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Process for preparing silicon material containing sulfonic group

A siliceous material, technology containing sulfonic acid groups, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, physical/chemical process catalysts, etc., can solve the problem of long sulfonation time, high price, sulfhydryl Eliminate problems such as shedding, achieve high conversion rate, no corrosion of equipment, and less pollution

Inactive Publication Date: 2007-04-11
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method effectively overcomes the disadvantages of expensive mercaptosilane, long sulfonation time, and easy oxidation of mercapto to disulfide bonds or falling off the surface of silicon materials during the oxidation process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Take commercially available silica gel 15g, in 50mL 6mol L -1 Soak in hydrochloric acid solution for 4 hours, wash with deionized water until neutral, and dry in a vacuum oven at 130°C for 2 hours before use.

[0042] Add 10g of dried silica gel, 4.75g of chloropropyltrichlorosilane, and 50ml of anhydrous cyclohexane into a dry three-necked flask, and stir for 14 hours at room temperature under a nitrogen atmosphere. The HCl generated during the reaction is absorbed by sodium hydroxide lye . After filtering, the filtrate was extracted by Soxhlet with cyclohexane as solvent for 4h. Vacuum drying at 60°C for 2 hours to obtain chloropropyl-silica gel, referred to as silica gel-CP.

[0043] Put 5g of silica gel-CP, 40ml of ammonium sulfite solution (concentration ≥ 25%), and 10ml of deionized water into a 100ml three-necked flask, and stir at 85°C for 3 hours. During the reaction, N 2 Protect. After filtration, rinse and filter with 50ml 1mol / L HCl and 100ml deionized w...

Embodiment 2

[0045]Put 1g of pure silicon SBA-15, 3.2g of chloropropyltrichlorosilane, and 100g of anhydrous cyclohexane into a 250ml three-necked flask, stir and reflux for 24h under the protection of nitrogen, and absorb the HCl produced during the reaction with sodium hydroxide lye . After the reaction was completed, it was filtered, and the filtrate was extracted by Soxhlet with cyclohexane for 4 hours. Vacuum drying at 60°C for 2 hours to obtain surface-modified molecular sieves containing chloropropyl groups, referred to as SBA-15-CP.

[0046] Put the obtained SBA-15-CP, 40ml ammonium sulfite solution (concentration ≥ 25%), and 10ml deionized water into a 100ml three-necked flask, stir at 85°C for 3 hours, and feed N 2 Protect. After the reaction is completed, filter, rinse and filter with 100ml of 1mol / L HCl to obtain a solid, and then wash with 100ml of deionized water to remove chloride ions. Vacuum drying at 65°C for 2 hours to obtain SBA-15-SO modified with sulfonic acid grou...

Embodiment 3

[0048] Add 25ml of 30% sulfuric acid, 100ml of SiO 2 2% sodium silicate solution, 1.36g chloropropyltriethoxysilane, 2 drops of N, N dimethylformamide, and stir. During stirring, 10 ml of a solution containing 1.5 g of sodium bisulfite was added dropwise, and the addition was completed within 30 minutes. Stir and react for 10 hours at 35°C and pH 3.5; let the sol naturally turn into a gel after standing still, then age for 36 hours at 30°C; wash with deionized water for 3 to 6 times, and dry in vacuum at 60°C for 2 hours , to get Silica-SO 3 H;

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Abstract

The present invention relates to two processes of preparing silicon material containing sulfo group. The first process has haloalkyl silicon material as the precursor, and includes sulfonation with basic sulfite or bisulfite as sulfonating agent and subsequent exchange of metal ion or ammonium ion with hydrogen ion to obtain silicon material containing sulfo group in the surface. The second process has bisulfite and haloalkyl silane added to produce hydrolysis of ethyl silicate or sodium silicate and the sulfonation of haloalkyl silane synchronously, so as to prepare silicon material containing sulfo group in one step. The present invention has relatively low material cost, short sulfonation time and other advantages, and the silicon material containing sulfo group may be used as catalyst for esterification, etc. and is superior to traditional concentrated sulfuric acid catalyst.

Description

technical field [0001] The invention relates to a method for preparing silicon materials, in particular to a method for preparing silicon materials containing sulfonic acid groups. Background technique [0002] Usually mesoporous silicone molecular sieve PMO-SO 3 H. SBA-15-SO 3 The synthesis of H is to introduce -SH to the surface of the silicon material by using mercaptosilane, and then oxidize -SH with hydrogen peroxide to obtain sulfonic acid groups. The medium of the oxidation reaction is hydrogen peroxide, methanol and aqueous solution, and stir at room temperature for 12 hours. This sulfonation method has certain defects: mercaptosilane is expensive, the sulfonation time is long, and mercapto groups are easily oxidized into disulfide bonds or fall off from the surface of silicon materials during the oxidation process. [0003] The sulfonic acid group on the mesoporous silicon molecular sieve functionalized with benzenesulfonic acid group is generally obtained by sulf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18B01J27/02B01J21/08
Inventor 苏继新屈文潘齐王晓鹏
Owner SHANDONG UNIV
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