CN103896279A - Combined method for preparing dichlorosilane - Google Patents

Combined method for preparing dichlorosilane Download PDF

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Publication number
CN103896279A
CN103896279A CN201210589213.3A CN201210589213A CN103896279A CN 103896279 A CN103896279 A CN 103896279A CN 201210589213 A CN201210589213 A CN 201210589213A CN 103896279 A CN103896279 A CN 103896279A
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CN
China
Prior art keywords
silicon
hydrogen
tetrachloro silicane
dichloro
trichlorosilane
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Pending
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CN201210589213.3A
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Chinese (zh)
Inventor
原东风
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Tianjin Taiyuan Industrial Gas Co Ltd
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Tianjin Taiyuan Industrial Gas Co Ltd
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Priority to CN201210589213.3A priority Critical patent/CN103896279A/en
Publication of CN103896279A publication Critical patent/CN103896279A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a combined method for preparing dichlorosilane. Based on disproportionation, the process of silicon tetrachloride hydrogenation is increased, so as to fully use the by-product, in a chlorhydrogenation reactor, at the presence of hydrogen and tetrachlorosilane with the molar ratio of 1:(1-4), hydrochlorination is carried out on metallurgical grade silicon, the reacted airflow contains dichlorosilane, trichlorosilane, tetrachlorosilane, hydrogen and unreacted silicon particles, the tetrachlorosilane and hydrogen are separated through condensation and rectification and are recycled. The trichlorosilane is obtained by virtue of a catalyst fixed bed, and is disproportionated into dichlorosilane and tetrachlorosilane, the disproportionated airflow is sent to a corresponding rectification unit for separating and purifying.

Description

A kind of method that adopts integrated process to produce dichloro-dihydro silicon
Technical field
The present invention adopts integrated process to produce dichloro-dihydro silicon, in chlorhydrogenation reactor, and under the existence of hydrogen and tetrachloro silicane, metallurgical grade silicon generation hydrochlorination.In reacted air-flow, contain dichloro-dihydro silicon, trichlorosilane, tetrachloro silicane, hydrogen and unreacted silicon grain, separate with rectifying through condensation.Tetrachloro silicane after separation and hydrogen gas recycle are used.Be disproportionated into dichloro-dihydro silicon and tetrachloro silicane by the catalyst fixed bed trichlorosilane that obtains, the air-flow after disproportionation is delivered to corresponding rectification cell and is separated and purifying.
Background technology
Dichloro-dihydro silicon is the silicon source gas in semiconductor epitaxial and chemical vapor deposition method.The production of silicoorganic compound.Make the necessary high quality silicon of large-scale integrated circuit source.Inflammable in air, the spontaneous combustion of more than 100 DEG C energy, generates hydrogenchloride and silicon oxide after burning.While being heated to more than 100 DEG C, can decompose voluntarily and generate hydrochloric acid.Chlorine, hydrogen and ambiguity silicon.While imposing strong shock, also can decompose voluntarily.In wet air, produce corrodibility smog.React with alkali, ethanol, acetone.Also can there is intense reaction even if contact a small amount of halogen or other oxygenants.
Summary of the invention
Problem to be solved by this invention is, overcomes the deficiencies in the prior art.Provide a kind of integrated process that adopts to produce the certain method of dichloro-dihydro silicon, it is characterized in that on discrimination method basis, increasing hydrogenation of silicon tetrachloride effect operation, by product is made full use of, thereby reduce costs.Compared with discrimination method, although productive rate is lower, the high-carbon impurity that catalyst-free brings, product does not need to carry out degree of depth purifying; In chlorhydrogenation reactor, under the existence of hydrogen and tetrachloro silicane, metallurgical grade silicon generation hydrochlorination; In reacted air-flow, contain dichloro-dihydro silicon, trichlorosilane, tetrachloro silicane, hydrogen and unreacted silicon grain, separate with rectifying through condensation; Tetrachloro silicane after separation and hydrogen gas recycle are used; Be disproportionated into dichloro-dihydro silicon and tetrachloro silicane by the catalyst fixed bed trichlorosilane that obtains, the air-flow after disproportionation is delivered to corresponding rectification cell and is separated and purifying.
Integrated process is on discrimination method basis, to increase hydrogenation of silicon tetrachloride effect operation, by product is made full use of, thereby reduce costs.Compared with discrimination method, although productive rate is lower, the high-carbon impurity that catalyst-free brings, product does not need to carry out degree of depth purifying.In chlorhydrogenation reactor, under the existence of hydrogen and tetrachloro silicane, metallurgical grade silicon generation hydrochlorination.In reacted air-flow, contain dichloro-dihydro silicon, trichlorosilane, tetrachloro silicane, hydrogen and unreacted silicon grain, separate with rectifying through condensation.Tetrachloro silicane after separation and hydrogen gas recycle are used.Be disproportionated into dichloro-dihydro silicon and tetrachloro silicane by the catalyst fixed bed trichlorosilane that obtains, the air-flow after disproportionation is delivered to corresponding rectification cell and is separated and purifying.
Embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.Raw material wherein can have been bought in market.
Embodiment 1
A kind of integrated process that adopts is produced the certain method of dichloro-dihydro silicon, it is characterized in that on discrimination method basis, increasing hydrogenation of silicon tetrachloride effect operation, by product is made full use of, thereby reduce costs.Compared with discrimination method, although productive rate is lower, the high-carbon impurity that catalyst-free brings, product does not need to carry out degree of depth purifying; In chlorhydrogenation reactor, under the existence of hydrogen and tetrachloro silicane, metallurgical grade silicon generation hydrochlorination; In reacted air-flow, contain dichloro-dihydro silicon, trichlorosilane, tetrachloro silicane, hydrogen and unreacted silicon grain, separate with rectifying through condensation; Tetrachloro silicane after separation and hydrogen gas recycle are used; Be disproportionated into dichloro-dihydro silicon and tetrachloro silicane by the catalyst fixed bed trichlorosilane that obtains, the air-flow after disproportionation is delivered to corresponding rectification cell and is separated and purifying.
Embodiment 2
A kind of integrated process that adopts is produced the certain method of dichloro-dihydro silicon, it is characterized in that on discrimination method basis, increasing hydrogenation of silicon tetrachloride effect operation, and by product is made full use of, and product does not need to carry out degree of depth purifying; In chlorhydrogenation reactor, under the existence of hydrogen and tetrachloro silicane, the mol ratio of hydrogen and tetrachloro silicane is 1:4 metallurgical grade silicon generation hydrochlorination; In reacted air-flow, contain dichloro-dihydro silicon, trichlorosilane, tetrachloro silicane, hydrogen and unreacted silicon grain, separate with rectifying through condensation; Tetrachloro silicane after separation and hydrogen gas recycle are used; Be disproportionated into dichloro-dihydro silicon and tetrachloro silicane by the catalyst fixed bed trichlorosilane that obtains, the air-flow after disproportionation is delivered to corresponding rectification cell and is separated and purifying.
Embodiment 3
A kind of integrated process that adopts is produced the certain method of dichloro-dihydro silicon, it is characterized in that on discrimination method basis, increasing hydrogenation of silicon tetrachloride effect operation, and by product is made full use of, and product does not need to carry out degree of depth purifying; In chlorhydrogenation reactor, under the existence of hydrogen and tetrachloro silicane, the mol ratio of hydrogen and tetrachloro silicane is 1:1 metallurgical grade silicon generation hydrochlorination; In reacted air-flow, contain dichloro-dihydro silicon, trichlorosilane, tetrachloro silicane, hydrogen and unreacted silicon grain, separate with rectifying through condensation; Tetrachloro silicane after separation and hydrogen gas recycle are used; Be disproportionated into dichloro-dihydro silicon and tetrachloro silicane by the catalyst fixed bed trichlorosilane that obtains, the air-flow after disproportionation is delivered to corresponding rectification cell and is separated and purifying.

Claims (1)

1. adopt integrated process to produce the certain method of dichloro-dihydro silicon, it is characterized in that on discrimination method basis, increasing hydrogenation of silicon tetrachloride effect operation, by product is made full use of, product does not need to carry out degree of depth purifying; In chlorhydrogenation reactor, under the existence of hydrogen and tetrachloro silicane, the mol ratio of hydrogen and tetrachloro silicane is 1:1-4 metallurgical grade silicon generation hydrochlorination; In reacted air-flow, contain dichloro-dihydro silicon, trichlorosilane, tetrachloro silicane, hydrogen and unreacted silicon grain, separate with rectifying through condensation; Tetrachloro silicane after separation and hydrogen gas recycle are used; Be disproportionated into dichloro-dihydro silicon and tetrachloro silicane by the catalyst fixed bed trichlorosilane that obtains, the air-flow after disproportionation is delivered to corresponding rectification cell and is separated and purifying.
CN201210589213.3A 2012-12-31 2012-12-31 Combined method for preparing dichlorosilane Pending CN103896279A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210589213.3A CN103896279A (en) 2012-12-31 2012-12-31 Combined method for preparing dichlorosilane

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Application Number Priority Date Filing Date Title
CN201210589213.3A CN103896279A (en) 2012-12-31 2012-12-31 Combined method for preparing dichlorosilane

Publications (1)

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CN103896279A true CN103896279A (en) 2014-07-02

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108516555A (en) * 2018-07-10 2018-09-11 天津科技大学 A kind of preparation method and equipment of dichlororosilane eiectronic grade

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108516555A (en) * 2018-07-10 2018-09-11 天津科技大学 A kind of preparation method and equipment of dichlororosilane eiectronic grade

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Application publication date: 20140702