CN103482573B - 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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- CN103482573B CN103482573B CN201310443666.XA CN201310443666A CN103482573B CN 103482573 B CN103482573 B CN 103482573B CN 201310443666 A CN201310443666 A CN 201310443666A CN 103482573 B CN103482573 B CN 103482573B
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- chloride gas
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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 one and be applicable to hydrogen chloride gas drying means and device in production of polysilicon.
Background technology
In polycrystalline silicon device, trichlorosilane synthesis procedure is reacted in a fluidized bed reactor at silica flour and hydrogen chloride gas, produces trichlorosilane.Trichlorosilane synthesizer has strict requirement to as moisture contained in the hydrogen chloride gas of raw material, general requirement is lower than 50ppm, it is use vitriol oil dehydration, the characteristic dry hydrogen chloride gas absorbed water by the vitriol oil that the method for current hydrogenchloride drying mainly contains three kinds: one; Two is use molecular sieve drying hydrogen chloride gas.Three is use liquid chlorosilane to spray hydrogen chloride gas, makes the moisture generation hydrolysis reaction in chlorosilane and hydrogenchloride, reaches the object of hydrogen chloride gas drying; Adopt the vitriol oil to dewater the hydrogenchloride water content that obtains at about 60ppm, but dried hydrogenchloride can take a small amount of sulfuric acid impurity out of, is unfavorable for that trichlorosilane synthesizes.The hydrogenchloride water-content after molecular sieve drying is adopted to reach below 20ppm, and inclusion-free, but equipment investment and running cost are too high.Use the method for chlorosilane dry hydrogen chloride, to cause in chlorosilane with the superfine silicon-dioxide produced after hydrolysis reaction, cannot process; In addition, containing a small amount of silica dioxide granule and part chlorosilane gas in dried hydrogen chloride gas, affect the quality of hydrogen chloride gas, the transformation efficiency causing trichlorosilane to synthesize reduces.Based on the method for chlorosilane dry hydrogen chloride, Chinese patent CN102249244A improves it, name is called the hydrogenchloride dehydration and purification method being applicable to trichlorosilane synthesis, dewatering process comprises vaporizes to silicon tetrachloride, silicon tetrachloride after vaporization and hydrogenchloride mix and filter in silicon-dioxide separator, again mixed gas is carried out companion's 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 the reaction of moisture in hydrogen chloride gas, cause in the hydrogenchloride entering trichlorosilane synthetic furnace containing fine silica, and can a large amount of chlorosilane be brought into trichlorosilane synthetic furnace while dry hydrogen chloride, can suppress the carrying out of building-up reactions, Synthesis conversion reduces.Therefore, find a kind of novel hydrogenchloride drying means and have important meaning for the production of trichlorosilane synthesizer and polysilicon.
Summary of the invention
For the defect of 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 chlorosilane dry method reduces hydrogen chloride gas body water content, and its step comprises:
1) chlorosilane is passed into well heater to vaporize;
2) chlorosilane steam is fully mixed in a mixer with hydrogen chloride gas;
3) mixed gas passes into retort, by hydrolysis reaction dry hydrogen chloride gas, generates fine silica simultaneously;
4) hydrogen chloride gas containing fine silica sends into fly-ash separator, and removing fine silica, obtains dry hydrogen chloride gas.
Well heater is sheathed heater, and gas mixer is venturi mixer, and retort is traverse baffle retort, and fly-ash separator is sack cleaner.
Chlorosilane in sheathed heater 90 DEG C vaporize.
The working pressure of each device is 0.1-0.3Mpa.
Detailed operation process is as follows:
1. the hydrogen chloride gas water-content before drying is detected, calculate the moisture content in hydrogen chloride gas;
2. according to water-content situation in hydrogenchloride, flow hydrolysis reaction occurring and needs chlorosilane is calculated;
3. appropriate chlorosilane is passed into sheathed heater to vaporize;
4. chlorosilane steam is mixed at mixing tank with hydrogen chloride gas;
5. mixed gas is passed into retort, by hydrolysis reaction dry hydrogen chloride gas;
6. the hydrogen chloride gas containing silica dust sends into sack cleaner, is removed by dust-filtering, obtains dry hydrogen chloride gas.
The present invention is that hydrogen chloride gas mixes in Venturi-type mixing tank with chlorosilane steam, enters reactor and fully reacts, and filters the silica dust in hydrogen chloride gas finally by high effect dust cleaner, obtains clean dry hydrogen chloride gas.In addition, first the present invention measures water content in hydrogenchloride, according to water content situation in hydrogenchloride, and the processing compound of adjustment chlorosilane and moisture, effectively can 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, mixes chlorosilane steam with hydrogen chloride gas, the moisture content in hydrogen chloride gas and chlorosilane generation hydrolysis reaction, reaches the object reducing water content in hydrogenchloride.
First, determine the flow needing dry hydrogen chloride gas, detect hydrogen chloride gas water-content, calculate hydrogen chloride gas total Water, according to hydrolysis equation:
SiCl
4 + 2H
2O→ SiO
2+ 4HCl
In hydrogenchloride, the mol ratio of total Water and chlorosilane is 1: 0.5 ~ 3, the water-content in hydrogenchloride can be reduced to 10 ~ 50ppm by hydrolysis reaction.
The present invention also comprises a kind of hydrogenchloride drying installation being applicable to polysilicon enterprise, comprising:
1, jacketed type well heater, by the steam heating of outer chuck, is vaporizated into chlorosilane steam by the liquid chlorosilane of internal layer.
2, gas mixer, adopts venturi principle, hydrogen chloride gas and chlorosilane steam is passed into gas mixer, fully mixes;
3, reactor, is connected with gas mixer by pipeline, and mixing tank gas enters reactor and to be hydrolyzed reaction, inside reactor has traverse baffle, effectively can extend the reaction times of mixed gas, ensure that moisture in hydrogen chloride gas is fully hydrolyzed, reach the object of dry hydrogen chloride gas.
4, deep bed filter, be connected with reactor by pipeline, the product of hydrolysis reaction is carried out gas solid separation, dry hydrogenchloride is thoroughly separated through filter bag with solid silica powder, then by the blowback of high pressure chlorination hydrogen, powder on filter bag is blown to filter bottom broach hopper, is discharged by slag-drip opening.
Above technical scheme mainly hydrogen chloride gas mixes in venturi mixer with chlorosilane steam, then enter in traverse baffle retort and fully react, filter the fine silica in hydrogen chloride gas finally by high effect dust cleaner, obtain clean clean hydrogen chloride gas.In addition, by the mensuration of water content in hydrogenchloride, the processing compound of adjustment silicon tetrachloride and moisture, the content of silicon tetrachloride effectively in the dried hydrogenchloride of control, avoids that silicon tetrachloride is excessive affects trichlorosilane transformation efficiency.
It is simple that the present invention has technique, and equipment composition is few, and processing ease, dried hydrogenchloride water content can drop to 10-50ppm.
Accompanying drawing explanation
Fig. 1 is a kind of process flow sheet being 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 the jacketed type well heater 2, gas mixer 1, reactor 3, the deep bed filter 4 that connect successively.
The character that the present invention utilizes chlorosilane very easily to react with water, mixes chlorosilane steam with hydrogen chloride gas, the moisture content in hydrogen chloride gas and chlorosilane generation hydrolysis reaction, reaches the object reducing water content in hydrogenchloride.
First, determine the flow needing dry hydrogen chloride gas, detect hydrogen chloride gas water-content, calculate hydrogen chloride gas total Water, according to hydrolysis equation:
SiCl
4 + 2H
2O→ SiO
2+ 4HCl
The mol ratio calculating 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 by heat vaporized to 90 DEG C, mix with hydrogen chloride gas at gas mixer 1, then mixed gas enters reactor 3, moisture in chlorosilane and hydrogen chloride gas is hydrolyzed and reacts, and product is dry hydrogen chloride gas and solid silica powder.Fraction solids SiO 2 powder is settled down to bottom reactor 3, by the taper slag-drip opening bottom reactor 3, solid silica is discharged, 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 filter bag surface, after 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 drop to the broach hopper of deep bed filter, by bottom residual cake valve discharger.The gas transferred out from deep bed filter top is dry hydrogen chloride gas, can meet the service requirements of trichlorosilane synthesis.Hydrogen chloride gas drying device working pressure controls at 0.1 ~ 0.3MPa, can be reduced to 10 ~ 50ppm through super-dry post chlorization hydrogen water-content.
The present invention is that hydrogen chloride gas mixes in Venturi-type mixing tank with chlorosilane steam, enter reactor fully to react, the silica dust in hydrogen chloride gas is filtered finally by high effect dust cleaner, finally obtain clean dry hydrogen chloride gas, the present invention can effectively avoid not exclusively causing in dry hydrogenchloride containing chlorosilane and SiO 2 powder owing to reacting, thus cause hydrogenchloride Quality Down, affect lower procedure and use.In addition, first the present invention measures water content in hydrogenchloride, according to water content situation in hydrogenchloride, and the processing compound of adjustment chlorosilane and moisture, effectively can control the content of silicon tetrachloride in dried hydrogenchloride, avoid the excessive situation causing 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, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. hydrogen chloride gas drying means and a device in production of polysilicon, is characterized by drying means as follows:
1) chlorosilane is passed into well heater to vaporize;
2) chlorosilane steam is fully mixed in a mixer with hydrogen chloride gas;
3) mixed gas passes into retort, by hydrolysis reaction dry hydrogen chloride gas, generates fine silica simultaneously;
4) hydrogen chloride gas containing fine silica sends into fly-ash separator, and removing fine silica, obtains dry hydrogen chloride gas,
Wherein, in described step 1), chlorosilane in sheathed heater 90 DEG C vaporize.
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 traverse baffle retort, and fly-ash separator is sack cleaner.
3. 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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| 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 |
| CN109368593B (en) * | 2018-11-26 | 2020-04-10 | 浙江博瑞电子科技有限公司 | Method for preparing electronic grade hydrogen chloride gas containing ppbv grade 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 |
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| 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 |
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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 |