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Process for preparing high specific surface area hetero phenyl silica-gel

A high specific surface area, silica gel technology, applied in chemical instruments and methods, silicon organic compounds, chemical recovery, etc., can solve the problems of large wastewater volume, high specific surface area, etc., and achieve the effect of easy operation

Inactive Publication Date: 2006-04-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method (F.Babonneau, L.Leite and S.Fontlupt, J.Mater.Chem., 1999, 9, 175.) that prepares the hybrid MCM-41 that contains phenyl group by template can't be used for preparing loading capacity too big phenyl hybrid silica gel, and the amount of wastewater generated is relatively large
Use the size of the inner core water in the inverse microemulsion to control the size of the hybrid silica particles to obtain a high specific surface area hybrid silica gel, and co-hydrolyze the organic substituted silicon source and ethyl silicate to prepare the hybrid silica gel containing phenyl groups on the outer surface Silica gel has not been reported so far

Method used

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  • Process for preparing high specific surface area hetero phenyl silica-gel
  • Process for preparing high specific surface area hetero phenyl silica-gel

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1 reverse phase microemulsion W 0 =30, phenyl substituted ethyl silicate / orthosilicate ethyl ester=1:2

[0024] Mix 50mL of heptane, 5.0mL of n-pentanol, 3.64g of CTAB (hexadecyltrimethylammonium bromide, hereinafter referred to as CTAB), and 5.4mL of 0.1M NaOH aqueous solution, and stir to clarify the material. Add a mixture of 5mL phenyl ethyl silicate and 10mL tetraethyl orthosilicate, heat up to a bath temperature of 60°C under stirring, continue stirring and maintain at this temperature for 12 hours, cool the material and lower the temperature of the material to room temperature, filter material, the filtrate is recovered, the filtrate is washed three times with acetone (25mL×3), and the filtrate is dried at room temperature, and its BET specific surface area is 272.4m 2 / g.

Embodiment 2

[0025] Embodiment 2 inverse microemulsion w 0 =30, phenyl substituted ethyl silicate / orthosilicate ethyl ester=1:5

[0026] Mix 50mL of heptane, 5.0mL of n-pentanol, 3.64g of CTAB, and 5.4mL of 0.1M NaOH aqueous solution, and stir to clarify the material. Add 2mL of ethyl phenyl silicate and 10mL of ethyl orthosilicate, heat up to bath temperature 60°C under stirring, continue to stir and maintain at this temperature for 12 hours, cool the material and let the temperature of the material drop to room temperature, filter material, the filtrate is recovered, the filtrate is washed three times with acetone (25mL×3), the filtrate is dried at room temperature, and its BET specific surface area is 500.8m 2 / g.

Embodiment 3

[0027] Embodiment 3 inverse microemulsion W 0 =30, phenyl substituted ethyl silicate / orthosilicate ethyl ester=1:10

[0028] Mix 50mL of heptane, 5.0mL of n-pentanol, 3.64g of CTAB, and 5.4mL of 0.1M NaOH aqueous solution, and stir to clarify the material. Add 2mL of ethyl phenyl silicate and 10mL of ethyl orthosilicate, heat up to 60°C under stirring, continue to stir and maintain at this temperature for 12 hours, cool the material and let the temperature of the material drop to room temperature, filter material, the filtrate is recovered, the filtrate is washed three times with acetone (25mL×3), the filtrate is dried at room temperature, and its BET specific surface area is 521.7m 2 / g.

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Abstract

Hetero phenyl silica gel with high specific surface area is prepared in inverse micro emulsion. In the stable inverse micro emulsion of cationic surfactant and fatty alcohol assistant, kernel water makes phenyl radical substitute and co-hydrolyze two kinds of silicon sources, tetraethyl silicate and tetraethyl metasilicate, and kernel water size is controlled to control the size of produced hetero material particles. Under optimized condition, the specific surface area of the produced hetero material may be greater than 500 se m / g.

Description

technical field [0001] The invention relates to a method for preparing a phenyl-containing hybrid silica gel with a high specific surface area, in particular to a method for preparing a phenyl-containing hybrid silica gel with a high specific surface area in an inverse microemulsion. technical background [0002] The phenyl-containing hybrid silica gel with high specific surface area is used as a support in chromatographic separation and the solid acid prepared by sulfonation is used as a catalyst for alkylation and acylation reactions. Because it is environmentally friendly and easy to separate, it is sometimes used as an example of green chemistry. reports. In the early days, people directly chlorinated the surface, and then reacted with Grignard reagent to introduce phenyl on the surface of silica gel (D.C.Locke, J.T.Schmermund and B.Banner, Anal.Chem., 1972, 44(1), 90.). However, the phenyl loading capacity of the hybrid silica obtained by this method is relatively low,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08B01J20/282
CPCY02P20/582
Inventor 李灿姜鹏李晓红应品良
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI