CN103482573A - Method and device for drying hydrogen chloride gas in polysilicon production - Google Patents
Method and device for drying hydrogen chloride gas in polysilicon production Download PDFInfo
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- CN103482573A CN103482573A CN201310443666.XA CN201310443666A CN103482573A CN 103482573 A CN103482573 A CN 103482573A CN 201310443666 A CN201310443666 A CN 201310443666A CN 103482573 A CN103482573 A CN 103482573A
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- hydrogen chloride
- chloride gas
- chlorosilane
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Abstract
The invention relates to the field of material processing in polysilicon production. As for drying of a material hydrogen chloride, a process scheme which is ideal in performance and cost has not been found. A method provided by the invention is further improved on the basis of a method for drying hydrogen chloride by using chlorosilane, and adopts the process flow as follows: firstly, mixing hydrogen chloride gas with chlorosilane vapor in a venturi mixer; secondly, entering a baffled reaction tank, and sufficiently reacting; and finally, filtering out silicon dioxide fine powder in the hydrogen chloride through an efficient dust-removing device to obtain clean and dry hydrogen chloride gas. The method has the advantages of simple process, few equipment composition and easiness operation; and the water content of the dried hydrogen chloride can be reduced to 10-50ppm.
Description
Technical field
The present invention relates to a kind of be applicable to hydrogen chloride gas drying means and device in production of polysilicon.
Background technology
In polycrystalline silicon device, the trichlorosilane synthesis procedure is that silica flour is reacted in fluidized-bed reactor with hydrogen chloride gas, produces trichlorosilane.Trichlorosilane synthesizer has strict requirement to moisture contained in the hydrogen chloride gas as raw material, general requirement is lower than 50ppm, the method of hydrogenchloride drying mainly contains three kinds at present: the one, use vitriol oil dehydration, the characteristic dry hydrogen chloride gas absorbed water by the vitriol oil; The 2nd, use the molecular sieve drying hydrogen chloride gas.The 3rd, use liquid chlorosilane to be sprayed hydrogen chloride gas, make the moisture generation hydrolysis reaction in chlorosilane and hydrogenchloride, reach the purpose of hydrogen chloride gas drying; The hydrogenchloride water content that adopts vitriol oil dehydration to obtain is in the 60ppm left and right, but dried hydrogenchloride can be taken a small amount of sulfuric acid impurity out of, is unfavorable for that trichlorosilane is synthetic.Hydrogenchloride water-content after the employing molecular sieve drying can reach below 20ppm, and inclusion-free, but equipment investment and running cost are too high.Use the method for chlorosilane dry hydrogen chloride, can cause in chlorosilane with the superfine silicon-dioxide produced after hydrolysis reaction, can't process; In addition, contain a small amount of silica dioxide granule and part chlorosilane gas in dried hydrogen chloride gas, affect the quality of hydrogen chloride gas, cause the synthetic transformation efficiency of trichlorosilane to reduce.Method based on the chlorosilane dry hydrogen chloride, Chinese patent CN102249244A improves it, name is called the synthetic hydrogenchloride dehydration and purification method of trichlorosilane that is applicable to, dewatering process comprises is vaporized to silicon tetrachloride, silicon tetrachloride after vaporization and hydrogenchloride mix and filter in the silicon-dioxide separator, again mixed gas is accompanied to heat, enter into trichlorosilane synthetic furnace, hydrogenchloride is dewatered.There is following defect in this patent: chlorosilane gas just simply mixes with hydrogenchloride, abundant not, hydrolysis time is short, chlorosilane easily after filtration with hydrogen chloride gas in reaction of moisture, cause in the hydrogenchloride that enters trichlorosilane synthetic furnace and contain fine silica, and can bring a large amount of chlorosilanes into trichlorosilane synthetic furnace when dry hydrogen chloride, and can suppress the carrying out of building-up reactions, Synthesis conversion reduces.Therefore, find a kind of novel hydrogenchloride drying means, for the production of trichlorosilane synthesizer and polysilicon, important meaning is arranged.
Summary of the invention
Defect for existing hydrogen chloride gas dry technology, the invention provides a kind of new hydrogen chloride gas dry technology and device.
The technical solution adopted in the present invention is that the chlorosilane dry method reduces the hydrogen chloride gas body water content, and its step comprises:
1) chlorosilane being passed into to well heater is vaporized;
2) chlorosilane steam is fully mixed in mixing tank with hydrogen chloride gas;
3) mixed gas passes into retort, by the hydrolysis reaction dry hydrogen chloride gas, generates fine silica simultaneously;
4) hydrogen chloride gas that contains fine silica is sent into fly-ash separator, removes fine silica, obtains dry hydrogen chloride gas.
Well heater is sheathed heater, and gas mixer is venturi mixer, and retort is the traverse baffle retort, and fly-ash separator is sack cleaner.
Chlorosilane in sheathed heater 90 ℃ vaporized.
The working pressure of each device is 0.1-0.3Mpa.
Operating process is as follows in detail:
1. the hydrogen chloride gas water-content before dry is detected, calculated the moisture content in hydrogen chloride gas;
2. according to water-content situation in hydrogenchloride, calculate the flow that hydrolysis reaction needs chlorosilane occurs;
3. appropriate chlorosilane being passed into to sheathed heater is vaporized;
4. chlorosilane steam is mixed at mixing tank with hydrogen chloride gas;
5. mixed gas is passed into to retort, by the hydrolysis reaction dry hydrogen chloride gas;
6. the hydrogen chloride gas that contains silica dust is sent into sack cleaner, and dust-filtering is removed, and obtains dry hydrogen chloride gas.
The present invention is that hydrogen chloride gas is mixed in the Venturi-type mixing tank with chlorosilane steam, enters reactor and fully reacts, and finally by high effect dust cleaner, filters the silica dust in hydrogen chloride gas, obtains clean dry hydrogen chloride gas.In addition, at first the present invention measures water content in hydrogenchloride, according to water content situation in hydrogenchloride, adjusts the processing compound of chlorosilane and moisture, can effectively control the content of chlorosilane in dried hydrogenchloride, avoid the excessive trichlorosilane transformation efficiency that causes of chlorosilane in hydrogenchloride to reduce.
The character that the present invention utilizes chlorosilane very easily to react with water, mix chlorosilane steam with hydrogen chloride gas, the moisture content in hydrogen chloride gas and chlorosilane generation hydrolysis reaction reach the purpose that reduces water content in hydrogenchloride.
At first, determine the flow that needs dry hydrogen chloride gas, detect the hydrogen chloride gas water-content, calculate the hydrogen chloride gas total Water, according to being hydrolyzed equation:
SiCl
4?+?2H
2O→?SiO
2?+?4HCl
In hydrogenchloride, the mol ratio of total Water and chlorosilane is 1: 0.5～3, can be by the reduced water content to 10 in hydrogenchloride～50ppm by hydrolysis reaction.
The present invention also comprises a kind of hydrogenchloride drying installation that is applicable to polysilicon enterprise, comprising:
1, jacketed type well heater, by the steam heating of outer chuck, be vaporizated into chlorosilane steam by the liquid chlorosilane of internal layer.
2, gas mixer, adopt venturi principle, and hydrogen chloride gas and chlorosilane steam are passed into to gas mixer, fully mixes;
3, reactor, be connected with gas mixer by pipeline, and mixing tank gas enters the reactor reaction that is hydrolyzed, inside reactor has traverse baffle, can effectively extend the reaction times of mixed gas, guarantee that moisture in hydrogen chloride gas fully is hydrolyzed, reach the purpose of dry hydrogen chloride gas.
4, deep bed filter, by pipeline, with reactor, be connected, the product of hydrolysis reaction is carried out to gas solid separation, dry hydrogenchloride is thoroughly separated through filter bag with the solid silica powder, then by the blowback of high pressure chlorination hydrogen, powder on filter bag is blown to the filter bottom broach hopper, discharge by slag-drip opening.
Above technical scheme is mainly that hydrogen chloride gas is mixed in venturi mixer with chlorosilane steam, then enter in the traverse baffle retort and fully react, finally by high effect dust cleaner, filter the fine silica in hydrogen chloride gas, obtain clean clean hydrogen chloride gas.In addition, by the mensuration of water content in hydrogenchloride, adjust the processing compound of silicon tetrachloride and moisture, effectively control the content of silicon tetrachloride in dried hydrogenchloride, avoided the excessive trichlorosilane transformation efficiency that affects of silicon tetrachloride.
It is simple that the present invention has technique, and equipment forms few, processing ease, and dried hydrogenchloride water content can drop to 10-50ppm.
The accompanying drawing explanation
Fig. 1 is a kind of process flow sheet that is applicable to the hydrogen chloride gas drying means of polysilicon enterprise of the present invention
In figure: 1-gas mixer 2-jacketed type well heater 3-reactor 4-deep bed filter.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further detailed explanation.
As shown in Figure 1, hydrogen chloride gas drying device of the present invention comprises jacketed type well heater 2, gas mixer 1, reactor 3, the deep bed filter 4 connected successively.
The character that the present invention utilizes chlorosilane very easily to react with water, mix chlorosilane steam with hydrogen chloride gas, the moisture content in hydrogen chloride gas and chlorosilane generation hydrolysis reaction reach the purpose that reduces water content in hydrogenchloride.
At first, determine the flow that needs dry hydrogen chloride gas, detect the hydrogen chloride gas water-content, calculate the hydrogen chloride gas total Water, according to being hydrolyzed equation:
SiCl
4?+?2H
2O→?SiO
2?+?4HCl
Calculating the mol ratio of total Water and chlorosilane in hydrogenchloride is 1: 0.5～3;
According to processing compound, chlorosilane is delivered to jacketed type well heater 2, chlorosilane is heated vaporization to 90 ℃, at gas mixer 1, with hydrogen chloride gas, mix, then mixed gas enters reactor 3, chlorosilane is hydrolyzed and reacts with moisture in hydrogen chloride gas, and product is dry hydrogen chloride gas and solid silica powder.Part solid silica powder is settled down to reactor 3 bottoms, taper slag-drip opening by reactor 3 bottoms is discharged solid silica, another part SiO 2 powder is followed hydrogen chloride gas and is entered deep bed filter 4, utilize deep bed filter 4 that remaining SiO 2 powder is filled into to the filter bag surface, after the deep bed filter inlet outlet pressure differential increases, by using the blowback of high pressure chlorination hydrogen, the SiO 2 powder on cloth bag surface is blown down, powder is deposited to the broach hopper of deep bed filter, by bottom residual cake valve discharger.The gas transferred out from the deep bed filter top is dry hydrogen chloride gas, can meet the synthetic service requirements of trichlorosilane.The hydrogen chloride gas drying device working pressure is controlled at 0.1～0.3MPa, through super-dry post chlorization hydrogen water-content, can be reduced to 10～50ppm.
The present invention is that hydrogen chloride gas is mixed in the Venturi-type mixing tank with chlorosilane steam, entering reactor fully reacts, finally by high effect dust cleaner, filter the silica dust in hydrogen chloride gas, finally obtain clean dry hydrogen chloride gas, the present invention can effectively avoid containing chlorosilane and SiO 2 powder because reaction not exclusively causes in dry hydrogenchloride, thereby cause the hydrogenchloride Quality Down, affect lower procedure and use.In addition, at first the present invention measures water content in hydrogenchloride, according to water content situation in hydrogenchloride, adjusts the processing compound of chlorosilane and moisture, can effectively control the content of silicon tetrachloride in dried hydrogenchloride, avoid the excessive situation that causes the trichlorosilane transformation efficiency to reduce of chlorosilane.
The present invention is not limited to above-mentioned preferred forms, and anyone can draw other various forms of technical schemes under enlightenment of the present invention.For a person skilled in the art, its technical scheme that still can put down in writing aforementioned each embodiment is modified, or part technical characterictic wherein is equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. hydrogen chloride gas drying means and device in a production of polysilicon is characterized by drying means as follows:
(1) chlorosilane being passed into to well heater is vaporized;
(2) chlorosilane steam is fully mixed in mixing tank with hydrogen chloride gas;
(3) mixed gas passes into retort, by the hydrolysis reaction dry hydrogen chloride gas, generates fine silica simultaneously;
(4) hydrogen chloride gas that contains fine silica is sent into fly-ash separator, removes fine silica, obtains dry hydrogen chloride gas.
2. hydrogen chloride gas drying means and device in production of polysilicon according to claim 1, it is characterized by well heater is sheathed heater, and gas mixer is venturi mixer, and retort is the traverse baffle retort, and fly-ash separator is sack cleaner.
3. according to hydrogen chloride gas drying means and device in the described production of polysilicon of right 1 or 2, it is characterized by chlorosilane in sheathed heater 90 ℃ vaporized.
4. hydrogen chloride gas drying means and device in production of polysilicon according to claim 1 and 2, the working pressure that it is characterized by each device is 0.1-0.3Mpa.
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| CN201310443666.XA CN103482573B (en) | 2013-09-26 | 2013-09-26 | Method and device for drying hydrogen chloride gas in polysilicon production |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629604A (en) * | 2016-11-28 | 2017-05-10 | 昆明理工大学 | Method for preparing gas-phase hydrogen chloride by utilizing chlorosilane residue |
| CN109368593A (en) * | 2018-11-26 | 2019-02-22 | 浙江博瑞电子科技有限公司 | A method of preparing the electronic grade hydrogen chloride gas of ppbv grades of moisture impurities |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249244A (en) * | 2011-06-15 | 2011-11-23 | 四川瑞能硅材料有限公司 | HCl dehydration and purification method suitable for synthesis of trichlorosilane |
| CN102417163A (en) * | 2011-07-28 | 2012-04-18 | 四川瑞能硅材料有限公司 | Improved Siemens method-HCL gas dehydration purifying method |
-
2013
- 2013-09-26 CN CN201310443666.XA patent/CN103482573B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249244A (en) * | 2011-06-15 | 2011-11-23 | 四川瑞能硅材料有限公司 | HCl dehydration and purification method suitable for synthesis of trichlorosilane |
| CN102417163A (en) * | 2011-07-28 | 2012-04-18 | 四川瑞能硅材料有限公司 | Improved Siemens method-HCL gas dehydration purifying method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629604A (en) * | 2016-11-28 | 2017-05-10 | 昆明理工大学 | Method for preparing gas-phase hydrogen chloride by utilizing chlorosilane residue |
| CN106629604B (en) * | 2016-11-28 | 2019-07-16 | 昆明理工大学 | A method of gas phase chlorination hydrogen is produced using chlorosilane raffinate |
| CN109368593A (en) * | 2018-11-26 | 2019-02-22 | 浙江博瑞电子科技有限公司 | A method of preparing the electronic grade hydrogen chloride gas of ppbv grades of moisture impurities |
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| CN103482573B (en) | 2015-07-22 |
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Application publication date: 20140101 Assignee: Inner Mongolia Xinte silicon material Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2022990000326 Denomination of invention: A method and device for drying hydrogen chloride gas in polysilicon production Granted publication date: 20150722 License type: Common License Record date: 20220627 Application publication date: 20140101 Assignee: Xinte silicon based new materials Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2022990000325 Denomination of invention: A method and device for drying hydrogen chloride gas in polysilicon production Granted publication date: 20150722 License type: Common License Record date: 20220627 |
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