CN101479192A - Process for producing trichlorosilane and trichlorosilane producing apparatus - Google Patents
Process for producing trichlorosilane and trichlorosilane producing apparatus Download PDFInfo
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- CN101479192A CN101479192A CNA2007800244818A CN200780024481A CN101479192A CN 101479192 A CN101479192 A CN 101479192A CN A2007800244818 A CNA2007800244818 A CN A2007800244818A CN 200780024481 A CN200780024481 A CN 200780024481A CN 101479192 A CN101479192 A CN 101479192A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
Abstract
An apparatus comprising reaction chamber (2) for forming of a reaction product gas from trichlorosilane and hydrogen chloride through introduction of tetrachlorosilane and hydrogen thereinside and reduction reaction thereof at 800 DEG C or higher; reaction product gas outside leading means (4) for leading outside the reaction product gas present in the reaction chamber (2); and cooling gas introduction means (5) for cooling of the reaction product gas by mixing hydrogen, or tetrachlorosilane, or hydrogen chloride into the reaction product gas led out by the reaction product gas outside leading means (4).
Description
Technical field
The present invention relates to convert tetrachloro silicane to the preparation method of trichlorosilane of trichlorosilane and the preparation facilities of trichlorosilane.
The application according on November 7th, 2006 spy in Japanese publication be willing to 2006-302056 number and on October 22nd, 2007 spy in Japanese publication be willing to advocate right of priority for 2007-273545 number, its content is quoted among the application.
Background technology
High-purity polycrystalline silicon for example can be with trichlorosilane (SiHCl
3: abbreviate TCS as), tetrachloro silicane (SiCl
4: abbreviate STC as) and hydrogen as raw material, prepare by the hydrogen reduction reaction of the trichlorosilane shown in the following formula (1), the pyrolysis of the trichlorosilane shown in the following formula (2).
SiHCl
3+H
2→Si+3HCl …(1)
4SiHCl
3→Si+3SiCl
4+2H
2 …(2)
In the above-mentioned formation reaction expellant gas by polysilicon, contain unreacted tetrachloro silicane, trichlorosilane and hydrogen, also contain the high boiling point chlorosilane class of trace such as lower boiling chlorosilane class, tetrachloro silicoethane or disilicone hexachloride such as secondary hydrogenchloride of giving birth to and dichlorosilane simultaneously.These chlorosilane classes can be carried out interim fractionation by distillation according to boiling point, can utilize as required again.
For example, can be raw material with the tetrachloro silicane that reclaims by fractionation by distillation in the exhaust of above-mentioned formation reaction, by the conversion reaction generation trichlorosilane of the hydrogen addition shown in the following formula (3).Reclaim this trichlorosilane, its preparation raw material as above-mentioned polysilicon can be utilized again.
SiCl
4+H
２→SiHCl
３+HCl …(3)
As the preparation this trichlorosilane device, for example in the known patent document 1 record conversion reaction device (converter).This conversion reaction device is that the reaction chamber of parcel heating element has two mistress and dual chambers of inner room that pipe forms by concentric arrangement, bottom at this reaction chamber is provided with heat exchanger, connect unstripped gas supply line and escape route via this heat exchanger, described unstripped gas supply line is supplied with hydrogen and tetrachloro silicane in reaction chamber, described escape route generates gas by discharging reaction in the reaction chamber; In above-mentioned heat exchanger, the heat passage supply gas of giving the supply response chamber that the reaction of autoreaction chamber discharge in the future generates gas carries out preheating, and the reaction of discharging simultaneously generates gas and cooled off.
Patent documentation 1: No. 3781439 communique of Japanese Patent
Summary of the invention
Invent problem to be solved
In above-mentioned existing trichlorosilane preparation facilities, in the heat exchanger of reaction chamber bottom, to react the generation gas cooling by carrying out heat exchange, but generate in the process of cooling of gas, the reversed reaction that trichlorosilane resolves into silicon tetrachloride and hydrogen will take place in reaction with supply gas.Therefore, improve the speed of cooling that reaction generates gas, manage in quenching in the following short period of time of temperature that reversed reaction does not obviously take place in order reversed reaction not to take place as far as possible.But therefore above-mentioned existing method of cooling can't avoid the generation of reversed reaction because speed of cooling is slow, the bad situation of the turnover ratio step-down of generation trichlorosilane occurs.The problems referred to above increase when under higher temperature conversion reaction taking place, particularly remarkable above the problems referred to above under 1200 ℃ the temperature.
Though can also under the temperature that does not obviously take place until reversed reaction at 1 second with interior utmost point quenching in the short period of time, but in this case, the secondary polymkeric substance of giving birth in process of cooling, therefore the problem that has the turnover ratio step-down, and secondary polymkeric substance of the giving birth to wall that is attached to pipeline first-classly blocking pipeline occurs, can't keep the bad situation of the good viability of pipeline etc.Need to prove that this polymkeric substance is the Si that contains the above silicon of 2 atoms
2Cl
6, Si
3Cl
8, Si
2H
2Cl
4Deng high price chlorosilane class.
The present invention establishes for the problems referred to above that solve among the existing trichlorosilane preparation method, purpose is to provide by importing specific cooling gas in the mixed gas that generates to conversion reaction, the mixed gas that the quenching of chemical reaction limit generates is controlled on the limit, can improve the preparation method and the trichlorosilane preparation facilities of the trichlorosilane of efficiency of conversion.
Solve the method for problem
The present invention relates to the preparation method that the formation shown in following by having [1]～[6] solves the trichlorosilane of above-mentioned problem.
[1] preparation method of trichlorosilane, this preparation method has following steps: tetrachloro silicane and hydrogen are imported in the reaction chamber, make it to react under the temperature more than 800 ℃, generate the step of the mixed gas that comprises trichlorosilane and hydrogenchloride; And when deriving above-mentioned mixed gas, in this mixed gas, import the step of cooling off this mixed gas based at least a cooling gas in hydrogen, tetrachloro silicane or the hydrogenchloride by above-mentioned reaction chamber.
[2] preparation method of the trichlorosilane of above-mentioned [1], the temperature that wherein imports to the cooling gas in the mixed gas is-60 ℃～650 ℃.
[3] preparation method of the trichlorosilane of above-mentioned [1] or [2], wherein the temperature of reaction of mixed gas generation step is more than 1200 ℃.
[4] preparation method of each trichlorosilane in above-mentioned [1]～[3] wherein imports the cooling gas based on hydrogen or tetrachloro silicane, and above-mentioned mixed gas is cooled to below 650 ℃.
[5] preparation method of each trichlorosilane in above-mentioned [1]～[3] wherein imports the cooling gas based on hydrogenchloride, with above-mentioned mixed gas at 1 second with below the internal cooling to 650 ℃.
[6] preparation method of each trichlorosilane in above-mentioned [1]～[4], the mixed gas that wherein will import cooling gas imports in the water cooler, and the unreacted hydrogen of condensation separation utilizes isolating hydrogen-containing gas as cooling gas again.
The invention still further relates to the formation shown in following by having [7]～[11] and solve the preparation facilities of the trichlorosilane of above-mentioned problem.
[7] preparation facilities of trichlorosilane, this preparation facilities possesses following equipment: make tetrachloro silicane and hydrogen react the reaction chamber that generates the mixed gas that comprises trichlorosilane and hydrogenchloride under the temperature more than 800 ℃; The mixed gas that above-mentioned mixed gas is exported to the reaction chamber outside is derived equipment; And will import to cooling gas introducing equipment in the above-mentioned mixed gas based at least a cooling gas in hydrogen, tetrachloro silicane or the hydrogenchloride, this cooling gas introducing equipment is connected on the above-mentioned mixed gas derivation equipment.
[8] the trichlorosilane preparation facilities of above-mentioned [7], wherein temperature of reaction is more than 1200 ℃.
[9] the trichlorosilane preparation facilities of above-mentioned [7] or [8], wherein on the cooling gas introducing equipment, be connected with supply line based on the cooling gas of hydrogen or tetrachloro silicane, to import to based on the cooling gas of hydrogen or tetrachloro silicane in the above-mentioned mixed gas, above-mentioned mixed gas will be cooled to below 650 ℃.
[10] the trichlorosilane preparation facilities of above-mentioned [7] or [8], wherein on the cooling gas introducing equipment, be connected with supply line based on the cooling gas of hydrogenchloride, to import to based on the cooling gas of hydrogenchloride in the above-mentioned mixed gas, with above-mentioned mixed gas at 1 second with below the internal cooling to 650 ℃.
[11] each trichlorosilane preparation facilities in above-mentioned [7]～[10], it possesses: import the water cooler of mixed gas, imported cooling gas in the above-mentioned mixed gas; And in the cooling gas introducing equipment, supply with circulation line based on the hydrogen-containing gas of unreacted hydrogen through the water cooler condensation separation.
According to the method for above-mentioned [1] and the device of above-mentioned [7], tetrachloro silicane and H-H reaction are generated in the conversion reaction of trichlorosilane, cool off above-mentioned generation mixed gas by in the mixed gas that generates, importing based at least a cooling gas in hydrogen, tetrachloro silicane or the hydrogenchloride, therefore in the cooling down high-temperature mixed gas, the hydrogen that the reversed reaction of trichlorosilane is imported into, tetrachloro silicane suppress, the pair life of polymkeric substance is chlorinated hydrogen and suppresses, thereby can improve the turnover ratio of trichlorosilane.Need to prove, about cooling gas, be that main body is meant in the scope of the effect that can not reduce these compositions significantly and can contains a spot of other compositions with at least a in hydrogen, tetrachloro silicane or the hydrogenchloride.
The hydrogen, tetrachloro silicane or the hydrogenchloride that import can be sneaked into any separately, also can sneak into multiple simultaneously.In addition, can set according to the speed of cooling of above-mentioned generation mixed gas, for example shown in above-mentioned [2], use-60 ℃～650 ℃ cooling gas based on the temperature of the cooling gas of hydrogen, tetrachloro silicane or hydrogenchloride.Can also will import after the prior preheating of cooling gas.These cooling gases can be used in combination with other method of cooling.
In the device of the method for above-mentioned [1] and above-mentioned [7], the temperature of the generation conversion reaction of trichlorosilane is more than 800 ℃, and in the device of the method for above-mentioned [3] and above-mentioned [8], temperature of reaction is more than 1200 ℃.When shift reaction temperature was lower than 800 ℃, the production rate of trichlorosilane (turnover ratio) reduced significantly.Conversion reaction further obtains promoting under the temperature of reaction more than 1200 ℃, can improve the turnover ratio that generates trichlorosilane.
The conversion reaction of the high more generation trichlorosilane of temperature obtains promoting more, but when surpassing 1000 ℃ of left and right sides, a part of trichlorosilane that reaction generates in the gas resolves into hydrogenchloride and intermediate product SiCl
2High more this decomposition reaction of temperature is carried out more, is particularly surpassing under 1200 ℃ the temperature, and reaction generates SiCl in the gas
2Become main component.
Preparation method of the present invention and preparation facilities are because the hydrogen, tetrachloro silicane or the hydrogenchloride that import to the cooling gas in the generation mixed gas of conversion reaction are to this SiCl
2The generation effect even therefore carrying out under the situation of conversion reaction above under 1200 ℃ the temperature, also can suppress the reversed reaction that trichlorosilane decomposes effectively, can improve the turnover ratio that generates trichlorosilane.
In the device of the method for above-mentioned [4] and above-mentioned [9], importing is based on the cooling gas of hydrogen or tetrachloro silicane, with the temperature below the above-mentioned generation gas cooling to 650 ℃, therefore generate the temperature range that gas is cooled to the reversed reaction of the reaction that obviously do not change, the reversed reaction of conversion reaction is suppressed by hydrogen or tetrachloro silicane simultaneously.Need to prove that hydrogen of sneaking into or tetrachloro silicane can import any separately, perhaps both can be imported simultaneously.
In the device of the method for above-mentioned [5] and above-mentioned [1], importing is based on the cooling gas of hydrogenchloride, with above-mentioned generation gas with 1 second during with the temperature below the interior speed of cooling quenching to 650 ℃, even quenching was to the above-mentioned temperature range below 650 ℃ of the reversed reaction of the reaction that obviously do not change in the short period of time with the interior utmost point at 1 second, the pair of polymkeric substance is given birth to also can be chlorinated the hydrogen inhibition.Its result can suppress to be given birth to and the reduction of the turnover ratio that causes by the pair of polymkeric substance, can suppress the reversed reaction of conversion reaction simultaneously, can further improve turnover ratio.And, can prevent that secondary polymkeric substance of giving birth to is attached to the problem of the first-class blocking pipeline of wall of pipeline, keep the good order and condition of pipeline etc.Above-mentioned effect becomes big when under higher temperature conversion reaction taking place, particularly remarkable above above-mentioned effect under 1200 ℃ the temperature.
In the device of the method for above-mentioned [6] and above-mentioned [11], the mixed gas that has imported cooling gas is imported in the water cooler, the unreacted hydrogen of condensation separation utilizes isolating hydrogen-containing gas as cooling gas again, therefore can improve the service efficiency of hydrogen.
The invention effect
As mentioned above, preparation method and trichlorosilane preparation facilities according to trichlorosilane of the present invention, when deriving generation gas by reaction chamber, importing is cooled off above-mentioned generation gas based on the cooling gas of hydrogen, tetrachloro silicane or hydrogenchloride, therefore the generation gas of the condition of high temperature is by quenching, the reversed reaction of conversion reaction is suppressed simultaneously, and the pair of polymkeric substance is given birth to and also is suppressed, and therefore can obtain trichlorosilane with high-conversion rate.
The accompanying drawing summary
Fig. 1 is the pie graph of device integral body that shows an embodiment of the preparation method of trichlorosilane of the present invention and trichlorosilane preparation facilities.
Nomenclature
1 ... the trichlorosilane preparation facilities
2 ... reaction chamber
4 ... reaction generates gas and derives equipment
5 ... the cooling gas introducing equipment
6 ... heating installation
9 ... gas supply pipe
11 ... vapor pipe
14 ... the cooling gas ingress pipe
The best mode that carries out an invention
Below, specify the preparation method of trichlorosilane of the present invention and the embodiment of trichlorosilane preparation facilities with reference to Fig. 1.
The trichlorosilane preparation facilities (converter) 1 of embodiment shown in Figure 1 possesses: make tetrachloro silicane and hydrogen at the reaction chamber 2 that reacts the mixed gas that generates trichlorosilane and hydrogenchloride more than 800 ℃; Be connected the gas feeding apparatus 3 on the reaction chamber 2; Above-mentioned generation mixed gas is exported to outside generation gas derive equipment 4; And be connected this generation gas and derive cooling gas introducing equipment 5 on equipment 4.
Around reaction chamber 2, be provided with the heating installation 6 of this reaction chamber 2 of heating, and configuration thermal insulation material 7 make cover this reaction chamber 2 and heating installation 6 around, above-mentioned reaction chamber 2, heating installation 6 and thermal insulation material 7 are accommodated in the accommodating container 8.
Above-mentioned heating installation 6 possesses the heating element one heating part 6a that makes encapsulation reaction chamber 2 on every side that is configured in reaction chamber 2.This heating part 6a is formed by carbon.Heating installation 6 control heating make the temperature that reaches in the reaction chamber 2 in 800 ℃～1900 ℃ scopes.Need to prove that turnover ratio improves during with the temperature that is set in the reaction chamber more than 1200 ℃.That is, utilize the conversion reaction that surpasses under 1200 ℃ the temperature, can obtain a large amount of trichlorosilanes.
Above-mentioned reaction chamber 2 is formed by carbon, simultaneously can be at the top coat silicon carbide of this carbon.In addition, above-mentioned accommodating container 8 is preferably stainless steel.
Above-mentioned gas supply arrangement 3 possesses: the gas supply pipe 9 of base feed gas and the mixing tank 10 that is connected on this gas supply pipe 9 in reaction chamber 2.In this mixing tank 10, supply with hydrogen, and supply with tetrachloro silicane, they are mixed in mixing tank 10, import in the reaction chamber again from vaporizer (diagram is omitted).Need to prove, can comprise the silicoethane class in the tetrachloro silicane of supply, also can remove the silicoethane class.
The above-mentioned generation gas derivation equipment 4 that is connected on the reaction chamber 2 possesses: the generation mixed gas in the reaction chamber is exported to outside vapor pipe 11; Be connected the cooling separator 12 on this vapor pipe 11; And be connected water distilling apparatus 13 on the cooling separator 12.This generation gas is derived on the equipment 4 and is connected with above-mentioned cooling gas introducing equipment 5.This cooling gas introducing equipment 5 possesses cooling gas ingress pipe 14, and this cooling gas ingress pipe 14 is connected in the base end part of above-mentioned vapor pipe 11.
Cooling gas ingress pipe 14 is connected on the supply source (diagram omit) of cooling gas, for example is connected on the supply source of hydrogen, tetrachloro silicane or hydrogenchloride (diagram is omitted) by supply line (diagram is omitted).To import to based on the cooling gas of hydrogen, tetrachloro silicane or hydrogenchloride in the generation gas by this cooling gas ingress pipe 14.
In example shown in Figure 1, cooling gas ingress pipe 14 is connected on the above-mentioned cooling separator 12, forms by the mode that above-mentioned cooling gas ingress pipe 14 is directed in the above-mentioned vapor pipe 11 according to isolating unreacted hydrogen in this cooling separator 12.
Above-mentioned cooling gas introducing equipment 5 is according to the cold gas scale of construction that can adjust importing, makes reaction generate the mode of the temperature below the gas cooling to 650 ℃ and forms.Need to prove,, can in the base end part of vapor pipe 11, temperature sensor be set for the reaction of measuring, control quenching generates the temperature of gas.
Next, the preparation method to the trichlorosilane that uses above-mentioned trichlorosilane preparation facilities describes.
At first, the unstripped gas that will comprise tetrachloro silicane and hydrogen by gas supply pipe 9 is imported to the inside of reaction chamber 2 by mixing tank 10.Utilize heating installation 6 to be heated to temperature of reaction in reaction chamber, the reaction by unstripped gas generates trichlorosilane and hydrogenchloride etc.This reaction generates gas and exports to the outside by vapor pipe 11.At this moment, utilize cooling gas introducing equipment 5, cooling gas is imported in the base end part of vapor pipe 11, sneak into reaction and generate in the gas by cooling gas ingress pipe 14.
By importing this cooling gas the reaction of the condition of high temperature is generated temperature below the quenching of gases to 650 ℃.Adjust the temperature and the import volume of cooling gas, make reaction generate gas and reach below 650 ℃.Need to prove that this moment is for the abundant quenching effect of the reversed reaction that decomposition took place of the trichlorosilane that is inhibited, preferably at 1 second with interior quenching to 650 ℃.Next, the reaction that has imported cooling gas is generated gas import in the cooling separator 12 by vapor pipe 11, here be further cooled, isolating trichlorosilane is directed in the water distilling apparatus 13, and condensation is collected.
In addition, in example shown in Figure 1, separate unreacted hydrogen etc. in above-mentioned cooling separator 12, this hydrogen imports to by cooling gas ingress pipe 14 in the base end part of vapor pipe 11, utilizes as cooling gas again.
In embodiments of the present invention, in using the example of hydrogen as cooling gas, when deriving reaction generation gas by reaction chamber 2, in reaction generation gas, sneak into hydrogen and cool off reaction generation gas, thereby make the reaction of the condition of high temperature generate quenching of gases, the reversed reaction that can suppress to change simultaneously improves the turnover ratio that generates trichlorosilane.Above-mentioned effect becomes big when under higher temperature conversion reaction taking place, particularly remarkable above above-mentioned effect under 1200 ℃ the temperature.Particularly sneak into hydrogen will react the temperature that generates below the gas cooling to 650 ℃ the time, reaction generate gas by quenching to the temperature range that can fully suppress the reversed reaction of conversion reaction, can improve the turnover ratio that generates trichlorosilane.
Use tetrachloro silicane to replace hydrogen or with it with hydrogen during as cooling gas, also can obtain effect identical when using hydrogen as cooling gas.Under this situation, can will import in the vapor pipe 11 by cooling gas ingress pipe 14 by water distilling apparatus 13 isolating a part of tetrachloro silicanes.
In addition, in embodiments of the present invention, in using the example of hydrogenchloride as cooling gas, by cooling gas ingress pipe 14 hydrogenchloride is imported in the vapor pipe 11, make reaction generate gas to be cooled to temperature below 650 ℃ with interior speed of cooling by sneaking into hydrogenchloride with 1 second, suppress the pair of polymkeric substance and give birth to, can improve the turnover ratio of trichlorosilane.
Usually, with reaction generate gas 1 second with interior utmost point short period of time quenching during to the temperature of the reversed reaction that decomposition was produced that trichlorosilane does not obviously take place, the secondary easily polymkeric substance of giving birth in process of cooling.The following generation of this polymkeric substance: shown in (4), because the SiCl that the decomposition of trichlorosilane generates
2, for another example shown in the following formula (5), SiCl
2With SiCl
4The generation polymkeric substance reacts.This SiCl
2At high temperature more generations.Therefore increase when the pair life of polymkeric substance under with higher temperature conversion reaction takes place, particularly surpass under 1200 ℃ the temperature remarkable.
SiHCl
3→SiCl
2+HCl …(4)
SiCl
2+SiCl
4→Si
2Cl
6 …(5)
On the other hand, shown in (6), hydrogenchloride and SiCl
2Reaction has promoted to generate the reaction of trichlorosilane, so hydrogenchloride has the secondary effect of giving birth to of the polymkeric substance that suppresses above-mentioned reaction formula (4).In addition, shown in following reaction formula (7), (8), (9) etc., hydrogenchloride also has the decomposition effect of secondary polymkeric substance of giving birth to for the time being.
SiCl
２+HCl→SiHCl
３ …(6)
Si
2Cl
6+HCl→SiHCl
3+SiCl
4 …(7)
Si
3Cl
8+2HCl→2SiHCl
3+SiCl
4 …(8)
Si
2H
2Cl
4+2HCl→2SiHCl
3 …(9)
Therefore, use hydrogenchloride as cooling gas, sneaking into hydrogenchloride will react and generate gas with 1 second during with the temperature below the interior speed of cooling quenching to 650 ℃, generate gas by the temperature range below the quenching to 650 ℃ by importing hydrogenchloride, the pair life of polymkeric substance simultaneously is inhibited, and can improve the turnover ratio of trichlorosilane.And can prevent that secondary polymkeric substance of giving birth to is attached on the wall of pipeline problems such as blocking pipeline, can keep pipeline etc. well.Above-mentioned effect increases when under higher temperature conversion reaction taking place, particularly remarkable above above-mentioned effect under 1200 ℃ the temperature.
Embodiment
Below, provide embodiments of the invention.Need to prove that technical scope of the present invention is not limited to above-mentioned embodiment and following examples, in the scope that does not break away from main idea of the present invention, can add various changes.
[embodiment 1]
Use preparation facilities shown in Figure 1, in reaction chamber, supply with the mixed gas (H of hydrogen and tetrachloro silicane
2/ STC mol ratio is 2), under the temperature of reaction shown in the table 1, react, generate trichlorosilane.By vapor pipe 11 mixed gas that generates is exported to when outdoor, the cooling gas shown in the table 1 is imported in the above-mentioned generation mixed gas, be cooled to the temperature shown in the table 1 generating mixed gas by cooling gas ingress pipe 14.It the results are shown in Table 1.
Shown in the result of table 1, by with H
2, STC imports to as cooling gas and generates in the mixed gas, can with generate mixed gas 1 second with below the interior quenching to 650 ℃, can improve the production rate of trichlorosilane (TCS).
[table 1]
(notes) cooling gas import volume is the amount with respect to Si:1mol contained among the raw material STC
The TCS production rate is the ratio (mol%) of TCS growing amount with respect to raw material STC
[embodiment 2]
Use HCl as cooling gas, under the conditions shown in Table 2 HCl is imported in the generation mixed gas, be cooled to the temperature shown in the table 2 generating mixed gas.It the results are shown in Table 2.Shown in the result of table 2,, HCl generates in the mixed gas, even quenching can not produce polymkeric substance yet by being imported to as cooling gas.
[table 2]
(notes) cooling gas import volume is the amount with respect to Si:1mol contained among the raw material STC
Industrial applicability
As mentioned above, preparation method and the trichlorosilane preparation according to trichlorosilane of the present invention fills Put, when deriving generation gas by reative cell, import take hydrogen, tetrachloro silicane or hydrogen chloride as main The refrigerating gas of body cools off above-mentioned generation gas, and is therefore rapid at the generation gas that makes the condition of high temperature In the time of cold, the back reaction of conversion reaction is suppressed, and also suppressed the pair of polymer and given birth to, so Can obtain trichlorosilane with high-conversion rate. Therefore, the present invention is industrial extremely useful.
Claims (11)
1. the preparation method of trichlorosilane, this preparation method has following steps: tetrachloro silicane and hydrogen are imported in the reaction chamber, make it to react under the temperature more than 800 ℃, generate the step of the mixed gas that comprises trichlorosilane and hydrogenchloride; And when deriving above-mentioned mixed gas, in this mixed gas, import the step of cooling off this mixed gas based at least a cooling gas in hydrogen, tetrachloro silicane or the hydrogenchloride by above-mentioned reaction chamber.
2. the preparation method of the trichlorosilane of claim 1, the temperature that wherein imports to the cooling gas in the mixed gas is-60 ℃～650 ℃.
3. the preparation method of the trichlorosilane of claim 1, wherein to generate the temperature of reaction of step be more than 1200 ℃ to mixed gas.
4. the preparation method of the trichlorosilane of claim 1 wherein imports the cooling gas based on hydrogen or tetrachloro silicane, and above-mentioned mixed gas is cooled to below 650 ℃.
5. the preparation method of the trichlorosilane of claim 1 wherein imports the cooling gas based on hydrogenchloride, with above-mentioned mixed gas at 1 second with below the internal cooling to 650 ℃.
6. the preparation method of the trichlorosilane of claim 1, the mixed gas that wherein will import cooling gas imports in the water cooler, and the unreacted hydrogen of condensation separation utilizes isolating hydrogen-containing gas as cooling gas again.
7. the preparation facilities of trichlorosilane, this preparation facilities possesses following equipment: tetrachloro silicane and hydrogen are reacted under the temperature more than 800 ℃, generate the reaction chamber of the mixed gas that comprises trichlorosilane and hydrogenchloride; The mixed gas that above-mentioned mixed gas is exported to the reaction chamber outside is derived equipment; And will import to cooling gas introducing equipment in the above-mentioned mixed gas based at least a cooling gas in hydrogen, tetrachloro silicane or the hydrogenchloride, this cooling gas introducing equipment is connected on the above-mentioned mixed gas derivation equipment.
8. the trichlorosilane preparation facilities of claim 7, wherein temperature of reaction is more than 1200 ℃.
9. the trichlorosilane preparation facilities of claim 7, wherein on the cooling gas introducing equipment, be connected with supply line based on the cooling gas of hydrogen or tetrachloro silicane, to import to based on the cooling gas of hydrogen or tetrachloro silicane in the above-mentioned mixed gas, above-mentioned mixed gas will be cooled to below 650 ℃.
10. the trichlorosilane preparation facilities of claim 7, wherein on the cooling gas introducing equipment, be connected with supply line based on the cooling gas of hydrogenchloride, to import to based on the cooling gas of hydrogenchloride in the above-mentioned mixed gas, with above-mentioned mixed gas at 1 second with below the internal cooling to 650 ℃.
11. the trichlorosilane preparation facilities of claim 7, it possesses: import the water cooler of mixed gas, imported cooling gas in the above-mentioned mixed gas; And in the cooling gas introducing equipment, supply with circulation line based on the hydrogen-containing gas of unreacted hydrogen through the water cooler condensation separation.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006302056 | 2006-11-07 | ||
| JP302056/2006 | 2006-11-07 | ||
| JP273545/2007 | 2007-10-22 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102753477A (en) * | 2010-01-18 | 2012-10-24 | 赢创德固赛有限公司 | "Closed loop" method for producing trichlorosilane from metallurgical silicon |
| CN103228664A (en) * | 2010-10-27 | 2013-07-31 | Gtat有限公司 | Hydrochlorination heater and related methods therefor |
| CN103261207A (en) * | 2010-12-17 | 2013-08-21 | 道康宁公司 | Method of making a trihalosilane |
| US9296765B2 (en) | 2012-08-13 | 2016-03-29 | Dow Corning Corporation | Method of preparing an organohalosilane |
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2007
- 2007-10-26 CN CNA2007800244818A patent/CN101479192A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102753477A (en) * | 2010-01-18 | 2012-10-24 | 赢创德固赛有限公司 | "Closed loop" method for producing trichlorosilane from metallurgical silicon |
| CN103228664A (en) * | 2010-10-27 | 2013-07-31 | Gtat有限公司 | Hydrochlorination heater and related methods therefor |
| CN103228664B (en) * | 2010-10-27 | 2016-06-22 | Gtat有限公司 | Hydrochlorination heater and correlation technique thereof |
| CN103261207A (en) * | 2010-12-17 | 2013-08-21 | 道康宁公司 | Method of making a trihalosilane |
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