CN103253676A - Preparation method of trichlorosilane - Google Patents
Preparation method of trichlorosilane Download PDFInfo
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- CN103253676A CN103253676A CN2013101699606A CN201310169960A CN103253676A CN 103253676 A CN103253676 A CN 103253676A CN 2013101699606 A CN2013101699606 A CN 2013101699606A CN 201310169960 A CN201310169960 A CN 201310169960A CN 103253676 A CN103253676 A CN 103253676A
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Abstract
The invention discloses a preparation method of trichlorosilane. The preparation method comprises the following equipment and process: the production equipment mainly consists of a coupling tower, a reboiler and a condenser, wherein the coupling tower is composed of a steam stripping section, a steam stripping reaction section, an absorption reaction section and a rectification section; novel differential reaction rectification devices are installed inside the steam stripping reaction section and the absorption reaction section; tower internals are installed inside the steam stripping section and the rectification section; the tower internals are tower plates or padding; the preparation process of trichlorosilane comprises the following steps of: feeding the raw material dichlorosilane into the tower from the part between the steam stripping reaction section and the absorption reaction section, feeding the raw material silicon tetrachloride into the tower from the part between the absorption reaction section and the rectification section; separating the trichlorosilane from the dichlorosilane; under the action of the differential reaction rectification devices, synthesizing the trichlorosilane, further separating trichlorosilane from reactant and mixing trichlorosilane with gas phase, and finally feeding the gas phase rich in trichlorosilane obtained from the absorption reaction section into the rectification section; and purifying the trichlorosilane.
Description
Technical field
The present invention relates to purify to the anti-disproportionation conversing technology of byproduct dichloro-dihydro silicon the solar-grade polysilicon production process from metallurgical-grade polysilicon, be specially a kind of preparation method of trichlorosilane.This method is to utilize a kind of novel differential reactive distillation equipment to realize the coupling of rectifying, absorption, reaction and stripping process, the anti-disproportionation of dichloro-dihydro silicon is converted into the preparation method of trichlorosilane.
Background technology
In polysilicon product was produced, the improvement Siemens Method was owing to technical maturity is widely adopted.This technology is raw material with the trichlorosilane, obtains polysilicon product by hydrogen reduction in reduction furnace.But in the synthetic of trichlorosilane and reduction workshop section, can generate chlorosilane byproducts such as silicon tetrachloride and dichloro-dihydro silicon, this has had a strong impact on product yield and production cost.At present, can adopt cold hydrogenation technology to make it be converted into trichlorosilane for silicon tetrachloride, but also can generate a part of dichloro-dihydro silicon simultaneously.For dichloro-dihydro silicon, be the technology of feedstock production polysilicon though have with it in the world, its technical difficulty and production cost are all higher.So most of enterprises adopt fixed-bed reactor, utilize anti-disproportionation know-why, realize the anti-disproportionation reaction of dichloro-dihydro silicon and silicon tetrachloride, make it be converted into trichlorosilane, but for dichloro-dihydro silicon being transformed as far as possible fully, adopted the silicon tetrachloride excessive response, made reactor outlet concentration trichlorosilane have only about 10%, this directly causes the later separation energy consumption higher.
Chinese patent CN101955187A discloses and has a kind ofly utilized anti-disproportionation reaction by reactive distillation trichlorosilane method and apparatus processed.This invention is by three tower process flow processs, can realize that dichloro-dihydro silicon and silicon tetrachloride are converted into trichlorosilane, and theoretical yield can reach 100%, but but not disclosing the product per pass conversion of energy consumption and the first reactive distillation Tata bottom outlet trichlorosilane concentration and realization in its invention, is that general say separation and the theoretical reaction conversion ratio of recirculation by material can reach 100%.In addition, purpose product trichlorosilane boiling point is between dichloro-dihydro silicon and silicon tetrachloride, and this reaction is liquid phase reaction, so when adopting the single reaction distillation technology to transform, once transform the high conversion that is difficult to the realization response thing, can only make the method for excessive unreacted reactant circulation realize the raising of transformation efficiency by later separation.
Chinese patent CN102516036A discloses a kind of differential apparatus for reactive distillation, has realized that by this equipment the MTBE catalytic distillation is synthetic.This invention has realized the column plate micronized, and catalytic unit and mass transfer unit are staggered, and has avoided catalyzed reaction and has separated the mass transfer process subregion and carry out, and has improved reaction conversion ratio and separation efficiency.This invention has also realized a kind of catalyst loading pattern of micronized in addition, has realized the micronized of fixed-bed reactor.Because this technology is last word, less to its experimental study, its shortcoming is not appeared in the newspapers.
Summary of the invention
At existing dichloro-dihydro silicon fixed-bed conversion technical deficiency, the technical problem that quasi-solution of the present invention is determined is, a kind of preparation method of trichlorosilane is provided, this preparation method utilizes differential catalytic rectifying tower plate, adopt integral design method, absorption, reaction, rectifying and four PROCESS COUPLING of stripping in same tower equipment, are realized that dichloro-dihydro silicon and silicon tetrachloride high conversion and the efficient energy-saving of coupling tower move.
The technical scheme that the present invention solve the technical problem is, designs a kind of preparation method of trichlorosilane, this preparation method, and this preparation method adopts following equipment and technology:
This production unit mainly is made of coupling tower, reboiler and condenser, and described coupling tower is made of stripping stage, stripping conversion zone, absorption reaction section and rectifying section; Differential catalytic rectifying tower plate is installed in stripping conversion zone and absorption reaction section, column internals is installed in stripping stage and the rectifying section, column internals is column plate or filler;
Trichlorosilane preparation technology is: raw material dichloro-dihydro silicon enters in the tower between stripping conversion zone and absorption reaction section, and the raw material silicon tetrachloride enters in the tower between absorption reaction section and the rectifying section; The part vaporization will take place at once in the dichloro-dihydro silicon that enters in the tower, the silicon tetrachloride that the dichloro-dihydro silicon of not vaporizing to enter stripping conversion zone and stripping stage rising downwards reacts, because temperature is higher, trichlorosilane meeting and dichloro-dihydro silicon that reaction obtains are vaporized together, the realization trichlorosilane separates with silicon tetrachloride, thereby improves transformation efficiency; Vaporization dichloro-dihydro silicon has directly entered the absorption reaction section, owing in the middle of gas phase, there is not catalyzer, so the dichloro-dihydro silicon in the gas phase must be absorbed in the liquid phase could react, the silicon tetrachloride that enters the absorption reaction section from top just plays the effect of absorption agent, dichloro-dihydro silicon in the middle of the gas phase is absorbed in the silicon tetrachloride, under the effect of differential reaction and rectification device, realize the synthetic of trichlorosilane, and with trichlorosilane and reactants separate in the middle of gas phase, the gas phase that is rich in trichlorosilane that obtains from the absorption reaction section enters rectifying section at last; Enter the gas phase of rectifying section, under the effect of trim the top of column, realize the purification to trichlorosilane, obtain the higher trichlorosilane product of concentration at cat head; The effect of tower bottom stripping stage is that the trichlorosilane that the stripping conversion zone does not have vaporization to remove further is removed to gas phase, and the still raffinate that makes tower reactor intermittently discharge does not contain trichlorosilane.
Preparation method's of the present invention condition is: working pressure 0.1-0.4MPa; Service temperature is 10-130 ℃; Operating reflux ratio is 1.0-3.0; Dichloro-dihydro silicon and silicon tetrachloride mol ratio are 1-1:1.2.
Compared with prior art, preparation method of the present invention is because utilize differential catalytic rectifying tower plate (novel differential reaction and rectification device), realized the coupling of micronized reaction, absorption, rectifying and stripping process, and only in a coupling tower, finish, realized the high reaction conversion ratio of dichloro-dihydro silicon and silicon tetrachloride, thereby having the operational path weak point, operation energy consumption is low, characteristics such as reaction efficiency height.
Description of drawings
Fig. 1 is production unit and the technological process synoptic diagram of a kind of embodiment of trichlorosilane preparation method of the present invention.
Embodiment
Further describe the present invention below in conjunction with embodiment and accompanying drawing thereof.
The trichlorosilane preparation method of the present invention's design (being called for short the preparation method, referring to Fig. 1), this preparation method adopts following production unit and technology:
This production unit mainly is made of coupling tower 1, reboiler 2 and condenser 7.Described coupling tower 1 is made of stripping stage 3, stripping conversion zone 4, absorption reaction section 5 and rectifying section 6; Differential catalytic rectifying tower plate is installed in stripping conversion zone 4 and absorption reaction section 5, in stripping stage 3 and the rectifying section 6 column internals is installed, column internals can be column plate or filler.
Trichlorosilane (TCS) preparation technology is: raw material dichloro-dihydro silicon (DCS) enters in the tower between stripping conversion zone 4 and absorption reaction section 5, and raw material silicon tetrachloride (STC) enters in the tower between absorption reaction section 5 and rectifying section 6.The part vaporization will take place at once in the dichloro-dihydro silicon that enters in the tower, the silicon tetrachloride (STC) that the dichloro-dihydro silicon of not vaporizing to enter stripping conversion zone 4 and stripping stage 3 risings downwards reacts, because temperature is higher, trichlorosilane meeting and dichloro-dihydro silicon that reaction obtains are vaporized together, the realization trichlorosilane separates with silicon tetrachloride, thereby improves transformation efficiency; Vaporization dichloro-dihydro silicon has directly entered absorption reaction section 5, owing in the middle of gas phase, there is not catalyzer, so the dichloro-dihydro silicon in the gas phase must be absorbed in the liquid phase could react, the silicon tetrachloride that enters absorption reaction section 5 from top just plays the effect of absorption agent, dichloro-dihydro silicon in the middle of the gas phase is absorbed in the silicon tetrachloride, under the effect of differential reaction and rectification device, realize the synthetic of trichlorosilane, and with trichlorosilane and reactants separate in the middle of gas phase, the gas phase that is rich in trichlorosilane that obtains from absorption reaction section 5 enters rectifying section at last.Enter the gas phase of rectifying section, under the effect of trim the top of column, realize the purification to trichlorosilane.The effect of tower bottom stripping stage 3 is that the trichlorosilane that stripping conversion zone 4 does not have vaporization to remove further is removed to gas phase, and the still raffinate that makes tower reactor intermittently discharge does not contain trichlorosilane.Reboiler 2 provides stripping stage 3 gas phases to reflux, and condenser 7 provides the liquid-phase reflux of rectifying section 6.
The operational condition of building-up process of the present invention is: working pressure 0.1-0.4MPa; Service temperature is 10-130 ℃; Operating reflux ratio is 1.0-3.0; Dichloro-dihydro silicon and silicon tetrachloride mol ratio are 1-1:1.2.
Chemical reaction involved in the present invention mainly is:
Production technology principle of the present invention and process are: the dichloro-dihydro silicon raw material by a last workshop section sends here enters in the tower between stripping conversion zone 4 and absorption reaction section 5; Because temperature is higher in the tower, the part vaporization takes place in the dichloro-dihydro silicon that enters in the tower at once, and the dichloro-dihydro silicon of vaporization has directly entered absorption reaction section 5, and another raw material silicon tetrachloride then enters in the tower between absorption reaction section 5 and rectifying section 6; Because its boiling point is higher, can directly enter reaction absorber portion 5, as the dichloro-dihydro silicon DCS in the absorption agent absorption gas phase, in liquid phase, generate trichlorosilane with the catalyzer contact reacts, under the effect of differential reactive distillation equipment, realize the synthetic of trichlorosilane, and with trichlorosilane and reactants separate in the middle of gas phase; The gas phase that is rich in trichlorosilane that obtains from absorption reaction section 5 enters rectifying section 6 at last; Enter the gas phase of rectifying section, under the cat head liquid-phase reflux effect that condenser 7 provides, realize trichlorosilane) purification, namely obtain the higher trichlorosilane product of concentration at cat head.
There is not the dichloro-dihydro silicon of vaporization then directly to enter stripping conversion zone 4 downwards, its can with stripping stage 3 rising gas in silicon tetrachloride react, and because this section temperature is higher, trichlorosilane meeting and dichloro-dihydro silicon that reaction obtains are vaporized together, and transfer in the middle of the gas phase, the realization trichlorosilane separates with silicon tetrachloride, thereby improves transformation efficiency.In addition, tower bottom stripping stage 3 is under the effect of the rising steam that tower bottom reboiler 2 provides, the trichlorosilane that the stripping conversion zone can not had vaporization to remove further is removed to gas phase, last tower reactor is not contained the still liquid of trichlorosilane and dichloro-dihydro silicon, and the still raffinate that is rich in silicon tetrachloride and impurity is intermittently discharged outside the coupling tower.
Below be specific embodiments of the invention.Described embodiment only is for specific descriptions the present invention, rather than restriction the application's claim.
The molar ratio of dichloro-dihydro silicon (DCS) and silicon tetrachloride (STC): 1:1.2;
Catalytic rectifying tower working pressure: 0.15MPa;
Service temperature: 10-85 ℃;
The tower structure pattern is from top to bottom: the efficient structured packing of 3m (rectifying section)+20 layer differential catalytic rectifying tower plate (absorption reaction section)+10 layers of differential catalytic rectifying tower plate (stripping conversion zone)+efficient structured packing of 3m (stripping stage);
Cat head is formed (m%): trichlorosilane (TCS): 80%, and dichloro-dihydro silicon (DCS): 0.5%, silicon tetrachloride (STC): 19.5%;
Form at the bottom of the tower (m%): trichlorosilane (TCS): 0.0%, dichloro-dihydro silicon (DCS): 0.0%, silicon tetrachloride (STC): 98%, other is 2% years old.
Dichloro-dihydro silicon (DCS) and silicon tetrachloride (STC) molar ratio: 1:1.05;
Catalytic rectifying tower working pressure: 0.2MPa;
Service temperature: 50-105 ℃;
The tower structure pattern is from top to bottom: 10 layers of column plate (rectifying section)+35 layer differential catalytic rectifying tower plate (absorption reaction section)+10 layers of differential catalytic rectifying tower plate (stripping conversion zone)+15 layers of column plate (stripping stage);
Cat head is formed (m%): trichlorosilane (TCS): 97.5%, and dichloro-dihydro silicon (DCS): 0.5%, silicon tetrachloride (STC): 2%;
Form at the bottom of the tower (m%): trichlorosilane (TCS): 0.0%, dichloro-dihydro silicon (DCS): 0.0%, silicon tetrachloride (STC): 98%, other: 2%.
Embodiment 3
Dichloro-dihydro silicon (DCS) and silicon tetrachloride (STC) molar ratio: 1:1;
Catalytic rectifying tower working pressure: 0.4MPa;
Service temperature: 60-115 ℃;
The tower structure pattern is from top to bottom: 10 layers of column plate (rectifying section)+35 layer differential catalytic rectifying tower plate (absorption reaction section)+10 layers of differential catalytic rectifying tower plate (stripping conversion zone)+15 layers of column plate (stripping stage);
Cat head is formed (m%): trichlorosilane (TCS): 97.0%, and dichloro-dihydro silicon (DCS): 1.0%, silicon tetrachloride (STC): 2%;
Form at the bottom of the tower (m%): trichlorosilane (TCS): 0.0%, dichloro-dihydro silicon (DCS): 0.0%, silicon tetrachloride (STC): 98%, other: 2%.
Claims (4)
1. the preparation method of a trichlorosilane, this preparation method adopts following equipment and technology:
This production unit mainly is made of coupling tower, reboiler and condenser, and described coupling tower is made of stripping stage, stripping conversion zone, absorption reaction section and rectifying section; Differential catalytic rectifying tower plate is installed in stripping conversion zone and absorption reaction section, column internals is installed in stripping stage and the rectifying section, column internals is column plate or filler;
Trichlorosilane preparation technology is: raw material dichloro-dihydro silicon enters in the tower between stripping conversion zone and absorption reaction section, and the raw material silicon tetrachloride enters in the tower between absorption reaction section and the rectifying section; The part vaporization will take place at once in the dichloro-dihydro silicon that enters in the tower, the silicon tetrachloride that the dichloro-dihydro silicon of not vaporizing to enter stripping conversion zone and stripping stage rising downwards reacts, because temperature is higher, trichlorosilane meeting and dichloro-dihydro silicon that reaction obtains are vaporized together, the realization trichlorosilane separates with silicon tetrachloride, thereby improves transformation efficiency; Vaporization dichloro-dihydro silicon has directly entered the absorption reaction section, owing in the middle of gas phase, there is not catalyzer, so the dichloro-dihydro silicon in the gas phase must be absorbed in the liquid phase could react, the silicon tetrachloride that enters the absorption reaction section from top just plays the effect of absorption agent, dichloro-dihydro silicon in the middle of the gas phase is absorbed in the silicon tetrachloride, under the effect of differential reaction and rectification device, realize the synthetic of trichlorosilane, and with trichlorosilane and reactants separate in the middle of gas phase, the gas phase that is rich in trichlorosilane that obtains from the absorption reaction section enters rectifying section at last; Enter the gas phase of rectifying section, under the effect of trim the top of column, realize the purification to trichlorosilane; The effect of tower bottom stripping stage is that the trichlorosilane that the stripping conversion zone does not have vaporization to remove further is removed to gas phase, and the still raffinate that makes tower reactor intermittently discharge does not contain trichlorosilane; Reboiler provides the stripping stage gas phase to reflux, and condenser provides the liquid-phase reflux of rectifying section;
Preparation method's of the present invention condition is: working pressure 0.1-0.4MPa; Service temperature is 10-130 ℃; Operating reflux ratio is 1.0-3.0; Dichloro-dihydro silicon and silicon tetrachloride mol ratio are 1-1:1.2.
2. the preparation method of trichlorosilane according to claim 1, the tower structure pattern that this preparation method adopts is from top to bottom: the efficient structured packing of the 3m+20 layers of differential catalytic rectifying tower plate+efficient structured packing of 10 layers of differential catalytic rectifying tower plate+3m;
Cat head is formed (m%): trichlorosilane 80%, dichloro-dihydro silicon 0.5%, silicon tetrachloride 19.5%;
Form at the bottom of the tower (m%): silicon tetrachloride 98%, other is 2% years old.
3. the preparation method of trichlorosilane according to claim 1, the tower structure pattern that this preparation method adopts is from top to bottom: 10 layers of column plate+35 layer differential catalytic rectifying tower plate+10 layers of differential catalytic rectifying tower plate+15 layers of column plate;
Cat head is formed (m%): trichlorosilane 97.5%, dichloro-dihydro silicon 0.5%, silicon tetrachloride 2%;
Form at the bottom of the tower (m%): silicon tetrachloride 98%, other is 2% years old.
4. the preparation method of trichlorosilane according to claim 1, the tower structure pattern that this preparation method adopts is from top to bottom: 10 layers of column plate+35 layer differential catalytic rectifying tower plate+10 layers of differential catalytic rectifying tower plate+15 layers of column plate;
Cat head is formed (m%): trichlorosilane 97.0%, dichloro-dihydro silicon 1.0%, silicon tetrachloride 2%;
Form at the bottom of the tower (m%): silicon tetrachloride 98%, other is 2% years old.
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| CN103553057A (en) * | 2013-11-11 | 2014-02-05 | 新特能源股份有限公司 | Method for treating chlorosilane waste gas through reaction distillation technology |
| CN104140104A (en) * | 2014-07-18 | 2014-11-12 | 中国恩菲工程技术有限公司 | Method for preparing trichlorosilane through device for preparing trichlorosilane |
| CN104140105A (en) * | 2014-07-18 | 2014-11-12 | 中国恩菲工程技术有限公司 | Device for preparing trichlorosilane |
| CN105948059A (en) * | 2016-05-03 | 2016-09-21 | 宜昌南玻硅材料有限公司 | System and method for recycling chlorosilane tail gas |
| CN108910894A (en) * | 2018-08-31 | 2018-11-30 | 内蒙古通威高纯晶硅有限公司 | Trichlorosilane rectification system and rectificating method |
| CN109173310A (en) * | 2018-08-29 | 2019-01-11 | 张家港市科华化工装备制造有限公司 | Dimethoxym ethane rectifying column |
| CN112843765A (en) * | 2020-12-03 | 2021-05-28 | 天津大学 | Micro-scale efficient rectification separation process strengthening device and process |
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| CN103553057A (en) * | 2013-11-11 | 2014-02-05 | 新特能源股份有限公司 | Method for treating chlorosilane waste gas through reaction distillation technology |
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| CN104140104A (en) * | 2014-07-18 | 2014-11-12 | 中国恩菲工程技术有限公司 | Method for preparing trichlorosilane through device for preparing trichlorosilane |
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| CN105948059A (en) * | 2016-05-03 | 2016-09-21 | 宜昌南玻硅材料有限公司 | System and method for recycling chlorosilane tail gas |
| CN109173310A (en) * | 2018-08-29 | 2019-01-11 | 张家港市科华化工装备制造有限公司 | Dimethoxym ethane rectifying column |
| CN108910894A (en) * | 2018-08-31 | 2018-11-30 | 内蒙古通威高纯晶硅有限公司 | Trichlorosilane rectification system and rectificating method |
| CN112843765A (en) * | 2020-12-03 | 2021-05-28 | 天津大学 | Micro-scale efficient rectification separation process strengthening device and process |
| CN112843765B (en) * | 2020-12-03 | 2022-04-01 | 天津大学 | Micro-scale efficient rectification separation process strengthening device and process |
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