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Oligo-Ethyl Silicate Using a Strong Acid Heterogeneous Polymerization Catalyst

A technology of ethyl silicate and tetraethyl orthosilicate, applied in glass forming, glass manufacturing equipment, manufacturing tools, etc., can solve problems such as catalyst pollution products and difficulties

Inactive Publication Date: 2015-09-23
国防研究与发展组织
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The major disadvantages of reactions using homogeneous catalysts are the contamination of the product due to the presence of the catalyst (e.g. sulfuric acid) and the need for additional difficult and expensive unit critical) treatment to remove catalyst, disposal of waste generated by said treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] In a stoppered plastic container, 9.020 g (0.0433 mol) of tetraethyl orthosilicate with a silicon dioxide content of 28% and 0.05 g (0.0028 mol) of water are taken. To the reaction mixture was added 1.032 g of a surface area of ​​330 m synthesized using a high internal phase emulsion polymerization methodology 2 / g of sulfonated poly(styrene-divinylbenzene) catalyst. The reaction mixture was heated at 60 °C for a period of 10 hours. The reaction mixture was then analyzed for tetraethylorthosilicate and ethanol by gas chromatography (GC). The reaction mixture was then filtered to remove the heterogeneous catalyst, followed by distillation to remove ethanol. Relative to ethyl silicate, 33.3% hydrolysis was achieved, and the silica content was measured gravimetrically at about 30%.

Embodiment 2

[0082] In a stoppered plastic container, 9.020 g (0.0433 mol) of tetraethyl orthosilicate and 0.100 g (0.0056 mol) of water are taken. To the reaction mixture was added 1.032 g of sulfonated poly(styrene-divinylbenzene) synthesized using high internal phase emulsion polymerization methodology. The reaction mixture was heated at 60 °C for a period of 10 hours. The reaction mixture was then analyzed for tetraethylorthosilicate and ethanol by gas chromatography (GC). The reaction mixture was then filtered to remove the heterogeneous catalyst, followed by distillation to remove ethanol. Relative to ethyl silicate, 46% hydrolysis was achieved, and the silica content, measured gravimetrically, was found to be about 32%.

Embodiment 3

[0084] In a stoppered plastic container, 9.020 g (0.0433 mol) of tetraethylorthosilicate and 0.201 g (0.0112 mol) of water are taken. To the reaction mixture was added 1.032 g of sulfonated poly(styrene-divinylbenzene) synthesized using high internal phase emulsion polymerization methodology. The reaction mixture was heated at 60 °C for a period of 10 hours. The reaction mixture was then analyzed for tetraethylorthosilicate and ethanol by gas chromatography (GC). The reaction mixture was then filtered to remove the heterogeneous catalyst, followed by distillation to remove ethanol. Relative to ethyl silicate, 50% hydrolysis was achieved, and the silica content, measured gravimetrically, was found to be about 34%.

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Abstract

The present invention provides a process for the synthesis of ethyl silicate with varying silica concentration, by hydrolysing ethyl silicate in varying water concentration in the presence of sulfonated catalysts having a styrene-divinyl benzene backbone. The present invention further relates to the preparation of beaded crosslinked polymers containing sulfonic acid moieties having an interconnected pore structure and surface area up to 400 m2 / g.

Description

technical field [0001] The present invention relates to the hydrolysis of ethyl silicate using sulfonated polymeric bead catalysts synthesized using high internal phase emulsion methodology. The present invention also relates to the preparation of beaded cross-linked polymers having aromatic rings present in the polymer backbone and synthesized using water-in-oil-in-water emulsion techniques which are further modified to create The introduction of sulfonic acid groups. Background technique [0002] Tetraethyl orthosilicate (EtO) 4 Si has excellent thermal stability and liquid behavior over a wide temperature range. Ethyl silicate-32 is used as a binder in paints and coatings. It is also used as a room temperature silicone for curing crosslinkers. Ethyl silicate-40 is stable and has a long shelf life. It is mainly used as a binder in paints, coatings, ceramics and precision castings, and also as a silicone room temperature vulcanizing agent. Ethyl silicate-28 is used as...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/02C08F2/30C08F8/36C03C1/00C03B19/12
CPCC08F8/36C08F2/30C03B19/12C08G77/02C03C1/00
Inventor M·德维韦迪H·S·R·劳卡宁迪R·K·M·斯里尼瓦苏鲁D·扎纳奇拉曼M·R·贝瓦拉R·K·斯里派拉姆布杜尔P·苏拉德拉R·R·切拉纳特图奇扎克凯玛达斯K·T·拉吉夫M·S·库雷西N·N·恰范S·B·德奥卡尔K·B·穆拉尼R·V·戈霍尔帕德S·S·波洪加勒A·C·那拉旺德K·V·松塔可凯S·M·波霍斯勒S·A·缪勒D·A·德霍波勒A·约翰W·A·L·谢克R·哈里克里斯西纳V·普尼萨拉苏M·S·穆明
Owner 国防研究与发展组织