摘要:
The invention relates to a method of preparing a halogenoalkyldialkylchlorosilane having formula (I): Hal-------(R2R3)Si---(CH2)s---Hal by hydrogen silylation reaction of a reaction medium comprising a silane having formula (II): Hal---(R2R3)Si-H and an alkene halide having formula (III): CH=CH-(CH2)s_2Hal, in the presence a catalytically-effective amount of a hydrogen silylation catalyst based on a platinum group metal. The inventive method is characterised in that, at the end of the hydrogen silylation reaction, the product formed having formula (I) and the platinum group catalytic metal are recovered. According to the invention, the catalytic metal recovery method is performed under the following conditions: a) the catalytic metal is recovered (1) directly from the reaction medium at the end of the reaction or (2) from the liquid distillation residue comprising the by-products and the platinum group metal, residue obtained after distillation of the reaction medium in order to separate the product having formula (I); b) the catalytic metal is recovered by bringing the reaction medium or the distillation residue into contact with an effective amount of a solid substance that absorbs the platinum group metal; and c) the adsorbent and the platinum group metal are separated so that said metal can be recovered. The invention can be used for the synthesis of 3-chloropropyldimethylchlorosilane with the recovery of the iridium-based catalyst.
摘要:
The invention relates to the preparation of organodialkylalkoxysilane using a continuous method consisting in bringing an alkanol into continuous contact with an omega-haloalkyl dialkylhalosilane in a countercurrent reactor, such as a plate column or a packed column. The reaction is performed in the aforementioned countercurrent reactor in the presence or absence of a non-reactive solvent with scavenging of the hydrochloric acid formed. The omega-haloalkyl dialkylalkoxysilane thus formed is particularly suitable for use as a starting material for the preparation of organosilicon compounds containing sulphur having general formula (I) by means of sulphidisation reaction on an alkaline metal polysulphide.
摘要:
The invention relates to producing an organo alcoxydialkylsilane by a method which consists in introducing by pouring an alcanol in a dialkylhalogenosilane omega-halogenalkyl + an organic solvent (s) phase mixture and in removing a halogen acid formed by entrainment with the aid of said organic solvent(s) phase and is characterised, in particular (i) by selecting a particular phase of solvent(s), for example based on cyclohexane, (2i) by carrying out an alcanol introduction mode which makes it possible to control the drawing off the halogen acid formed during reaction and by (3i) controlling the halogen acid quantity in a reaction medium. The thus obtained dialkylhalogenosilane omega-halogenalkyl is usable, in particular as an initial product for preparing organosilisic sulphur-containing compounds of general formula (IV) by a sulfidising reaction carried out on a alkali metal polysulfur.
摘要:
The present invention relates to a method for preparing an omega-haloalkyl dialkylhalosilane of formula (I) (Hal-------(R 2 R 3 )Si---(CH 2 ) s ---Hal) by means of a hydrosilylation reaction between a reaction medium comprising a silane of formula (II) (Hal---(R 2 R 3 )Si-H) and an alkene halide of formula (III) (CH=CH-(CH 2 ) s-2 Hal), in the presence of a catalytically effective amount of a hydrosilylation catalyst containing a platinum group metal. According to the method, once the hydrosilylation reaction is complete, the resulting product having formula (I) and the platinum group catalytic metal are recovered by distillation. Said method is characterised in that said catalytic metal is recovered by (i) subjecting the distillation residue to controlled hydrolysis to release the gaseous H-Hal haloacid, and providing an aqueous medium containing the catalytic metal with a low hydrolysable halide content Si-Hal = 2 %, expressed by weight of Hal, then (2i) recovering the platinum group catalytic metal from said aqueous medium by means of one of the conventional techniques specific to catalyst manufacturers that do not use a solid adsorbent and operate in ordinary facilities that do not have to be acid-resistant.
摘要:
The present invention relates to a method for preparing an omega-haloalkyl dialkylhalosilane of formula (I) (Hal-------(R2R3)Si---(CH2)s---Hal) by means of a hydrosilylation reaction between a reaction medium comprising a silane of formula (II) (Hal---(R2R3)Si-H) and an alkene halide of formula (III) (CH=CH-(CH2)s-2Hal), in the presence of a catalytically effective amount of a hydrosilylation catalyst containing a platinum group metal. According to the method, once the hydrosilylation reaction is complete, the resulting product having formula (I) and the platinum group catalytic metal are recovered by distillation. Said method is characterised in that said catalytic metal is recovered by (i) subjecting the distillation residue to controlled hydrolysis to release the gaseous H-Hal haloacid, and providing an aqueous medium containing the catalytic metal with a low hydrolysable halide content Si-Hal = 2 %, expressed by weight of Hal, then (2i) recovering the platinum group catalytic metal from said aqueous medium by means of one of the conventional techniques specific to catalyst manufacturers that do not use a solid adsorbent and operate in ordinary facilities that do not have to be acid-resistant.
摘要:
The invention relates to a method of preparing a halogenoalkyldialkylchlorosilane having formula (I): Hal-------(R R )Si---(CH2)s---Hal by hydrogen silylation reaction of a reaction medium comprising a silane having formula (II): Hal---(R R )Si-H and an alkene halide having formula (III): CH=CH-(CH2)s_2Hal, in the presence a catalytically-effective amount of a hydrogen silylation catalyst based on a platinum group metal. The inventive method is characterised in that, at the end of the hydrogen silylation reaction, the product formed having formula (I) and the platinum group catalytic metal are recovered. According to the invention, the catalytic metal recovery method is performed under the following conditions: a) the catalytic metal is recovered (1) directly from the reaction medium at the end of the reaction or (2) from the liquid distillation residue comprising the by-products and the platinum group metal, residue obtained after distillation of the reaction medium in order to separate the product having formula (I); b) the catalytic metal is recovered by bringing the reaction medium or the distillation residue into contact with an effective amount of a solid substance that absorbs the platinum group metal; and c) the adsorbent and the platinum group metal are separated so that said metal can be recovered. The invention can be used for the synthesis of 3-chloropropyldimethylchlorosilane with the recovery of the iridium-based catalyst.
摘要:
The invention concerns a method for hydrolyzing/condensing, by acid catalysis, silanes bearing hydrolyzable groups, preferably halogenosilanes and more preferably still chlorosilanes, in a polyphase reaction medium (preferably biphasic), said method consisting in bringing the silanes bearing the hydrolyzable groups in the presence of water, buffer solution and neutralizing agent, while stirring, then in separating the aqueous phase from the organic phase, which comprises the hydrolysis/condensation products, namely hydroxylated polyorganosiloxanes. Said method is characterized in that it consists in: (a) implementing intensively stirring means capable of producing, in the reaction medium, an agitation at least equivalent to that induced by a shearing corresponding to that provided by a rotor whereof the peripheral speed is not less than 8 m.s-1, preferably not less than 10 m.s-1, and more preferably still ranging between 15 and 20 m.s-1, enabling thus organic phase droplets to be formed, of d32 less than 500 νm; (b) and ensuring that the silanes/aqueous phase mass fraction is not less than 0.05, preferably not less than 0.10, and more preferably still ranging between 0.5 and 2.0.