CN101700886A - Method for preparing trichlorosilane from tetrachlorosilane - Google Patents

Method for preparing trichlorosilane from tetrachlorosilane Download PDF

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Publication number
CN101700886A
CN101700886A CN200910310631A CN200910310631A CN101700886A CN 101700886 A CN101700886 A CN 101700886A CN 200910310631 A CN200910310631 A CN 200910310631A CN 200910310631 A CN200910310631 A CN 200910310631A CN 101700886 A CN101700886 A CN 101700886A
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China
Prior art keywords
silicon tetrachloride
tetrachlorosilane
hydrogen
trichlorosilane
gasification installation
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CN200910310631A
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CN101700886B (en
Inventor
唐前正
何劲
赵新征
卢涛
彭卡
李品贤
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LESHAN LEDIAN TIANWEI SILICAS CO Ltd
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LESHAN LEDIAN TIANWEI SILICAS CO Ltd
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Priority to CN2009103106312A priority Critical patent/CN101700886B/en
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Abstract

The invention relates to a method for preparing trichlorosilane from tetrachlorosilane, belonging to the field of polysilicon production. The invention solves the technical problem of providing a method for preparing trichlorosilane from tetrachlorosilane with higher conversion rate. The method comprises the following step: introducing tetrachlorosilane and hydrogen with the molar ratio of 0.15-0.4:1 into a hydrogenation furnace with the pressure of 0.3-0.6Mpa for reaction. The method of the invention improves the conversion rate of the tetrachlorosilane (the conversion rate is improved to about 32%) and the conversion quantity in the same time, solves the problems of accumulation of a large amount of by-product tetrachlorosilane in the production process of polysilicon and environmental protection, has better economic benefit and wide application prospects, and provides a new choice for the processing method of tetrachlorosilane in the field.

Description

Produce the method for trichlorosilane by silicon tetrachloride
Technical field
The present invention relates to a kind ofly produce the method for trichlorosilane, belong to field of polysilicon production by silicon tetrachloride.
Background technology
The improvement Siemens Method is the main stream approach of producing polysilicon at present both at home and abroad, and this method adopts also original production polysilicon of trichlorosilane.But use trichlorosilane also can produce a large amount of by product-silicon tetrachlorides the original production polysilicon time.Silicon tetrachloride is a kind of poisonous and harmful liquid with severe corrosive, must handle, in order to avoid contaminate environment.
At present, each production of polysilicon producer mainly contains following several for the treatment process of silicon tetrachloride:
1, changes into trichlorosilane after the hydrogenation of silicon tetrachloride heat from hydrogenation
This technology is: under normal pressure silicon tetrachloride and hydrogen are heated in about 1250 ℃, make trichlorosilane and hydrogenchloride.But this hot hydrogenation process transformation efficiency is lower, only is about 20%, the energy consumption height, and the conversion complex procedures, facility investment is big, fails to be used on a large scale in production of polysilicon enterprise.
2, utilize silicon tetrachloride production to make products such as gas-phase silica, tetraethyl silicate, organosilicon
Owing to reasons such as the added value of product of transporting, produce are lower, this method is lower to the utilization ratio of silicon tetrachloride, and this method also fails to be used on a large scale in production of polysilicon enterprise.
Summary of the invention
Technical problem to be solved by this invention provide a kind of transformation efficiency higher produce the method for trichlorosilane by silicon tetrachloride.
The method that the present invention produces trichlorosilane by silicon tetrachloride is: feed mol ratio and be 0.15~0.4: 1 silicon tetrachloride and hydrogen in pressure is the hydrogenation furnace of 0.3~0.6Mpa and react.
Wherein, in order to improve the silicon tetrachloride transformation efficiency, reduce the reaction response time, above-mentioned silicon tetrachloride and hydrogen mix earlier before feeding hydrogenation furnace.
Further, above-mentioned silicon tetrachloride and hydrogen mix in the silicon tetrachloride gasification installation, wherein, pressure in the silicon tetrachloride gasification installation is 0.5~1.3Mpa, pressure in the silicon tetrachloride gasification installation to form pressure reduction, helps big flow charging greater than the pressure of hydrogenation furnace.
Further, when above-mentioned silicon tetrachloride and hydrogen mixed in the silicon tetrachloride gasification installation, the speed that hydrogen feeds the silicon tetrachloride gasification installation was 1100~1500Nm 3/ h, the speed that silicon tetrachloride feeds the silicon tetrachloride gasification installation is 2300~3500kg/h.The speed that hydrogen and silicon tetrachloride feed the silicon tetrachloride gasification installation can increase gradually.
Wherein, the temperature of above-mentioned silicon tetrachloride when hydrogen reaction is preferably 1000~1300 ℃, and reaction temperature is spent low, and the trichlorosilane of reaction gained can generate polysilicon with hydrogen reaction, and temperature of reaction is too high, and then energy consumption improves, and increases production cost.
The inventive method has following beneficial effect:
1, under the effect of pressurization, gas mixture forms big pressure reduction between silicon tetrachloride gasification installation and hydrogenation furnace, the condition of big flow charging is provided, has compared with existing silicon tetrachloride heat from hydrogenation method for hydrogenation, the silicon tetrachloride amount that feeds hydrogenation furnace in the unit time has improved 3~4 times.
2, the inventive method mixed gas flow is big, gas velocity by the gas entrance is also big, can cause the turbulence of hydrogenation gas stream in the stove better, subdue the gas boundary layer and the furnace gas phenomenon pockety of heater surfaces, help the carrying out that react, improved the transformation efficiency (transformation efficiency is promoted to about 32%) of silicon tetrachloride and inversion quantity in the identical time.
3, the inventive method is by improving the conversion rate that silicon tetrachloride is converted into trichlorosilane; solved hoarding and environmental protection problem of silicon tetrachloride as by-product a large amount of in the polysilicon production process; has favorable economic benefit; for the treatment process of this area silicon tetrachloride provides new selection, have broad application prospects.
Embodiment
Below in conjunction with embodiment the specific embodiment of the present invention is further described, does not therefore limit the present invention among the described scope of embodiments.
Embodiment adopts the inventive method to produce trichlorosilane by silicon tetrachloride
Silicon tetrachloride is added in the silicon tetrachloride gasification installation, and heating obtains silicon tetrachloride gas, feeds hydrogen simultaneously and controls that pressure is 0.5~1.3Mpa in the silicon tetrachloride gasification installation, makes mol ratio and be 0.15~0.4: 1 the silicon tetrachloride and the gas mixture of hydrogen.The speed that hydrogen feeds the silicon tetrachloride gasification installation is 1100~1500Nm 3/ h, the speed that silicon tetrachloride feeds the silicon tetrachloride gasification installation is 2300~3500kg/h, the speed that hydrogen and silicon tetrachloride feed the silicon tetrachloride gasification installation is raise gradually by low.
Feed hydrogen earlier in hydrogenation furnace, making the hydrogenation furnace internal pressure is 0.3~0.6Mpa, and the gas mixture that feeds silicon tetrachloride and hydrogen then reacts, and the interior temperature of hydrogenation furnace is controlled to be 1000~1300 ℃ during reaction.After measured, the transformation efficiency of silicon tetrachloride is 32%.

Claims (5)

1. produce the method for trichlorosilane by silicon tetrachloride, it is characterized in that: in pressure is the hydrogenation furnace of 0.3~0.6Mpa, feed mol ratio and be 0.15~0.4: 1 silicon tetrachloride and hydrogen and react.
2. according to claim 1ly produce the method for trichlorosilane by silicon tetrachloride, it is characterized in that: described silicon tetrachloride and hydrogen mix earlier before feeding hydrogenation furnace.
3. the method for producing trichlorosilane by silicon tetrachloride according to claim 2, it is characterized in that: described silicon tetrachloride and hydrogen mix in the silicon tetrachloride gasification installation, wherein, pressure in the silicon tetrachloride gasification installation is 0.5~1.3Mpa, and the pressure in the silicon tetrachloride gasification installation is greater than the pressure in the hydrogenation furnace.
4. according to claim 3ly produce the method for trichlorosilane by silicon tetrachloride, it is characterized in that: when hydrogen and silicon tetrachloride mixed, the speed that hydrogen feeds the silicon tetrachloride gasification installation was 1100~1500Nm 3/ h, the speed that silicon tetrachloride feeds the silicon tetrachloride gasification installation is 2300~3500kg/h.
5. each describedly produces the method for trichlorosilane by silicon tetrachloride according to claim 1~4, and it is characterized in that: the temperature of described silicon tetrachloride when hydrogen reaction is 1000~1300 ℃.
CN2009103106312A 2009-11-30 2009-11-30 Method for preparing trichlorosilane from tetrachlorosilane Expired - Fee Related CN101700886B (en)

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CN101700886B CN101700886B (en) 2011-08-03

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102408113A (en) * 2011-07-28 2012-04-11 河北东明中硅科技有限公司 Thermal hydrogenation method of silicon tetrachloride
CN103723734A (en) * 2012-10-10 2014-04-16 浙江昱辉阳光能源有限公司 Technology for preparing trichlorosilane
CN103787338A (en) * 2012-10-29 2014-05-14 王红卫 Trichlorosilane plasma preparation method and preparation apparatus thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4217334A (en) * 1972-02-26 1980-08-12 Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler Process for the production of chlorosilanes
CN1183034C (en) * 2002-02-08 2005-01-05 中国有色工程设计研究总院 Silicon tetrachloride hydrogenating process of producing trichloro hydrosilicon
CN101445245B (en) * 2008-12-26 2011-04-06 四川新光硅业科技有限责任公司 Method for producing trichlorosilane by using silicon tetrachloride

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102408113A (en) * 2011-07-28 2012-04-11 河北东明中硅科技有限公司 Thermal hydrogenation method of silicon tetrachloride
CN102408113B (en) * 2011-07-28 2013-04-24 河北东明中硅科技有限公司 Thermal hydrogenation method of silicon tetrachloride
CN103723734A (en) * 2012-10-10 2014-04-16 浙江昱辉阳光能源有限公司 Technology for preparing trichlorosilane
CN103723734B (en) * 2012-10-10 2015-09-09 浙江昱辉阳光能源有限公司 A kind of technique preparing trichlorosilane
CN103787338A (en) * 2012-10-29 2014-05-14 王红卫 Trichlorosilane plasma preparation method and preparation apparatus thereof

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