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Mesoporous silica resin and preparation method thereof

A technology of mesoporous silicon and resin is applied in the field of mesoporous silicon resin and its preparation, and achieves the effects of low glass transition temperature, environmental friendliness and easy availability of raw materials

Inactive Publication Date: 2012-04-18
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the difficulty of preparing silicone resin by this method lies in the selection and coordination of components such as inorganic precursors, surfactants, organic monomers, and organic solvents. At present, there is no relevant literature report on the preparation of mesoporous structures with ordered structures by self-assembly method. Silicone material

Method used

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  • Mesoporous silica resin and preparation method thereof
  • Mesoporous silica resin and preparation method thereof
  • Mesoporous silica resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Preparation of methylphenylsilane (MPS) resin solution

[0038] Put a 250ml four-necked flask equipped with a stirrer, dropping funnel, reflux condenser and thermometer in a water bath, add 100g of water and 65g of tetrahydrofuran into the four-necked flask, and stir well; add 8g of Ph 2 SiCl 2 , 18g PhSiCl 3 , 9g (CH 3 ) 2 SiCl 2 , 15g (CH 3 ) SiCl 3 , Mix these monomers evenly; raise the temperature of the four-necked flask to 50°C, start adding the mixture of monomers dropwise, control the temperature between 50~70°C, and complete the dropwise addition in 1 hour; continue stirring after the dropwise addition 30min; Pour the reaction product into a separatory funnel, let stand to separate the water layer, wash the solvent layer with 60°C distilled water for 4 times, and then neutralize the solvent layer with 0.01~0.05ml of NaOH with a concentration of 20~40wt% until neutral to obtain Prepolymer of silicone resin; vacuum distillation of silicone re...

Embodiment 2

[0039] Example 2 Preparation of Mesoporous Silicone Materials

[0040] By solvent evaporation-induced self-assembly (EISA) method, methylphenylsiloxane (MPS) was used as the resin matrix, and PDMS-PEO diblock copolymer was used as the template to synthesize the mesoporous silicone resin material. The steps were as follows: 1.0 g The PDMS-PEO block copolymer was dissolved in 20.0 g tetrahydrofuran (THF) solvent and stirred at 30-50 °C for 10 min to obtain a clear solution. A THF solution of 10.0 g of 30 wt % MPS resin was added. Continue stirring for 0.3–0.6 h, and transfer the mixture to a Petri dish. Volatilize at room temperature for 5-8 h to remove THF, and then thermally polymerize in an oven at 150 °C for 20-24 h. The product obtained was a pale yellow transparent layer or film material which was scraped off the evaporating dish and ground to a powder. The mesoporous silicone resin material was obtained by firing in a tube furnace at 300°C for 3-5 h under a nitrogen ...

Embodiment 3

[0041] Example 3 The structure of the obtained material was characterized by JEOL JEM2011 high-resolution transmission electron microscope (TEM) at an accelerating voltage of 200 kV. The sample preparation process is as follows: the powdered material is dissolved in ethanol to form a slurry state, and the slurry is hung on a copper net with a carbon film, and can be directly used for observation after drying. The TEM image of the obtained mesoporous silicone resin material is as follows image 3 shown. Depend on image 3 It can be seen that the average pore size of the obtained material is 25nm. It shows that the silicone resin material with a porous structure can be produced by using the PDMS-PEO block copolymer as a template.

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Abstract

The invention relates to a mesoporous silica resin. By using methyl phenyl siloxane (MPS) as a resin matrix, block polymer polydimethylsiloxane-polyoxyethylene (PDMS-PEO) as a template agent and tetrahydrofuran (THF) as a solvent, a solvent volatilization induced self-assembly method is carried out to prepare the mesoporous silica resin. The mesoporous silica resin has ordered and uniform mesoporous structure and large pore size; and the BET specific area, pore volume and average pore size are respectively 260-800m<2> / g, 0.15-0.50cm<3> / g and 5-50nm. In addition, the mesoporous silica resin has excellent high-temperature stability and frame stability, and still maintains the mesoporous structure after being subjected to 600 DEG C heat treatment for 1-3 hours, while the frame shrinkage after treatment is only 5-15%. The mesoporous silica resin material has wide application prospects in the fields of thermal protection systems, heat exchangers, catalysis, separation, light-weight structural materials and the like.

Description

Technical field [0001] The present invention involves the field of nanomaterial production technology, especially a medium silicon resin and its preparation methods. Background technique [0002] The orderly medium material refers to a type of porous solid material with a pore diameter of about 2 ~ 50 nm, an orderly structure, and an uniform pore diameter. According to the composition of its skeleton, it can be divided into inorganic medium materials and organic polymer media.At present, great progress has been made in the research of orderly inorganic medium materials, and orderly sihole silica and a variety of derivatives represented by SBA-15 and SBA-16 have been synthesized.However, there are fewer research reports of orderly medium polymers. This is mainly because the thermal stability and mechanical stability of the organic polymer skeleton are poor, and the pore wall is easy to deform and collapse during the preparation process.The orderly medium polymer not only has a hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08J9/36C08L83/04C08K3/36C08G77/04
Inventor 刘玉荣
Owner CHONGQING UNIV OF ARTS & SCI
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