CN103193235B - Device for hydrolyzing silicon tetrachloride - Google Patents

Device for hydrolyzing silicon tetrachloride Download PDF

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Publication number
CN103193235B
CN103193235B CN201310114815.8A CN201310114815A CN103193235B CN 103193235 B CN103193235 B CN 103193235B CN 201310114815 A CN201310114815 A CN 201310114815A CN 103193235 B CN103193235 B CN 103193235B
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China
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liquid outlet
silicon tetrachloride
still liquid
reaction pot
hydrolytic reaction
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Expired - Fee Related
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CN201310114815.8A
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Chinese (zh)
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CN103193235A (en
Inventor
刘玉敏
郝丛
蒋子超
武朋涛
花秀艳
张向京
胡永其
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Hebei University of Science and Technology
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Hebei University of Science and Technology
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Abstract

The invention discloses a device for hydrolyzing silicon tetrachloride. The device comprises a flow-jet ejector (8), a hydrolysis reaction kettle (16) and two circulation systems; the flow-jet ejector (8) is communicated with a material liquid inlet (9) of the hydrolysis reaction kettle (16); the flow-jet ejector (8) is provided with an opening (6) and a silicon tetrachloride (7); a kettle liquid outlet (10a) is formed in the lower part of one side of the hydrolysis reaction kettle (16); the kettle liquid outlet (10a) is communicated with a circulating pump (3a) and an opening (6) of the flow-jet ejector (8) by a pipeline so as to form a first circulation system; the circulating pump (3a) is communicated with a water inlet pipeline; a kettle liquid outlet (10b) is formed in the lower part of the other side of the hydrolysis reaction kettle (16); the hydrolysis reaction kettle (16) is provided with a circulating liquid inlet (13); and a kettle liquid outlet (10b) is communicated with a circulating pump (3b) and the circulating liquid inlet (13) of the hydrolysis reaction kettle (16) by the pipeline so as to form the other circulation system. The device can be used for enhancing the mixing degree of the silicon tetrachloride and water so that the hydrolysis reaction is quickly and fully proceeded, the reaction time is shortened, and the production capability of each device is improved.

Description

A kind of device for hydrolyzing silicon tetrachloride
Technical field
The invention belongs to chemical field, be specifically related to a kind of device for hydrolyzing silicon tetrachloride.
Background technology
In recent years, along with information technology and the develop rapidly of solar energy industry band, the domestic demand growth to polysilicon was swift and violent.Polysilicon enterprise is a large amount of silicon tetrachloride of by-product in process of production, if silicon tetrachloride can not be utilized well, not only can make resource cause waste, and can cause serious pollution to environment.Domestic enterprise mainly adopts thermal silica generating process processing silicon chloride, and the high temperature hydrolysis furnace by silicon tetrachloride and a certain amount of hydrogen and oxygen at 1000-1200 ℃ reacts.The method is high to equipment requirements, and technical sophistication yields poorly.About utilizing hydrolyzing silicon tetrachloride device report seldom, and mainly there is following problem: 1) hydrolyzing silicon tetrachloride is a rapid reaction, and industrial mixing speed is lower, be difficult to realize uniformly and mix; 2) hydrolyzing silicon tetrachloride produces a large amount of hydrogenchloride, etching apparatus.Therefore, solve silicon tetrachloride and water and mix of crucial importance that this problem just shows.
Summary of the invention
The object of the present invention is to provide the device for hydrolyzing silicon tetrachloride of a kind of strength imparting material mixing, slowing down corrosion.
For solving above technical problem, technical scheme of the present invention is: this device comprises jet ejectors, hydrolytic reaction pot and two recycle systems; Described jet ejectors is communicated with the liquor inlet of hydrolytic reaction pot, has opening and silicon tetrachloride import on jet ejectors;
One side lower part of described hydrolytic reaction pot is provided with the first still liquid outlet; The first described still liquid outlet, by the open communication of pipeline and the first recycle pump and jet ejectors, forms first recycle system; Described the first recycle pump is communicated with suction culvert;
The opposite side bottom of described hydrolytic reaction pot is provided with the second still liquid outlet, and hydrolytic reaction pot top is provided with circulation fluid import; The second described still liquid outlet is communicated with the circulation fluid import of hydrolytic reaction pot by pipeline and the second recycle pump, forms another recycle system.
The pipeline of first recycle system of the present invention is provided with the first still liquid outlet valve and first flow meter; The pipeline of described another recycle system is provided with the second still liquid outlet valve and the second under meter.
The top of hydrolytic reaction pot of the present invention is tower reactor, and filler is inside housed, and top is provided with hydrogenchloride outlet and circulation fluid import; Bottom is tank reactor, is provided with the leakage fluid dram of liquor inlet, the first still liquid outlet, the second still liquid outlet and bottom.
The liner of hydrolytic reaction pot of the present invention is enamel material, and described the first recycle pump and the second recycle pump are all selected acid and alkali-resistance vacuum pump, and described jet ejectors is selected corrosion resistant surge pump.
The present invention in use, water enters first recycle system by the first recycle pump, utilize water to flow and cause suction to take silicon tetrachloride to jet ejectors in pipeline, mix with water, directly enter below the liquid level in hydrolytic reaction pot, still liquid exports by the first still liquid of hydrolytic reaction pot one side the import that enters the first recycle pump, completes once circulation.In hydrolytic reaction pot, still liquid also can enter another recycle system by the second still liquid outlet of hydrolytic reaction pot opposite side, thereby forms two recycle systems, strengthens the degree of mixing of silicon tetrachloride and water, accelerates the hydrolysis of silicon tetrachloride; The still liquid of another recycle system flows down from hydrolytic reaction pot top, flow to filler, the silicon tetrachloride of the vaporization producing in can absorption reaction process, and hydrogenchloride exports discharge by hydrogenchloride, the silicon-dioxide that reaction produces is discharged from the leakage fluid dram of hydrolytic reaction pot.
Adopted after technique scheme, the invention has the beneficial effects as follows: because the present invention has two recycle systems, bottom and the top of described Matter Transfer pipeline connection hydrolytic reaction pot, silicon tetrachloride joins in circulating system by jet ejectors, in described circulation line, be equipped with recycle pump, so, solution ceaselessly circulates in circulation line, strengthened the degree of mixing of silicon tetrachloride and water, hydrolysis reaction is carried out fast fully, Reaction time shorten, improves single device throughput.The liner of hydrolytic reaction pot of the present invention adopts enamel material, and hydrogenchloride can be instant from hydrogenchloride outlet, discharges, thereby has effectively reduced the corrosion of hydrogenchloride to equipment.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention's device used.
In accompanying drawing: 1-water feed valve; 2-the first still liquid outlet valve; 3a-the first recycle pump; 3b-the second recycle pump; 4-first flow meter; 5-silicon tetrachloride feeding valve; 6-opening; The import of 7-silicon tetrachloride; 8-jet ejectors; 9-liquor inlet; 10a-the first still liquid outlet; 10b-the second still liquid outlet; 11-vent valve; The outlet of 12-hydrogenchloride; The import of 13-circulation fluid; 14-shower nozzle; 15-filler; 16-hydrolytic reaction pot; 17-leakage fluid dram; 18-tapping valve; 19-the second still liquid outlet valve; 20-the second under meter.
Embodiment
Shown in Fig. 1, this device for hydrolyzing silicon tetrachloride comprises jet ejectors 8, hydrolytic reaction pot 16 and two recycle systems.Described hydrolytic reaction pot 16 adopts enamel reaction still, and its top is tower reactor, and filler 15 is inside housed, and top is provided with hydrogenchloride outlet 12 and circulation fluid import 13, and the hydrogenchloride of generation exports 12 by hydrogenchloride and discharges, and hydrogenchloride outlet 12 is provided with vent valve 11; Bottom is tank reactor, is provided with the leakage fluid dram 17 of liquor inlet 9, the first still liquid outlet 10a, the second still liquid outlet 10b and bottom; The silicon-dioxide that reaction produces is discharged from the leakage fluid dram 17 of hydrolytic reaction pot 16 bottoms, and leakage fluid dram 17 is provided with tapping valve 18.Described jet ejectors 8 is communicated with the liquor inlet 9 of hydrolytic reaction pot 16, is provided with opening 6 and silicon tetrachloride import 7 on jet ejectors 8; Described jet ejectors 8 is preferably selected corrosion resistant surge pump.Bottom and the top of the pipeline connection hydrolytic reaction pot 16 of two described recycle systems, be provided with the first recycle pump 3a and the second recycle pump 3b in described circulation line, described recycle pump is preferably selected acid and alkali-resistance vacuum pump.
Shown in Fig. 1, this device for hydrolyzing silicon tetrachloride connects the import of the first recycle pump 3a for controlling the outlet of the water feed valve 1 of water inlet, the outlet of the first recycle pump 3a connects the import of first flow meter 4, the outlet of first flow meter 4 connects the opening 6 of jet ejectors 8, silicon tetrachloride enters jet ejectors 8 by silicon tetrachloride feeding valve 5 and silicon tetrachloride import 7 to be mixed with water, by liquor inlet 9, enter below the liquid level in hydrolytic reaction pot 16, still liquid enters circulating line by being positioned at the first still liquid outlet 10a of hydrolytic reaction pot 16 1 side lower parts, be that still liquid is by being communicated with successively the first still liquid outlet 10a, the first still liquid outlet valve 2, the first recycle pump 3a, first flow meter 4, after the pipeline of the opening 6 of squirt pump, enter hydrolytic reaction pot 16 and form first recycle system.
Shown in Fig. 1, between the second still liquid outlet 10b of these hydrolytic reaction pot 16 opposite side bottoms for the device of hydrolyzing silicon tetrachloride and the second recycle pump 3b, be provided with between the second still liquid outlet valve 19, the second recycle pump 3b and circulation fluid import 13 and be provided with the second under meter 20; Like this, still liquid enters hydrolytic reaction pot 16 by shower nozzle 14 after the pipeline of the second still liquid outlet 10b, the second still liquid outlet valve 19, the second recycle pump 3b, the second under meter 20, circulation fluid import 13 and forms another recycle systems by being communicated with successively.
This hydrolysing step for the device of hydrolyzing silicon tetrachloride is: the feed valve 1 of fetching boiling water, make water enter the first recycle pump 3a, by the first recycle pump 3a and first flow meter 4, get to jet ejectors 8, silicon tetrachloride enters in jet ejectors 8 by silicon tetrachloride feeding valve 5 and silicon tetrachloride import 7, mix with water, by liquor inlet 9, enter below the liquid level in hydrolytic reaction pot 16; Open the first still liquid outlet valve 2, make still liquid flow into the first recycle pump 3a from the first still liquid outlet 10a, thereby enter first recycle system.Open the second still liquid outlet valve 19 and the second recycle pump 3b, the interior still liquid of hydrolytic reaction pot 16 flows to the second recycle pump 3b, the second under meter 20 and shower nozzle 14 from the second still liquid outlet 10b simultaneously, thereby make still liquid enter hydrolytic reaction pot 16, forms another recycle system.The silicon tetrachloride of the vaporization producing in reaction process is absorbed by filler 15, and hydrogenchloride exports 12 by hydrogenchloride and discharges; The silicon-dioxide that reaction produces is discharged from the leakage fluid dram 17 of hydrolytic reaction pot 16.
Concrete use case 1: the recycle system that 45L water is got to by the first recycle pump 3a, silicon tetrachloride 4.3L enters hydrolytic reaction pot by jet ejectors, and temperature of reaction is 40 ℃, and the reaction times is 1h, and the yield of product silicon-dioxide is 80%.
Concrete use case 2: 45L water is got to the recycle system by the first recycle pump 3a, and silicon tetrachloride 4.3L enters hydrolytic reaction pot by jet ejectors, and temperature of reaction is 45 ℃, and the reaction times is 1.5h, and the yield of product silicon-dioxide is 85%.
Concrete use case 3: 45L water is got to the recycle system by the first recycle pump 3a, and silicon tetrachloride 4.3L enters hydrolytic reaction pot by jet ejectors, and temperature of reaction is 50 ℃, and the reaction times is 2h, and the yield of product silicon-dioxide is 75%.

Claims (4)

1. for a device for hydrolyzing silicon tetrachloride, it is characterized in that:
This device comprises jet ejectors (8), hydrolytic reaction pot (16) and two recycle systems; Described jet ejectors (8) is communicated with the liquor inlet (9) of hydrolytic reaction pot (16), has opening (6) and silicon tetrachloride import (7) on jet ejectors (8);
One side lower part of described hydrolytic reaction pot (16) is provided with the first still liquid outlet (10a); The first described still liquid outlet (10a) is communicated with the opening (6) of jet ejectors (8) by pipeline and the first recycle pump (3a), forms first recycle system; Described the first recycle pump (3a) is communicated with suction culvert;
The opposite side bottom of described hydrolytic reaction pot (16) is provided with the second still liquid outlet (10b), and hydrolytic reaction pot (16) top is provided with circulation fluid import (13); The second described still liquid outlet (10b) is communicated with the circulation fluid import (13) of hydrolytic reaction pot (16) by pipeline and the second recycle pump (3b), forms another recycle system.
2. a kind of device for hydrolyzing silicon tetrachloride according to claim 1, is characterized in that: the pipeline of described first recycle system is provided with the first still liquid outlet valve (2) and first flow meter (4); The pipeline of described another recycle system is provided with the second still liquid outlet valve (19) and the second under meter (20).
3. a kind of device for hydrolyzing silicon tetrachloride according to claim 1 and 2, it is characterized in that: the top of described hydrolytic reaction pot (16) is tower reactor, filler (15) is inside housed, and top is provided with hydrogenchloride outlet (12) and circulation fluid import (13); Bottom is tank reactor, is provided with the leakage fluid dram (17) of liquor inlet (9), the first still liquid outlet (10a), the second still liquid outlet (10b) and bottom.
4. a kind of device for hydrolyzing silicon tetrachloride according to claim 3, it is characterized in that: the liner of described hydrolytic reaction pot (16) is enamel material, described recycle pump (3a, 3b) is selected acid and alkali-resistance vacuum pump, and described jet ejectors (8) is selected corrosion resistant surge pump.
CN201310114815.8A 2013-04-03 2013-04-03 Device for hydrolyzing silicon tetrachloride Expired - Fee Related CN103193235B (en)

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CN103193235B true CN103193235B (en) 2014-11-19

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1208016A (en) * 1998-08-27 1999-02-17 沈阳化工股份有限公司 Gas phase process preparing white carbon
CN201309832Y (en) * 2008-12-11 2009-09-16 张家港市华菱化工机械有限公司 Dry process tail gas recovery silicon tetrachloride elution column in production of polysilicon
CN101940898A (en) * 2010-09-26 2011-01-12 河北科技大学 Method and device for recycling silicon tetrachloride
CN202272745U (en) * 2011-08-09 2012-06-13 四川君和环保工程有限公司 Material separating device for silicon tetrachloride hydrolysis to prepare white carbon black

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1208016A (en) * 1998-08-27 1999-02-17 沈阳化工股份有限公司 Gas phase process preparing white carbon
CN201309832Y (en) * 2008-12-11 2009-09-16 张家港市华菱化工机械有限公司 Dry process tail gas recovery silicon tetrachloride elution column in production of polysilicon
CN101940898A (en) * 2010-09-26 2011-01-12 河北科技大学 Method and device for recycling silicon tetrachloride
CN202272745U (en) * 2011-08-09 2012-06-13 四川君和环保工程有限公司 Material separating device for silicon tetrachloride hydrolysis to prepare white carbon black

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