CN103253676B - Preparation method of trichlorosilane - Google Patents
Preparation method of trichlorosilane Download PDFInfo
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- CN103253676B CN103253676B CN201310169960.6A CN201310169960A CN103253676B CN 103253676 B CN103253676 B CN 103253676B CN 201310169960 A CN201310169960 A CN 201310169960A CN 103253676 B CN103253676 B CN 103253676B
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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 and purify to the anti-disproportionation conversing technology of byproduct dichlorosilane solar-grade polysilicon production process from metallurgical-grade polysilicon, be specially a kind of preparation method of trichlorosilane.The method utilizes that a kind of novel differential reactive distillation equipment realizes rectifying, absorption, reaction are coupled with stripping process, anti-for dichlorosilane disproportionation are converted into the preparation method of trichlorosilane.
Background technology
In polysilicon product is produced, improved Siemens is widely adopted due to technical maturity.This technique is raw material with trichlorosilane, in reduction furnace, obtain polysilicon product by hydrogen reduction.But in synthesis and the reduction workshop section of trichlorosilane, can generate the chlorosilane such as silicon tetrachloride and dichlorosilane byproduct, this has had a strong impact on product yield and production cost.At present, cold hydrogenation technology can be adopted to make it be converted into trichlorosilane for silicon tetrachloride, but also can generate a part of dichlorosilane simultaneously.For dichlorosilane, although in the world existing with it for the technology of polysilicon prepared by raw material, its technical difficulty and production cost are all higher.So most enterprises adopts fixed-bed reactor, utilize anti-disproportionation know-why, realize the anti-disproportionation reaction of dichlorosilane and silicon tetrachloride, it is made to be converted into trichlorosilane, but in order to dichlorosilane being transformed as far as possible completely, have employed silicon tetrachloride excessive response, make reactor outlet concentration trichlorosilane only have about 10%, this directly causes later separation energy consumption higher.
Chinese patent CN101955187A discloses one and utilizes anti-disproportionation reaction by reactive distillation trichlorosilane method and apparatus.This invention is by three tower process flow processs, dichlorosilane can be realized and converting silicon tetrachloride is trichlorosilane, and theoretical yield can reach 100%, but the product per pass conversion of but not openly energy consumption and the first reactive distillation column tower bottom outlet trichlorosilane concentration and realization in its invention, just general saying can reach 100% by the separation of material and recycle theory reaction conversion ratio.In addition, object product trichlorosilane boiling point is between dichlorosilane and silicon tetrachloride, and this reaction is liquid phase reaction, so when adopting single reaction distillation technology to transform, once transform and be difficult to the high conversion of realization response thing, method that excessive unreacted reactant circulates can only be made to realize the raising of transformation efficiency by later separation.
Chinese patent CN102516036A discloses a kind of differential apparatus for reactive distillation, by this device achieves that MTBE catalytic distillation synthesizes.This invention achieves column plate micronized, and catalytic unit and mass transfer unit are staggered, and avoids catalyzed reaction and is separated mass transfer process subregion and carries out, and improves reaction conversion ratio and separation efficiency.This invention also achieves a kind of catalyst loading pattern of micronized in addition, achieves the micronized of fixed-bed reactor.Because this technology is last word, less to its experimental study, its shortcoming has no report.
Summary of the invention
For existing dichlorosilane 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 column plate, adopt integral design method, absorption, reaction, rectifying and stripping Four processes are coupling in same tower equipment, the efficient energy-saving realizing dichlorosilane and silicon tetrachloride high conversion and coupled runs.
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 process:
This production unit is formed primarily of coupled, reboiler and condenser, and described coupled is made up of stripping stage, stripping conversion zone, absorption reaction section and rectifying section; In stripping conversion zone and absorption reaction section, install differential catalytic rectifying column plate, install column internals in stripping stage and rectifying section, column internals is column plate or filler;
Trichlorosilane preparation technology is: raw material dichlorosilane enters in tower between stripping conversion zone and absorption reaction section, and raw material silicon tetrachloride enters in tower between absorption reaction section and rectifying section; The dichlorosilane entered in tower will generating portion be vaporized at once, the silicon tetrachloride that the dichlorosilane of not vaporizing enters stripping conversion zone and stripping stage rising downwards reacts, because temperature is higher, the trichlorosilane be obtained by reacting can be vaporized together with dichlorosilane, realize being separated of trichlorosilane and silicon tetrachloride, thus improve transformation efficiency; Vaporization dichlorosilane directly enters absorption reaction section, owing to there is no catalyzer in the middle of gas phase, so the dichlorosilane in gas phase must be absorbed in liquid phase and could react, the silicon tetrachloride entering absorption reaction section from top just plays the effect of absorption agent, dichlorosilane in the middle of gas phase is absorbed in silicon tetrachloride, under the effect of differential reaction and rectification device, realize the synthesis of trichlorosilane, and by the middle of trichlorosilane and reactants separate to gas phase, the gas phase being rich in trichlorosilane obtained from absorption reaction section finally enters rectifying section; 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 products of concentration at tower top; The effect of tower lower stripping section is that the trichlorosilane removed of not vaporized by stripping conversion zone is removed to gas phase further, and the still raffinate that tower reactor interval is discharged is not containing trichlorosilane.
The condition of preparation method of the present invention is: working pressure 0.1-0.4MPa; Service temperature is 10-130 DEG C; Operating reflux ratio is 1.0-3.0; Dichlorosilane 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 column plate (novel differential reaction and rectification device), achieve micronized reaction, absorb, the coupling of rectifying and stripping process, and only complete in a coupled, achieve the high reaction conversion ratio of dichlorosilane and silicon tetrachloride, thus have operational path short, operation energy consumption is low, reaction efficiency high.
Accompanying drawing explanation
Fig. 1 is production unit and the technological process schematic diagram of a kind of embodiment of trichlorosilane preparation method of the present invention.
Embodiment
The present invention is further described below in conjunction with embodiment and accompanying drawing thereof.
The trichlorosilane preparation method (being called for short preparation method, see Fig. 1) of the present invention's design, this preparation method adopts following production unit and technique:
This production unit is formed primarily of coupled 1, reboiler 2 and condenser 7.Described coupled 1 is made up of stripping stage 3, stripping conversion zone 4, absorption reaction section 5 and rectifying section 6; In stripping conversion zone 4 and absorption reaction section 5, install differential catalytic rectifying column plate, install column internals in stripping stage 3 and rectifying section 6, column internals can be column plate or filler.
Trichlorosilane (TCS) preparation technology is: raw material dichlorosilane (DCS) enters in tower between stripping conversion zone 4 and absorption reaction section 5, and raw material silicon tetrachloride (STC) enters in tower between absorption reaction section 5 and rectifying section 6.The dichlorosilane entered in tower will generating portion be vaporized at once, the silicon tetrachloride (STC) that the dichlorosilane of not vaporizing enters stripping conversion zone 4 and stripping stage 3 rising downwards reacts, because temperature is higher, the trichlorosilane be obtained by reacting can be vaporized together with dichlorosilane, realize being separated of trichlorosilane and silicon tetrachloride, thus improve transformation efficiency; Vaporization dichlorosilane directly enters absorption reaction section 5, owing to there is no catalyzer in the middle of gas phase, so the dichlorosilane in gas phase must be absorbed in liquid phase and could react, the silicon tetrachloride entering absorption reaction section 5 from top just plays the effect of absorption agent, dichlorosilane in the middle of gas phase is absorbed in silicon tetrachloride, under the effect of differential reaction and rectification device, realize the synthesis of trichlorosilane, and by the middle of trichlorosilane and reactants separate to gas phase, the gas phase being rich in trichlorosilane obtained from absorption reaction section 5 finally enters rectifying section.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 lower stripping section 3 is that the trichlorosilane not had by stripping conversion zone 4 vaporization to remove is removed to gas phase further, and the still raffinate that tower reactor interval is discharged is not containing trichlorosilane.Reboiler 2 provides stripping stage 3 gas phase 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 DEG C; Operating reflux ratio is 1.0-3.0; Dichlorosilane and silicon tetrachloride mol ratio are 1-1:1.2.
Chemical reaction involved in the present invention is mainly:
Production technology principle of the present invention and process are: the dichlorosilane raw material sent here by a upper workshop section, enters in tower between stripping conversion zone 4 and absorption reaction section 5; Because in tower, temperature is higher, enter the dichlorosilane generating portion vaporization at once in tower, the dichlorosilane of vaporization directly enters absorption reaction section 5, and another raw material silicon tetrachloride then enters in tower between absorption reaction section 5 and rectifying section 6; Because its boiling point is higher, can directly enter reactive absorption section 5, the dichlorosilane DCS in gas phase is absorbed as absorption agent, react with catalyst exposure in the liquid phase and generate trichlorosilane, under the effect of differential reactive distillation equipment, realize the synthesis of trichlorosilane, and by the middle of trichlorosilane and reactants separate to gas phase; The gas phase being rich in trichlorosilane obtained from absorption reaction section 5 finally enters rectifying section 6; Enter the gas phase of rectifying section, under the tower top liquid-phase reflux effect that condenser 7 provides, realize trichlorosilane) purification, namely obtain the higher trichlorosilane products of concentration at tower top.
Do not have vaporize dichlorosilane then directly under enter stripping conversion zone 4, the silicon tetrachloride that it can rise in gas with stripping stage 3 reacts, and due to this section of temperature higher, the trichlorosilane be obtained by reacting can be vaporized together with dichlorosilane, and transfer in the middle of gas phase, realize being separated of trichlorosilane and silicon tetrachloride, thus improve transformation efficiency.In addition, under the effect of the upflowing vapor that tower lower stripping section 3 provides at tower bottom reboiler 2, the trichlorosilane removed of stripping conversion zone can not being vaporized is removed to gas phase further, last tower reactor obtains the still liquid not containing trichlorosilane and dichlorosilane, and the still raffinate interval being rich in silicon tetrachloride and impurity is discharged outside coupled.
Below specific embodiments of the invention.Described embodiment is only for specifically describing the present invention, instead of the claim of restriction the application.
Embodiment 1
The molar ratio of dichlorosilane (DCS) and silicon tetrachloride (STC): 1:1.2;
Catalytic rectifying column working pressure: 0.15MPa;
Service temperature: 10-85 DEG C;
Tower structure pattern is from top to bottom: 3m High Efficient Standard Packing (rectifying section)+20 layers of differential catalytic rectifying column plate (absorption reaction section)+10 layers of differential catalytic rectifying column plate (stripping conversion zone)+3m High Efficient Standard Packing (stripping stage);
Tower top composition (m%): trichlorosilane (TCS): 80%, dichlorosilane (DCS): 0.5%, silicon tetrachloride (STC): 19.5%;
(m%) is formed: trichlorosilane (TCS): 0.0%, dichlorosilane (DCS): 0.0%, silicon tetrachloride (STC): 98%, other 2% at the bottom of tower.
Embodiment 2
Dichlorosilane (DCS) and silicon tetrachloride (STC) molar ratio: 1:1.05;
Catalytic rectifying column working pressure: 0.2MPa;
Service temperature: 50-105 DEG C;
Tower structure pattern is from top to bottom: 10 layers of column plate (rectifying section)+35 layers of differential catalytic rectifying column plate (absorption reaction section)+10 layers of differential catalytic rectifying column plate (stripping conversion zone)+15 layers of column plate (stripping stage);
Tower top composition (m%): trichlorosilane (TCS): 97.5%, dichlorosilane (DCS): 0.5%, silicon tetrachloride (STC): 2%;
(m%) is formed: trichlorosilane (TCS): 0.0%, dichlorosilane (DCS): 0.0%, silicon tetrachloride (STC): 98% at the bottom of tower, other: 2%.
Embodiment 3
Dichlorosilane (DCS) and silicon tetrachloride (STC) molar ratio: 1:1;
Catalytic rectifying column working pressure: 0.4MPa;
Service temperature: 60-115 DEG C;
Tower structure pattern is from top to bottom: 10 layers of column plate (rectifying section)+35 layers of differential catalytic rectifying column plate (absorption reaction section)+10 layers of differential catalytic rectifying column plate (stripping conversion zone)+15 layers of column plate (stripping stage);
Tower top composition (m%): trichlorosilane (TCS): 97.0%, dichlorosilane (DCS): 1.0%, silicon tetrachloride (STC): 2%;
(m%) is formed: trichlorosilane (TCS): 0.0%, dichlorosilane (DCS): 0.0%, silicon tetrachloride (STC): 98% at the bottom of tower, other: 2%.
Claims (3)
1. a preparation method for trichlorosilane, this preparation method adopts following equipment and process:
This production unit is formed primarily of coupled, reboiler and condenser, and described coupled is made up of stripping stage, stripping conversion zone, absorption reaction section and rectifying section; In stripping conversion zone and absorption reaction section, install differential catalytic rectifying column plate, install column internals in stripping stage and rectifying section, column internals is column plate or filler;
Trichlorosilane preparation technology is: raw material dichlorosilane enters in tower between stripping conversion zone and absorption reaction section, and raw material silicon tetrachloride enters in tower between absorption reaction section and rectifying section; The dichlorosilane entered in tower will generating portion be vaporized at once, the silicon tetrachloride that the dichlorosilane of not vaporizing enters stripping conversion zone and stripping stage rising downwards reacts, because temperature is higher, the trichlorosilane be obtained by reacting can be vaporized together with dichlorosilane, realize being separated of trichlorosilane and silicon tetrachloride, thus improve transformation efficiency; Vaporization dichlorosilane directly enters absorption reaction section, owing to there is no catalyzer in the middle of gas phase, so the dichlorosilane in gas phase must be absorbed in liquid phase and could react, the silicon tetrachloride entering absorption reaction section from top just plays the effect of absorption agent, dichlorosilane in the middle of gas phase is absorbed in silicon tetrachloride, under the effect of differential reaction and rectification device, realize the synthesis of trichlorosilane, and by the middle of trichlorosilane and reactants separate to gas phase, the gas phase being rich in trichlorosilane obtained from absorption reaction section finally enters rectifying section; 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 lower stripping section is that the trichlorosilane removed of not vaporized by stripping conversion zone is removed to gas phase further, and the still raffinate that tower reactor interval is discharged is not containing trichlorosilane; Reboiler provides stripping stage gas phase to reflux, and condenser provides the liquid-phase reflux of rectifying section;
The condition of preparation method is: working pressure 0.1-0.4MPa; Service temperature is 10-130 DEG C; Operating reflux ratio is 1.0-3.0; Dichlorosilane and silicon tetrachloride mol ratio are 1-1:1.2;
This preparation method adopt tower structure pattern from top to bottom: 3m High Efficient Standard Packing+20 layers of differential catalytic rectifying column plate+10 layers of differential catalytic rectifying column plate+3m High Efficient Standard Packing;
Tower top composition m%: trichlorosilane 80%, dichlorosilane 0.5%, silicon tetrachloride 19.5%;
M% is formed: silicon tetrachloride 98%, other 2% at the bottom of tower.
2. a preparation method for trichlorosilane, this preparation method adopts following equipment and process:
This production unit is formed primarily of coupled, reboiler and condenser, and described coupled is made up of stripping stage, stripping conversion zone, absorption reaction section and rectifying section; In stripping conversion zone and absorption reaction section, install differential catalytic rectifying column plate, install column internals in stripping stage and rectifying section, column internals is column plate or filler;
Trichlorosilane preparation technology is: raw material dichlorosilane enters in tower between stripping conversion zone and absorption reaction section, and raw material silicon tetrachloride enters in tower between absorption reaction section and rectifying section; The dichlorosilane entered in tower will generating portion be vaporized at once, the silicon tetrachloride that the dichlorosilane of not vaporizing enters stripping conversion zone and stripping stage rising downwards reacts, because temperature is higher, the trichlorosilane be obtained by reacting can be vaporized together with dichlorosilane, realize being separated of trichlorosilane and silicon tetrachloride, thus improve transformation efficiency; Vaporization dichlorosilane directly enters absorption reaction section, owing to there is no catalyzer in the middle of gas phase, so the dichlorosilane in gas phase must be absorbed in liquid phase and could react, the silicon tetrachloride entering absorption reaction section from top just plays the effect of absorption agent, dichlorosilane in the middle of gas phase is absorbed in silicon tetrachloride, under the effect of differential reaction and rectification device, realize the synthesis of trichlorosilane, and by the middle of trichlorosilane and reactants separate to gas phase, the gas phase being rich in trichlorosilane obtained from absorption reaction section finally enters rectifying section; 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 lower stripping section is that the trichlorosilane removed of not vaporized by stripping conversion zone is removed to gas phase further, and the still raffinate that tower reactor interval is discharged is not containing trichlorosilane; Reboiler provides stripping stage gas phase to reflux, and condenser provides the liquid-phase reflux of rectifying section;
The condition of preparation method is: working pressure 0.1-0.4MPa; Service temperature is 10-130 DEG C; Operating reflux ratio is 1.0-3.0; Dichlorosilane and silicon tetrachloride mol ratio are 1-1:1.2;
This preparation method adopt tower structure pattern from top to bottom: 10 layers of column plate+35 layers of differential catalytic rectifying column plate+10 layers of differential catalytic rectifying column plate+15 layers of column plate;
Tower top composition m%: trichlorosilane 97.5%, dichlorosilane 0.5%, silicon tetrachloride 2%;
M% is formed: silicon tetrachloride 98%, other 2% at the bottom of tower.
3. a preparation method for trichlorosilane, this preparation method adopts following equipment and process:
This production unit is formed primarily of coupled, reboiler and condenser, and described coupled is made up of stripping stage, stripping conversion zone, absorption reaction section and rectifying section; In stripping conversion zone and absorption reaction section, install differential catalytic rectifying column plate, install column internals in stripping stage and rectifying section, column internals is column plate or filler;
Trichlorosilane preparation technology is: raw material dichlorosilane enters in tower between stripping conversion zone and absorption reaction section, and raw material silicon tetrachloride enters in tower between absorption reaction section and rectifying section; The dichlorosilane entered in tower will generating portion be vaporized at once, the silicon tetrachloride that the dichlorosilane of not vaporizing enters stripping conversion zone and stripping stage rising downwards reacts, because temperature is higher, the trichlorosilane be obtained by reacting can be vaporized together with dichlorosilane, realize being separated of trichlorosilane and silicon tetrachloride, thus improve transformation efficiency; Vaporization dichlorosilane directly enters absorption reaction section, owing to there is no catalyzer in the middle of gas phase, so the dichlorosilane in gas phase must be absorbed in liquid phase and could react, the silicon tetrachloride entering absorption reaction section from top just plays the effect of absorption agent, dichlorosilane in the middle of gas phase is absorbed in silicon tetrachloride, under the effect of differential reaction and rectification device, realize the synthesis of trichlorosilane, and by the middle of trichlorosilane and reactants separate to gas phase, the gas phase being rich in trichlorosilane obtained from absorption reaction section finally enters rectifying section; 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 lower stripping section is that the trichlorosilane removed of not vaporized by stripping conversion zone is removed to gas phase further, and the still raffinate that tower reactor interval is discharged is not containing trichlorosilane; Reboiler provides stripping stage gas phase to reflux, and condenser provides the liquid-phase reflux of rectifying section;
The condition of preparation method is: working pressure 0.1-0.4MPa; Service temperature is 10-130 DEG C; Operating reflux ratio is 1.0-3.0; Dichlorosilane and silicon tetrachloride mol ratio are 1-1:1.2;
This preparation method adopt tower structure pattern from top to bottom: 10 layers of column plate+35 layers of differential catalytic rectifying column plate+10 layers of differential catalytic rectifying column plate+15 layers of column plate;
Tower top composition m%: trichlorosilane 97.0%, dichlorosilane 1.0%, silicon tetrachloride 2%;
M% is formed: silicon tetrachloride 98%, other 2% at the bottom of tower.
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| CN103553057B (en) * | 2013-11-11 | 2016-01-20 | 新特能源股份有限公司 | A kind of method utilizing reaction rectification technique process chlorosilane waste gas |
| 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 |
| CN105948059B (en) * | 2016-05-03 | 2018-05-08 | 宜昌南玻硅材料有限公司 | Recycle the system and method for 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 |
| 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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| CN102068829A (en) * | 2010-11-24 | 2011-05-25 | 天津大学 | Baffle reaction-rectification equipment and anti-disproportionation reaction between dichlorosilane and silicon tetrachloride |
| WO2012013123A1 (en) * | 2010-07-29 | 2012-02-02 | Byd Company Limited | Process and system for preparing silane from trichlorosilane |
| CN102516036A (en) * | 2011-12-14 | 2012-06-27 | 河北工业大学 | Process method for preparing methyl tert-butyl ether by differential reaction rectification and equipment for same |
| CN103086380A (en) * | 2013-01-21 | 2013-05-08 | 天津大学 | Method and device for treating dichlorosilane waste by utilizing reactive distillation |
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| US20100150809A1 (en) * | 2008-12-11 | 2010-06-17 | Bill Jr Jon M | enhancements for a chlorosilane redistribution reactor |
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| WO2012013123A1 (en) * | 2010-07-29 | 2012-02-02 | Byd Company Limited | Process and system for preparing silane from trichlorosilane |
| CN102068829A (en) * | 2010-11-24 | 2011-05-25 | 天津大学 | Baffle reaction-rectification equipment and anti-disproportionation reaction between dichlorosilane and silicon tetrachloride |
| CN102516036A (en) * | 2011-12-14 | 2012-06-27 | 河北工业大学 | Process method for preparing methyl tert-butyl ether by differential reaction rectification and equipment for same |
| CN103086380A (en) * | 2013-01-21 | 2013-05-08 | 天津大学 | Method and device for treating dichlorosilane waste by utilizing reactive distillation |
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