentage content of C, H, N elements of the sample was determined by elem...

Embodiment 3

[0015] 5.0 g of chloropropyltrimethoxysilane was added to 37 g of cyclohexane to prepare a solution, 3.7 g of silica was added to it after ultrasonic wave (working frequency 28KHz) dispersed uniformly, and sealed. The reaction system was oscillated with ultrasonic waves (working frequency 28KHz) for 1.7 hours. The samples were extracted with toluene for 11 hours and dried under vacuum at 85°C for 11 hours. That is to get Cl / SiO 2 . Then 1.8g TBD was added to 30g cyclohexane solution, and the above 3.7gCl / SiO 2 Immerse in it and seal. The reaction system was oscillated with ultrasonic waves (working frequency 28KHz) for 0.8 hours. The samples were extracted with toluene for 11 hours and dried under vacuum at 85°C for 11 hours. That is to obtain TBD functionalized silica (TBD / SiO 2 ). The mass percentage content of C, H, N elements of the sample was determined by elemental analyzer. The results are shown in Table 1.

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Abstract

A process for preparing the amino functionated SiO2 includes such steps as preparing cyclohexane solution of chloropropylmethoxy silane, ultrasonic dispersing, immersing SiO2 in it, sealing, ultrasonic oscillation, extracting in toluene, vacuum drying to obtain the chloropropyl functionated SiO2, preparing cyclohexane solution of organoamine, ultrasonic dispersing, immersing said chloropropyl functionated SiO2 in it, sealing, ultrasonic oscillation, extracting in toluene, and vacuum drying.

Description

technical field [0001] The invention belongs to a preparation method of amine-based functionalized silica. Background technique [0002] In the past decade, the immobilization of different homogeneous organic amines has become one of the research hotspots of researchers and has achieved rapid development. Immobilized organic amines are widely used in the fields of catalysis, adsorption, separation, host-guest chemistry, and preparation of functional materials. At present, the raw materials required for the preparation of grafted organic solid bases are mainly organosilane coupling agents and weak polarities. Solvents (such as toluene, xylene, dichloromethane, chloroform and cyclohexane, etc.), and the carrier is a metal oxide with hydroxyl groups on the surface mainly composed of silicon-based mesoporous molecular sieve and silica. In the traditional preparation method, the reaction system is mainly heated, refluxed, and stirred. In order to improve the degree of condensati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J21/08B01J37/00
Inventor 孙予罕魏伟张雪红
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI