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DOI£º10.11951/j.issn.1005-0299.20120101

·ÖÀàºÅ:O613. 72

»ù½ðÏîÄ¿:¹ú¼Ò¸ß¼¼ÊõÑо¿·¢Õ¹¼Æ»®×ÊÖúÏîÄ¿(2006BAE01B09).



Monosilane obtained from disproportionation of trimethoxysilanecatalyzed with quaternary ammonium hydroxide resin

YANG Kai¹, AN Mao zhong¹, YANG Chun hui¹, ZHANG Lei², HU Cheng fa³, GE Shi bin¹

1.School of Chemical Engineering and Technology,Harbin Institute of Technology,Harbin 150001,China,Email:yangchh@ hit. edu. cn;2.School of Chemical Engineering and Technology,Harbin Institute of Technology,Harbin 150001,China,;3.Email:yangchh@ hit. edu. cn

Abstract:

High purity monosilane was prepared from disproportionation of trimethoxysilane catalyzed with quaternary ammonium hydroxide resin.Crude monosilane was analyzed by pulse discharge helium ionization detector.By product tetramethoxysilane rectified was analyzed with gas chromatography mass spectrometry and inductively coupled plasma mass spectrometry.Experimental results show that the reaction conditions is the temperature range of 30~50 ¡æ and the pressure range of 0.2~0.3 MPa.Contents of H2,O2,Ar,N2,and CH4 of crude monosilane were 221.12,1.76,1.61,17.97 and 0.15 ¦Ìg/L,respectively.Content of tetramethoxysilane was 99.9wt%,and total metal impurities of tetramethoxysilane was less than 0.15 ¦Ìg/L.Furthermore,the tetramethoxysiane can be material of high purity silica sol.The disproportionation reaction of trimethoxysilane catalyzed with quaternary ammonium hydroxide resin was happen at mild reaction conditions,and conversation of trimethoxysilane was 96wt%,and yield of monosilane was 95wt%.Catalyst is easy to buy,and fixed bed reactor is easy to control the reaction,and easy to continuous feeding,and then the technology has industrial production value.

Key words:  quaternary ammonium hydroxide  anion exchange resin  trimethoxysilane  monosilane