CN218452199U - Decomposition treatment device for high-boiling by-products in polycrystalline silicon production - Google Patents
Decomposition treatment device for high-boiling by-products in polycrystalline silicon production Download PDFInfo
- Publication number
- CN218452199U CN218452199U CN202222363202.5U CN202222363202U CN218452199U CN 218452199 U CN218452199 U CN 218452199U CN 202222363202 U CN202222363202 U CN 202222363202U CN 218452199 U CN218452199 U CN 218452199U
- Authority
- CN
- China
- Prior art keywords
- boiling
- chlorosilane
- reaction
- bottle
- decomposition treatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Silicon Compounds (AREA)
Abstract
The utility model discloses a high boiling by-product decomposition processing apparatus in polycrystalline silicon production belongs to polycrystalline silicon production technical field, including the reaction bulb, the reaction bulb lower extreme is provided with the heating device that adjusts the temperature, the reaction bulb passes through the intake pipe and links to each other with the hydrogen chloride gas bomb, the reaction bulb passes through the outlet duct and links to each other with the chlorosilane collecting bottle, be provided with the condenser on the outlet duct. And (3) putting the high-boiling-point substances and the discharged silicon powder into a reaction bottle, heating by a temperature-regulating heating device, introducing hydrogen chloride gas, condensing the chlorosilane obtained by the reaction by a condenser, and storing the condensed chlorosilane in a chlorosilane collecting bottle. The device does not need to add an additive additionally, and the reaction temperature is moderate.
Description
Technical Field
The utility model relates to a polycrystalline silicon production technical field, concretely relates to decomposition treatment device for medium and high boiling by-products in polycrystalline silicon production.
Background
SiHCl produced during the process of producing polysilicon by the modified Siemens process 3 And H 2 The gas enters a reduction furnace according to a certain proportion, the temperature of a silicon core carrier in the furnace reaches above 1050 ℃, and SiHCl 3 And H 2 The mixed gas generates reduction reaction SiHCl on the surface of the carrier 3 +H 2 = Si +3HCl and thermal decomposition reaction 4SiHCl 3 ＝Si+3SiCl 4 +2H 2 And depositing the generated silicon on the surface of a silicon core to form a polysilicon rod. In the reduction process, except silicon and SiCl 4 、SiH 2 Cl 2 、H 2 And HCl, etc., and Si 2 Cl 6 、Si 2 HCl 5 、Si 2 H 2 Cl 4 、Cl 6 OSi 2 And Si 3 Cl 8 And the side products of the double-silicon and multi-silicon atom compounds are generated, and the boiling points of the double-silicon and multi-silicon atom compounds are higher than those of trichlorosilane and silicon tetrachloride, namely the double-silicon and multi-silicon atom compounds are chlorosilane high-boiling-point substances.
The substances other than the silicon are discharged in the form of a reduction off-gas which is driedAfter recovery by the method and rectification and purification, siHCl 3 、SiCl 4 、SiH 2 Cl 2 、H 2 And HCl and other materials are returned to a system for recycling, after chlorosilane high-boiling residues and part of silicon tetrachloride are discharged from a rectifying tower kettle, most enterprises generally adopt a method of further concentrating the chlorosilane high-boiling residues to recover the silicon tetrachloride and then directly hydrolyzing, namely, reacting the chlorosilane high-boiling residues with water in a special hydrolysis device, leaching and absorbing hydrogen chloride gas generated by hydrolysis, neutralizing with alkali liquor, adjusting the pH until the pH value is neutral, generating a large amount of precipitates of metal compounds, further separating solid from liquid by means of filtration, centrifugation and the like, and directly transporting the solid substances out for landfill or utilization.
Chinese patent No. CN212315556U, published as 2021.01.08, discloses a cracking system for high-boiling chlorosilane by-product in polysilicon production, which is characterized by comprising: the filtering unit (10) is used for filtering chlorosilane high-boiling residues which are byproducts in the production of polycrystalline silicon to obtain purified high-boiling residues; a cracking unit, wherein the cracking unit comprises a cracking reactor, the cracking reactor is provided with a lower feeding section (31), a middle filling section (33) and an upper feeding section (35) which are sequentially communicated, the filtering unit (10) is connected with the upper feeding section (35) and is used for providing the purified high-boiling-point substances for the cracking reactor, the middle filling section (33) is filled with a solid alkali supported catalyst, and the solid alkali supported catalyst is a macroporous resin supported organic amine catalyst; a hydrogen chloride feed unit (20) connected to the lower feed section (31) for providing hydrogen chloride to the cracking reactor. The system still has the following problems: (1), higher reaction temperature is needed, and energy consumption is higher; (2) additional catalyst addition is required.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the problems in the prior art and provides a decomposition treatment device for high-boiling by-products in the production of polysilicon,
the utility model aims at realizing through the following technical scheme:
the utility model provides a high-boiling by-product decomposition processing apparatus in polycrystalline silicon production, includes the reaction flask, the reaction flask lower extreme is provided with the heating device that adjusts the temperature, the reaction flask passes through the intake pipe and links to each other with the hydrogen chloride gas bomb, the reaction flask passes through the outlet duct and links to each other with the chlorosilane collecting bottle, be provided with the condenser on the outlet duct.
Preferably, the chlorosilane collecting bottle is connected with the hydrofluoric acid absorption bottle through a first exhaust pipe.
Preferably, the hydrofluoric acid absorption bottle is connected with the tail gas absorption device through a second exhaust pipe.
Preferably, the tail gas absorption device is connected with the fan through a third exhaust pipe.
Preferably, an air inlet valve is arranged on the air inlet pipe.
Preferably, the reaction bottle is a round-bottom flask.
Preferably, the condenser is a Freon condenser.
The beneficial effects of this technical scheme are as follows:
1. the utility model provides a pair of high boiling by-product decomposition processing apparatus in polycrystalline silicon production, with high boiling thing and outer silica flour of arranging put into the reaction flask, let in hydrogen chloride gas after the heating of the heating device that adjusts the temperature, the reaction obtains chlorosilane and preserves in the chlorosilane collecting bottle after the condenser condensation. The device does not need to add additives additionally, and the reaction temperature is moderate.
2. The utility model provides a pair of high-boiling by-product decomposition treatment device in polycrystalline silicon production, the hydrofluoric acid absorption bottle is got rid of chlorosilane.
3. The utility model provides a pair of high-boiling by-product decomposition processing device in polycrystalline silicon production, tail gas absorbing device get rid of the silicon fluoride and the hydrogen chloride that do not get rid of.
Drawings
Fig. 1 is a schematic structural view of the present invention;
fig. 2 is a schematic structural diagram of another embodiment of the present invention;
wherein: 1. a reaction bottle; 2. a temperature adjusting and heating device; 3. an air inlet pipe; 4. a hydrogen chloride gas bomb; 5. an air outlet pipe; 6. a chlorosilane collecting bottle; 7. a condenser; 8.1, a first exhaust pipe; 8.2, a second exhaust pipe; 8.3, a third exhaust pipe; 9. a hydrofluoric acid absorption bottle; 10. a tail gas absorption device; 11. a fan; 12. an intake valve.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
It will be understood that when an element is referred to as being "on," "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
It should be noted that the terms of left, right, up and down in the embodiments of the present invention are only relative concepts or are referred to the normal use status of the product, and should not be considered as limiting.
Example 1
As shown in fig. 1, the decomposition treatment device for medium-high boiling byproducts in polysilicon production comprises a reaction bottle 1, wherein a temperature-adjusting heating device 2 is arranged at the lower end of the reaction bottle 1, the reaction bottle 1 is connected with a hydrogen chloride gas storage bottle 4 through an air inlet pipe 3, the reaction bottle 1 is connected with a chlorosilane collecting bottle 6 through an air outlet pipe 5, and a condenser 7 is arranged on the air outlet pipe 5. High-boiling residues and discharged silicon powder are placed in a reaction bottle 1, a temperature-adjusting heating device 2 is heated (to 300-350 ℃) and then is filled with hydrogen chloride gas, and chlorosilane obtained through reaction is condensed by a condenser 7 and then is stored in a chlorosilane collecting bottle 6. The device does not need to add an additive additionally, and the reaction temperature is moderate.
Example 2
As shown in fig. 2, the present embodiment is different from embodiment 1 in that: the chlorosilane collecting bottle 6 is connected with a hydrofluoric acid absorbing bottle 9 through a first exhaust pipe 8.1. The hydrofluoric acid absorption bottle 9 removes the uncondensed chlorosilane.
Wherein, the hydrofluoric acid absorption bottle 9 is connected with the tail gas absorption device 10 through a second exhaust pipe 8.2. The off-gas absorbing apparatus 10 removes silicon fluoride and hydrogen chloride that have not been removed.
Wherein, the tail gas absorption device 10 is connected with a fan 11 through a third exhaust pipe 8.3. The arrangement of the fan 11 makes the exhaust gas easier to discharge.
Wherein an intake valve 12 is provided on the intake pipe 3.
Wherein, the reaction bottle 1 adopts a round-bottom flask.
Wherein, the condenser 7 adopts a Freon condenser 7.
The using method of the device comprises the following steps:
(1) Putting the discharged silicon powder and the high-boiling residues into a reaction bottle 1;
(2) The inlet valve 12 is then opened and the tempering heating device 2 starts heating (up to 300-350 ℃);
(3) Gas is condensed through condenser 7 after the reaction, and most chlorosilane is got off by the condensation, and the gas of noncondensation gets into hydrofluoric acid absorption bottle 9, and during gas got into tail gas treatment bottle afterwards, unreacted gas passed through tail gas outlet duct 5 and discharges, through fan 11 with tail gas discharge system.
The chemical reaction that this device involves has:
high boiling + HCl + Si → (350 ℃/heavy metal catalyzed) SiHCl 3 +SiCl 4 +4H 2 ↑
SiHCl 3 + 2H 2 O =SiO 2 + 3HCl + H 2 ↑
SiO 2 +4HF=SiF 4 +2H 2 O
SiF 4+ 6NaOH →Na 2 SiO 3 +4NaF+3H 2 O
According to the device, no extra catalyst is needed, the discharged silicon powder and the high-boiling-point substance are directly added, the hydrogen chloride gas is introduced after heating to obtain chlorosilane, silicon chloride and hydrogen, and the chlorosilane is collected in a chlorosilane collecting bottle 6 after being condensed by a condenser 7; the uncondensed chlorosilane, the uncondensed silicon chloride and the uncondensed hydrogen enter a hydrofluoric acid absorption bottle 9, the chlorosilane reacts with water to obtain silicon dioxide, hydrogen chloride and the hydrogen, the silicon dioxide reacts with hydrofluoric acid to obtain silicon fluoride, and the hydrogen chloride and the silicon fluoride are absorbed by an alkali solution in a tail gas absorption device 10. Unreacted gas is discharged directly through the fan 11.
The above is only the preferred embodiment of the present invention, not to the limitation of the present invention in any form, all the technical matters of the present invention all fall into the protection scope of the present invention to any simple modification and equivalent change of the above embodiments.
Claims (7)
1. A decomposition treatment device for high-boiling byproducts in polysilicon production is characterized in that: including reaction flask (1), reaction flask (1) lower extreme is provided with heating device (2) adjust the temperature, reaction flask (1) links to each other with hydrogen chloride gas bomb (4) through intake pipe (3), reaction flask (1) links to each other with chlorosilane receiving flask (6) through outlet duct (5), be provided with condenser (7) on outlet duct (5).
2. The apparatus for decomposition treatment of high-boiling by-products in polysilicon production as recited in claim 1, wherein: the chlorosilane collecting bottle (6) is connected with a hydrofluoric acid absorption bottle (9) through a first exhaust pipe (8.1).
3. The decomposition treatment device for the high-boiling by-products in the production of polysilicon according to claim 2, characterized in that: and the hydrofluoric acid absorption bottle (9) is connected with the tail gas absorption device (10) through a second exhaust pipe (8.2).
4. The decomposition treatment device for the high-boiling by-products in the production of polysilicon according to claim 3, characterized in that: and the tail gas absorption device (10) is connected with a fan (11) through a third exhaust pipe (8.3).
5. The apparatus according to claim 1 or 4, wherein the apparatus comprises: and an air inlet valve (12) is arranged on the air inlet pipe (3).
6. The decomposition treatment device for the high-boiling by-products in the production of polysilicon according to claim 5, wherein: the reaction bottle (1) adopts a round-bottom flask.
7. The decomposition treatment device for the high-boiling by-products in the production of polysilicon according to claim 6, characterized in that: the condenser (7) adopts a Freon condenser.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222363202.5U CN218452199U (en) | 2022-09-06 | 2022-09-06 | Decomposition treatment device for high-boiling by-products in polycrystalline silicon production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222363202.5U CN218452199U (en) | 2022-09-06 | 2022-09-06 | Decomposition treatment device for high-boiling by-products in polycrystalline silicon production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN218452199U true CN218452199U (en) | 2023-02-07 |
Family
ID=85124373
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202222363202.5U Active CN218452199U (en) | 2022-09-06 | 2022-09-06 | Decomposition treatment device for high-boiling by-products in polycrystalline silicon production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN218452199U (en) |
-
2022
- 2022-09-06 CN CN202222363202.5U patent/CN218452199U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101143723B (en) | Modified method and device for preparing trichlorosilane and multicrystal silicon | |
| JP5621957B2 (en) | Method and apparatus for producing trichlorosilane | |
| JP4740646B2 (en) | Method for producing silicon | |
| CN101569817B (en) | Tail gas recycling method in trichlorosilane production | |
| CN105314637B (en) | Halogen silicon polymer cracking prepares the method and device of halosilanes | |
| CN101125276A (en) | Method for recovering tail gas of trichlorosilane production | |
| CN103382032A (en) | Preparation method for trichlorosilane from silicon tetrachloride | |
| CN103449446B (en) | Method for preparing trichlorosilane | |
| CN102923716A (en) | Process for producing trichlorosilane through inverse disporportionation of dichlorosilane | |
| CN218452199U (en) | Decomposition treatment device for high-boiling by-products in polycrystalline silicon production | |
| CN212315556U (en) | Cracking system for byproduct chlorosilane high-boiling residues in polycrystalline silicon production | |
| CN103449440B (en) | Equipment for preparing polycrystalline silicon | |
| CN204057977U (en) | For the apparatus system of halogen silicon polymer cracking for halosilanes | |
| CN103466626B (en) | A kind of production method of polysilicon | |
| CN102030335B (en) | Method and device for removing boron impurity in chlorosilane system by rectification through double-tower thermocouple reaction | |
| CN109467089B (en) | Polycrystalline silicon production method | |
| CN201136791Y (en) | Device for conversing silicon tetrachloride to be trichlorosilane by hydrochlorination process | |
| CN103482630B (en) | Prepare the method for polysilicon | |
| CN107074561A (en) | Use the poly plant and method of high-efficiency hybrid horizontal reactor | |
| CN205099363U (en) | System for production silicon nitride | |
| CN101519413B (en) | Method for circularly producing silane coupling agent | |
| CN106032275B (en) | Trichlorosilane synthesis process and system | |
| CN211078489U (en) | System for handle chlorosilane raffinate | |
| CN103449447B (en) | Prepare the equipment of trichlorosilane | |
| CN101481114A (en) | Method for recycling polysilicon by-product silicon tetrachloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |