Preparation of fluorosilicon compounds
US-2018346492-A1 · Dec 6, 2018 · US
US9718844B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9718844-B2 |
| Application number | US-201314416952-A |
| Country | US |
| Kind code | B2 |
| Filing date | May 28, 2013 |
| Priority date | Jul 24, 2012 |
| Publication date | Aug 1, 2017 |
| Grant date | Aug 1, 2017 |
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Described is a method for producing alkenyl halosilanes by reacting alkenyl halide selected from the group comprising vinyl halide, vinylidene halide, and allyl halide with halosilane selected from the group comprising monohalosilane, dihalosilane, and trihalosilane in the gas phase in a reactor comprising a reaction tube ( 1 ) that has an inlet ( 2 ) at one end and an outlet ( 3 ) at the other end, said reactor further comprising an annular-gap nozzle ( 4 ) that is mounted on the inlet ( 2 ), extends into the reaction tube ( 1 ), and has a central supply duct ( 5 ) for one reactant ( 7 ) and a supply duct ( 6 ), which surrounds the central supply duct ( 5 ), for the other reactant ( 8 ). In order to carry out said method, alkenyl halide is injected into the reaction tube ( 1 ) through the central supply duct ( 5 ), halosilane is injected thereinto through the surrounding supply duct ( 6 ), and both substances flow through the reaction tube ( 1 ) in the direction of the outlet ( 3 ). The described method allows alkenyl halosilanes to be produced at a high yield and with great selectivity. The amount of soot formed is significantly lower than in conventional reactors. The invention also relates to a reactor for carrying out gas-phase reactions, said reactor being characterized by at least the following elements: A) a reaction tube ( 1 ) that has B) an inlet ( 2 ) at one end, C) an outlet ( 3 ) at the other end, and D) an annular-gap nozzle ( 4 ) which includes a central supply duct ( 5 ) for one reactant ( 7 ) and a supply duct ( 6 ), which surrounds the central supply duct ( 5 ), for another reactant ( 8 ), said nozzle being mounted on the inlet ( 2 ) and extending into the reaction tube ( 1 ).
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The invention claimed is: 1. A reactor suitable for gas phase reactions, comprising: a reaction tube comprising an inlet at one side of the tube, an outlet at the other side of the tube, the outlet opening to a reservoir vessel suitable to contain a cooled product of the gas phase reaction, an annular gap nozzle comprising a central feed for one reactant and a feed surrounding the central feed for another reactant, which is mounted at the inlet and opens into the reaction tube, wherein the feed surrounding the central feed has a side wall angled towards the central feed of the annular gap nozzle a preheating zone connected to the inlet in such a way so as to heat reactants for the gas phase reaction to a reaction temperature, and a line connected from the reservoir to near the outlet, the line configured to recycle the cooled product in the reaction mixture. 2. The reactor according to claim 1 , further comprising a means to vary the flow rate of the reactant(s) in the annular gap nozzle positioned at the central feed and/or at the feed surrounding the central feed. 3. A process for preparing alkenylhalosilanes by reacting alkenyl halide selected from the group consisting of vinyl halide, vinylidene halide and allyl halide with halosilane selected from the group consisting of mono-, di- and trihalosilane in the gas phase in the reactor according to claim 1 wherein the alkenyl halide is injected into the reaction tube through the central feed and halosilane through the surrounding feed, and they flow through the reaction tube in the direction of outlet ( 3 ). 4. The process according to claim 1 , wherein the alkenyl halide is vinyl chloride, vinyl bromide, vinylidene chloride, vinylidene bromide, allyl chloride or allyl bromide, and the halosilane is di- or trichlorosilane or di- or tribromosilane. 5. The process according to claim 1 , wherein the alkenyl halide is vinyl chloride or allyl chloride, and the halosilane is trichlorosilane. 6. The process according to claim 1 , characterized in that the annular gap nozzle is a two-phase nozzle. 7. The process according to claim 1 , wherein the reactor further comprises a device to vary the flow rate of the reactant(s) positioned at the central feed and/or at the feed surrounding the central feed. 8. The process according to claim 1 , wherein the mono-, di- or trihalosilane to alkenyl halide is in a ratio of 1.0 to 10 mol:mol. 9. The process according to claim 1 , wherein a hot reaction mixture is quenched with a liquid crude product at the product end of the reaction tube. 10. The process according to claim 1 , wherein the temperature in the interior of the reaction tube is between 400 and 700° C. 11. The process according to claim 1 , wherein the pressure in the interior of the reaction tube is from 1.0 to 2.0 bar abs. 12. The process according to claim 1 , wherein the flow rate of the alkenyl halide in central feed is controlled by a closed-loop temperature control circuit. 13. The process according to claim 1 , wherein the residence time of the reaction mixture in the reactor from opening of the annular nozzle to the outlet is 0.5 to 10 sec.
controlling the pressure · CPC title
adding a temperature modifying medium to the reactants · CPC title
Controlling the temperature · CPC title
by reactions involving the formation of Si-C linkages (hydrosilylation reactions C07F7/14; direct synthesis C07F7/16) · CPC title
involving reactant liquids · CPC title
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