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Preparation method of alkylated silica gel

A technology of alkylated silica gel and silica gel, applied in the directions of silica and silica, can solve the problems of uneven and regular surface polymerization layer, multi-layer structure, blockage of silica gel pores, etc., to achieve the best stability and anti-hydrolysis performance, operation Simple, low-labor effect

Inactive Publication Date: 2007-09-26
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this synthesis method first partially hydrolyzes the silane coupling agent in an organic solvent, and then grafts it on the surface of silica gel, which will inevitably lead to condensation reaction of some silanol groups when the silane coupling agent enters the surface of silica gel for grafting reaction. The surface polymerization layer is uneven and regular, and multi-layer structure is easy to appear, which is more likely to cause the condensation polymer of silane coupling agent to block the silica gel channel and other problems.

Method used

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  • Preparation method of alkylated silica gel
  • Preparation method of alkylated silica gel
  • Preparation method of alkylated silica gel

Examples

Experimental program
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Embodiment 1

[0025] The particle size of raw silica gel is 40-60 mesh, the average pore size is 11-12nm, and the surface area is 430m 2 / g, bulk density 0.43g / mL; chloropropyltrichlorosilane is the coupling agent, the molecular formula is Cl(CH 2 ) 3 SiCl 3 , at 20°C, the specific gravity r = 1.359-1.360; the synthesis method and preparation process of alkylated silica gel are as follows:

[0026]

[0027] 1. Preparation of activated silica gel: Add 200 grams of silica gel with a particle size of 40-60 mesh into the pickling kettle, add 800 mL of HNO with a concentration of 1 mol / L 3 The solution was boiled for 6 hours at boiling point temperature (bubble point temperature 103°C). After the pickling step, the reaction solution was immediately filtered through a sand core funnel, the silica gel was washed successively with pure water and methanol to make the pH reach 6, and then dried in an oven at 100°C to constant weight.

[0028] 2. Preparation of hydrated silica gel: Put the acti...

Embodiment 2

[0036]The particle size of raw silica gel is 16-80 mesh, the average pore diameter is 15nm, and the bulk density is 0.463g / mL; chloropropyltrichlorosilane is the coupling agent, and the molecular formula is Cl(CH 2 ) 3 SiCl 3 , at 20°C, the specific gravity r=1.359-1.360; the preparation process of alkylated silica gel is as follows:

[0037] 1. Preparation of activated silica gel: Add 10Kg of pre-dried microspherical silica gel directly into the enamel stirring pickling kettle with a volume of 50L, measure and add 40L of hydrochloric acid solution with a concentration of 1mol / L, and then add it at boiling point temperature and stirring speed of 54rpm. Boil at reflux for 6 hours. The acid-containing vapor evaporated from the pickling kettle is condensed by the glass condenser and returned to the pickling kettle in time. After filtering and washing, dry at 100~120°C until constant weight.

[0038] 2. Preparation of hydrated silica gel: put 10Kg of silica gel after pickling ...

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Abstract

The invention discloses a silica gel and inorganic material power surface modify and preparing method, especially involves a preparing method of alkylated silica gel. The preparing method of alkylated silica gel includes the preparation of activated silica gel, hydrated silica gel and alkylated silica gel. The alkylated silica gel possess good stability and hydrolytic stability, which can be used as water treatment agent, gas adsorbent, absorptive parting material, bulk additive and activator.

Description

technical field [0001] The invention relates to a surface modification of silica gel and inorganic material powder and a preparation method thereof, in particular to a preparation method of monomolecular layer organic polymer bonded alkylated silica gel. Background technique [0002] Alkylated silica gel is a functional material that uses silica gel as the skeleton material and grafts various organic groups on its surface through surface silanization treatment. It can be used as water treatment agent, gas adsorbent, adsorption and separation material, catalyst and chromatography. Carrier and other materials are used. In the field of chromatography, the alkylated bonded silica gel stationary phase is the main filler used in the reverse liquid chromatography analysis method. Due to factors such as steric hindrance during its synthesis, the end-capping technology cannot completely eliminate the influence of the silanol group, resulting in When polar compounds are used, the chr...

Claims

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Application Information

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IPC IPC(8): C01B33/14
Inventor 范忠雷李殿卿刘大壮
Owner ZHENGZHOU UNIV