CN101445245B - Method for producing trichlorosilane by using silicon tetrachloride - Google Patents
Method for producing trichlorosilane by using silicon tetrachloride Download PDFInfo
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- CN101445245B CN101445245B CN2008101480674A CN200810148067A CN101445245B CN 101445245 B CN101445245 B CN 101445245B CN 2008101480674 A CN2008101480674 A CN 2008101480674A CN 200810148067 A CN200810148067 A CN 200810148067A CN 101445245 B CN101445245 B CN 101445245B
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- silicon tetrachloride
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Abstract
This invention discloses a method for producing SiHCl3 by using SiCl4, comprising following steps: firstly, rectifying, refining and purifying to the silicon tetrachloride so as to make the purity of the silicon tetrachloride be 99%; secondly, purifying the hydrogen so as to make the purity of the hydrogen be more than 99%; thirdly, mixing the purified silicon tetrachloride with hydrogen, wherein the proportion of the silicon tetrachloride and the hydrogen is 1mol: 2-5mol; fourthly, leading the mixed gas to react under the condition that is temperature is 1200 to 1400 degrees centigrade and the pressure is 0.2- 0.60MPa, with the air input of 260-530Nm3/h. This method is convenient for being controlled, and is in favor of recovering the silicon tetrachloride and in favor of industry construction, greatly.
Description
Technical field
The present invention relates to field polysilicon, especially a kind of is the method that raw material is produced trichlorosilane with the silicon tetrachloride.
Background technology
The reasonable utilization of silicon tetrachloride in the production of polysilicon, be to guarantee that polysilicon normally moves, the important topic of large-scale production, though silicon tetrachloride has multiple use (as white carbon black, organosilicon, quartz ware etc.), but do not belong to the production of polysilicon industry technology, to in production of polysilicon, should make good use of silicon tetrachloride, way the most easily; Be exactly that it is passed through special technique technology, change into the raw material trichlorosilane of polysilicon.Silicon tetrachloride, hydrogen, silica flour direct synthesis technique were once arranged for many years, but it is all tediously long because of flow process, the device structure complexity, the material requirement is harsh, technology adds the solid nickel powder, the silica flour condition is restive, can be handling difficult, be difficult to realize the continous-stable operation, difficultly hold into the production of polysilicon flow process with continuity.
Notification number CN101254921A has mentioned hot method for hydrogenation, relies on Electric heating with SiCl
4Be converted into SiHCl
3Because existing reaction conditions is not easy to recycling SiCl
4, hot in addition hydrogenation process transforms SiCl
4A transformation efficiency only 20%, so energy consumption height, and facility investment is huge.The therefore existing uneconomical practicality of this method.
Summary of the invention
The purpose of this invention is to provide a kind of SiCl of utilization
4The SiHCl that produces
3Method, these method concrete steps are as follows:
The first step is carried out rectification and purification to silicon tetrachloride and is purified, and makes silicon tetrachloride purity 99%.
Second step purified hydrogen, and hydrogen purity is reached more than 90%, and is preferred more than 99%.
The 3rd step, silicon tetrachloride and hydrogen after purifying are mixed, wherein the ratio of silicon tetrachloride and hydrogen is 1mol: 2-5mol.According to reaction formula, this reaction is for waiting mol reaction, i.e. the H2 of the STC of 1mol and 1mol reaction generates the TCS of 1mol and the HCL of 1mol.The ratio of H2 and STC is 1: 1, and present method can make reaction carry out towards the positive reaction direction by improving concentration of reactants.So more help the conversion of STC, and help improving speed of response.
In the 4th step, with air input 260-530Nm3/h mixed gas is fed under the condition that temperature is 1200-1400 ℃ and pressure 0.2-0.60MPaG and to react.More help the carrying out that react owing to increase pressure, increased the chance of reactant molecule with the heating element contact, make the transformation efficiency of single reaction higher, but the too high requirement to system device of pressure also uprises thereupon, increase equipment research and development and production cost, the safe and stable operation of simultaneously also unfavorable and system.This method is selected the pressure parameter of 0.2-0.6MPa for use, on the one hand higher transformation efficiency is arranged, and is not high to equipment requirements on the other hand, operating safety.
This method is according to STC structure of matter characteristics, according to surface heat chemical reaction thermodynamics, kinetics mechanism, under temperature 1200-1400 ℃, pressure 0.2-0.60MPaG, with the gas mixture proportioning; H2/STC=2-5/1 (MOL) breaks the STC molecular structure, and according to the extremely strong avidity of H+, CL-, feeds the 260-530Nm3/h gas mixture in thermal field, obtain STC and changed into TCS, this method is convenient to control, helps the silicon tetrachloride circulation and reclaims, and is very beneficial for industrial implementation.
Embodiment
Disclosed all features in this specification sheets, or the step in disclosed all methods or the process except mutually exclusive feature and/or step, all can make up by any way.
Disclosed arbitrary feature in this specification sheets (comprising any accessory claim, summary and accompanying drawing) is unless special narration all can be replaced by other equivalences or the alternative features with similar purpose.That is, unless special narration, each feature is an example in a series of equivalences or the similar characteristics.
The step of present method is as follows:
The first step is carried out rectification and purification to silicon tetrachloride (STC) and is purified, and makes silicon tetrachloride purity be not less than 99%.
Second step purified hydrogen, and hydrogen purity is reached more than 90%, and is preferred more than 99%.
The 3rd step, silicon tetrachloride and hydrogen after purifying are mixed, wherein the ratio of silicon tetrachloride and hydrogen is 1mol: 2-5mol.According to reaction formula, this reaction is for waiting mol reaction, i.e. the H2 of the STC of 1mol and 1mol reaction generates the trichlorosilane (TCS) of 1mol and the HCL of 1mol.The ratio of H2 and STC is 1: 1, and present method can make reaction carry out towards the positive reaction direction by improving concentration of reactants.So more help the conversion of STC, and help improving speed of response.
In the 4th step, with air input 260-530Nm3/h mixed gas is fed under the condition that temperature is 1200-1400 ℃ and pressure 0.2-0.60MPaG and to react.More help the carrying out that react owing to increase pressure, increased reactant molecule and increased effective collision between the reaction molecular simultaneously with the chance of heating element contact, make the transformation efficiency of single reaction higher, but the too high requirement to system device of pressure also uprises thereupon, increase equipment research and development and production cost, the safe and stable operation of simultaneously also unfavorable and system.This method is selected the pressure parameter of 0.2-0.6MPa for use, on the one hand higher transformation efficiency is arranged, and is not high to equipment requirements on the other hand, operating safety.
Wherein the output rating of the size of air input (being mixed gas flow) and reactor volume, well heater, the real reaction temperature in the reactor are relevant.Air input is too big, and promptly mixed gas flow is too big, can cause temperature to be difficult to reach the temperature of needs, and air input is too little, and promptly mixed gas flow is too little, and temperature raises too fast, and easily above temperature required, heat energy utilization is low on the one hand, and temperature is too high also dangerous in addition.General air input should determine that air flow should make temperature of reactor in needed temperature range according to temperature of reactor, and such as 1200-1300 ℃, air flow is that 260-530Nm3/h is proper under the existence conditions.
Table 1 embodiment 1-4
| Sequence number | H 2/STC (MOL) | Temperature ℃ | Pressure MPaG | A transformation efficiency % |
| 1 | 1∶1 | 1250 | 0.3 | 10 |
| 2 | 2∶1 | 1250 | 0.3 | 13 |
| 3 | 4∶1 | 1250 | 0.3 | 24 |
| 4 | 5∶1 | 1250 | 0.3 | 25 |
Table 1 is embodiment 1-4, under the identical situation of temperature and pressure, the conversion situation under the ratio different situations of silicon tetrachloride and hydrogen, as can be seen, by increase silicon tetrachloride and hydrogen ratio reaction is carried out towards the positive reaction direction, so more help the conversion of STC.
Table 2 embodiment 5-10
| Sequence number | H 2/STC (MOL) | Temperature ℃ | Pressure MPaG | A transformation efficiency % |
| 5 | 3∶1 | 1250 | 0.3 | 23 |
| 6 | 3∶1 | 1250 | 0.2 | 15 |
| 7 | 3∶1 | 1250 | 0.25 | 20 |
| 8 | 3∶1 | 1250 | 0.35 | 23 |
| 9 | 3∶1 | 1250 | 0.4 | 23 |
| 10 | 3∶1 | 1250 | 0.55 | 24 |
Embodiment 5-10 is identical in temperature, under the identical situation of the ratio of silicon tetrachloride and hydrogen, conversion situation under the situation of continuous adjustment pressure, as can be seen, more help the carrying out that react by increasing pressure within the specific limits, increased reactant molecule and increased effective collision between the reaction molecular simultaneously with the chance of heating element contact, make the transformation efficiency of single reaction higher, but increased pressure arrives to a certain degree, provide little to transformation efficiency, and the requirement of system device also uprised thereupon, increase equipment research and development and production cost, the safe and stable operation of simultaneously also unfavorable and system.Generally select the pressure parameter of 0.3-0.6MPa for use, on the one hand higher transformation efficiency is arranged, not high to equipment requirements on the other hand, operating safety.
Table 2 embodiment 11-16
| Sequence number | H 2/STC (MOL) | Temperature ℃ | Pressure MPaG | A transformation efficiency % |
| 11 | 3∶1 | 1000 | 0.3 | 14 |
| 12 | 3∶1 | 1100 | 0.3 | 15 |
| 13 | 3∶1 | 1200 | 0.3 | 19 |
| 14 | 3∶1 | 1250 | 0.3 | 23 |
| 15 | 3∶1 | 1300 | 0.3 | 23 |
| 16 | 3∶1 | 1400 | 0.3 | 24 |
Under the situation that embodiment 11-16 is identical at pressure, the ratio of silicon tetrachloride and hydrogen is identical, constantly adjust the conversion situation of temperature, increase temperature as can be seen within the specific limits and help reaction, but transformation efficiency also is difficult to improve when to a certain degree increasing temperature again when temperature increases to, general temperature choose 1200-1400 ℃ proper.
Though condition of the present invention can not improve transformation efficiency, described condition realizes that easily this method is convenient to control, helps the silicon tetrachloride circulation and reclaims, and is very beneficial for industrial implementation.
The present invention is not limited to aforesaid embodiment.The present invention expands to any new feature or any new combination that discloses in this manual, and the arbitrary new method that discloses or step or any new combination of process.
Claims (4)
1. one kind is utilized SiCl
4Produce SiHCl
3Method, these method concrete steps are as follows:
The first step is carried out rectification and purification to silicon tetrachloride and is purified, and makes silicon tetrachloride purity 99%;
Second step purified hydrogen, and hydrogen purity is reached more than 99%;
The 3rd step, silicon tetrachloride and hydrogen after purifying are mixed, wherein the ratio of silicon tetrachloride and hydrogen is 1mol: 2-5mol;
In the 4th step, mixed gas fed under the condition that temperature is 1250-1400 ℃ and pressure 0.2-0.6MPaG react;
The described air input that mixed gas is fed should determine that air input should make temperature of reactor in needed temperature range according to temperature of reactor, and described air input is 260-530Nm
3/ h.
2. the SiCl that utilizes as claimed in claim 1
4Produce SiHCl
3Method, it is characterized in that: the ratio of silicon tetrachloride and hydrogen is 1mol: 3-5mol.
3. the SiCl that utilizes as claimed in claim 1
4Produce SiHCl
3Method, it is characterized in that: temperature is 1250 ℃.
4. the SiCl that utilizes as claimed in claim 1
4Produce SiHCl
3Method, it is characterized in that: pressure is 0.25-0.30MPaG.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101480674A CN101445245B (en) | 2008-12-26 | 2008-12-26 | Method for producing trichlorosilane by using silicon tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101480674A CN101445245B (en) | 2008-12-26 | 2008-12-26 | Method for producing trichlorosilane by using silicon tetrachloride |
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| Publication Number | Publication Date |
|---|---|
| CN101445245A CN101445245A (en) | 2009-06-03 |
| CN101445245B true CN101445245B (en) | 2011-04-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101480674A Expired - Fee Related CN101445245B (en) | 2008-12-26 | 2008-12-26 | Method for producing trichlorosilane by using silicon tetrachloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101700886B (en) * | 2009-11-30 | 2011-08-03 | 乐山乐电天威硅业科技有限责任公司 | Method for preparing trichlorosilane from tetrachlorosilane |
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