CN216935386U - Chlorosilane tail gas cooling crystallization treatment system - Google Patents
Chlorosilane tail gas cooling crystallization treatment system Download PDFInfo
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- CN216935386U CN216935386U CN202220375317.3U CN202220375317U CN216935386U CN 216935386 U CN216935386 U CN 216935386U CN 202220375317 U CN202220375317 U CN 202220375317U CN 216935386 U CN216935386 U CN 216935386U
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Abstract
The utility model discloses a chlorosilane tail gas cooling crystallization treatment system, which comprises a hydrolysis neutralization device, a temperature reduction cooling crystallization device, an alkali liquor configuration device and a water seal device, wherein the hydrolysis neutralization device is connected with the temperature reduction cooling crystallization device; the slag discharging outlet of the hydrolysis neutralization device is connected with the temperature-reducing cooling crystallization device, and the generated slag-containing solution is sent into the temperature-reducing cooling crystallization device for crystallization; an exhaust port of the hydrolysis neutralization device is connected with the water seal device, and gas generated in the hydrolysis neutralization process is sent into the water seal device to be treated and then is exhausted into the atmosphere; the water seal device is connected with the alkali liquor configuration device, and redundant make-up water in the water seal device is sent into the alkali liquor configuration device to be used as configuration water; a liquid outlet of the alkali liquor configuration device is connected to the hydrolysis neutralization device, and alkali liquor is supplemented to the hydrolysis neutralization device for neutralization reaction; and a liquid outlet of the temperature-reducing cooling crystallization device is connected to the alkali liquor preparation device, and the solution generated in the temperature-reducing cooling crystallization process is sent to the alkali liquor preparation device for reuse.
Description
Technical Field
The utility model belongs to the field of polycrystalline silicon preparation, and particularly relates to a chlorosilane tail gas cooling crystallization treatment system.
Background
At present, the main processes for producing polycrystalline silicon in the photovoltaic industry are an improved Siemens method and a silane method, wherein the main production raw materials of the two methods are metallic silicon, hydrogen, trichlorosilane and the like, and the main production working sections of the improved Siemens method comprise a chlorine hydrogenation (cold hydrogenation) unit, a reduction unit, a rectification unit, a tail gas treatment unit and the like; the main production sections of the silane method comprise a chlorine hydrogenation (cold hydrogenation) unit, a silane synthesis unit, a granular silicon fluidized bed unit, a tail gas treatment unit and the like. The tail gas treatment units of the two are mainly used for treating Silicon Tetrachloride (STC), Dichlorosilane (DCS), Trichlorosilane (TCS), hydrogen chloride (HCl) and nitrogen (N) produced in the production process of polycrystalline silicon2) Hydrogen (H)2) And the like or safely venting the gas.
Most of polysilicon tail gas treatment systems condense chlorosilane in tail gas mainly through one-stage or multi-stage cooling devices, and part of the chlorosilane is condensed and recovered, or a chlorosilane condensation and recovery facility is arranged in a tail gas generation unit. However, chlorosilane and hydrogen chloride in the tail gas are not condensed and cannot be directly discharged, alkali liquor (lime milk or sodium hydroxide solution) is used for hydrolysis neutralization treatment, and the treated sewage with slag (mainly silicon powder, silicon dioxide, calcium chloride and the like) enters a subsequent waste residue and wastewater treatment system for treatment. At present, a newly-built polysilicon project does not allow wastewater discharge, and the content of chloride ions in the discharged water is also limited for old enterprises which are put into production. Therefore, a large amount of energy and material consumption still needs to be consumed for emission, and enterprises need to bear certain environmental protection and benefit pressure.
SUMMERY OF THE UTILITY MODEL
Utility model purpose: the utility model aims to solve the technical problem that the existing commonly used tail gas treatment process is improved aiming at the defects of a tail gas treatment unit in the production process of polycrystalline silicon, so that the waste water containing chloride ions is not discharged, the cyclic utilization of water is realized, the energy consumption and material consumption loss are reduced, the treatment pressure of the subsequent procedures is relieved, the production cost is reduced, and the environment friendliness is realized.
In order to achieve the purpose, the technical scheme adopted by the utility model is as follows:
a chlorosilane tail gas cooling crystallization treatment system comprises a hydrolysis neutralization device, a temperature reduction cooling crystallization device, an alkali liquor preparation device and a water sealing device;
a slag discharge outlet of the hydrolysis neutralization device is connected with a temperature-reducing cooling crystallization device, and the generated slag-containing solution is sent into the temperature-reducing cooling crystallization device for crystallization; an exhaust port of the hydrolysis neutralization device is connected with a water seal device, and gas generated in the hydrolysis neutralization process is sent into the water seal device to be treated and then is exhausted into the atmosphere;
the water seal device is connected with the alkali liquor configuration device, and redundant make-up water in the water seal device is sent into the alkali liquor configuration device to be used as configuration water;
a liquid outlet of the alkali liquor configuration device is connected to the hydrolysis neutralization device, and alkali liquor is supplemented to the hydrolysis neutralization device for neutralization reaction;
and a liquid outlet of the temperature-reducing cooling crystallization device is connected to the alkali liquor preparation device, and the solution generated in the temperature-reducing cooling crystallization process is sent to the alkali liquor preparation device for reuse.
Furthermore, the hydrolysis neutralization devices are a group and are sequentially connected in series; discharging the slag-containing alkali liquor generated by the upper stage hydrolysis neutralization device into the next stage hydrolysis neutralization device for further treatment, and sending the gas generated by the lower stage hydrolysis neutralization device into the upper stage hydrolysis neutralization device for further treatment.
Furthermore, the device also comprises a solution heating device which is connected between the temperature-reducing cooling crystallization device and the alkali liquor preparation device and is used for heating the solution generated in the temperature-reducing cooling crystallization process and then sending the solution into the alkali liquor preparation device.
Preferably, the hydrolysis neutralization device is any one of a hydrolysis neutralization tank, a reaction kettle, a reaction tank, a reaction tower and a washing tower with stirring or mixing.
Preferably, the temperature-reducing cooling crystallization device is any one of an internal circulation cooling type crystallizer, an external circulation cooling type crystallizer, a rotary drum cooling crystallizer, a cooling crystallization pool and a cooling crystallization tank.
Preferably, the water sealing device is any one of a dynamic wave type water sealing device, a water sealing tank and a water sealing tank.
Has the beneficial effects that:
the system cooling crystallization device is used for crystallization after hydrolysis and neutralization of polycrystalline silicon tail gas, and the discharged solution of the cooling crystallization device can be recycled, so that zero emission is realized. Can realize the discharge of waste water containing chloride ions and realize the cyclic utilization of water. The existing polycrystalline silicon tail gas treatment system is conveniently optimized and improved, or in the new project, the closed cycle of the Siemens method polycrystalline silicon production is perfected, the material loss is reduced, the production cost is reduced, zero emission is realized, and the environment friendliness is realized.
Drawings
The foregoing and/or other advantages of the utility model will become further apparent from the following detailed description of the utility model when taken in conjunction with the accompanying drawings.
FIG. 1 is a block diagram of a chlorosilane tail gas cooling crystallization treatment system in example 1.
FIG. 2 is a flow chart of a chlorosilane tail gas cooling crystallization treatment system in example 1.
FIG. 3 is a flow chart of a chlorosilane tail gas cooling crystallization treatment system in example 2.
Detailed Description
The utility model will be better understood from the following examples.
The structures, proportions, and dimensions shown in the drawings and described in the specification are for understanding and reading the present disclosure, and are not intended to limit the scope of the present disclosure, which is defined in the claims, and are not essential to the skilled in the art. In addition, the terms "upper", "lower", "front", "rear" and "middle" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the relative positions may be changed or adjusted without substantial technical changes.
Example 1
As shown in the figures 1 and 2, the chlorosilane tail gas cooling crystallization treatment system comprises a hydrolysis neutralization device 1, a temperature-reducing cooling crystallization device 2, an alkali liquor configuration device 3 and a water sealing device 4.
Wherein, the slag discharging outlet of the hydrolysis neutralization device is connected with the temperature-reducing cooling crystallization device, and the generated slag-containing solution is sent into the temperature-reducing cooling crystallization device for crystallization; the gas outlet of the hydrolysis neutralization device is connected with the water seal device, and gas generated in the hydrolysis neutralization process is sent into the water seal device for treatment and then discharged into the atmosphere.
The water seal device is connected with the alkali liquor configuration device, and the redundant make-up water in the water seal device is sent into the alkali liquor configuration device to be used as configuration water.
And a liquid outlet of the alkali liquor configuration device is connected to the hydrolysis neutralization device, and alkali liquor is supplemented to the hydrolysis neutralization device for neutralization reaction.
And a liquid outlet of the temperature-reducing cooling crystallization device is connected to the alkali liquor preparation device, and the solution generated in the temperature-reducing cooling crystallization process is sent to the alkali liquor preparation device for reuse.
The system also comprises a solution heating device 5 which is connected between the desuperheating cooling crystallization device and the alkali liquor preparation device, and the solution generated in the desuperheating cooling crystallization process is sent to the solution heating device 5 by a diaphragm pump to be heated and then sent into the alkali liquor preparation device.
Specifically, in this embodiment, the hydrolysis neutralization device is a hydrolysis neutralization tank with stirring or mixing, the desuperheating cooling crystallization device is an internal circulation cooling crystallizer, and the water seal device is a water seal tank.
Example 2
As shown in fig. 3, the difference from example 1 is that the hydrolysis neutralization apparatus has two stages, which are connected in series; discharging the slag-containing alkali liquor generated by the upper stage hydrolysis neutralization device into the next stage hydrolysis neutralization device for further treatment, and sending the gas generated by the lower stage hydrolysis neutralization device into the upper stage hydrolysis neutralization device for further treatment.
After tail gas from each section of polycrystalline silicon production is condensed by a multi-stage cooling device to recover chlorosilane or condensed by a tail gas generating unit to recover chlorosilane, the gas components of the residual polycrystalline silicon tail gas are mainly extremely small amount of uncondensed chlorosilane, hydrogen chloride, nitrogen, hydrogen and the like, the gas enters a primary hydrolysis neutralization device to perform neutralization reaction, the neutralization device mainly adopts alkali liquor to perform neutralization reaction, the main components of reaction vent gas are nitrogen, hydrogen, trace hydrogen chloride and other gases which can not be neutralized or are not neutralized, the gas enters a secondary hydrolysis neutralization device to perform neutralization reaction, the vent gas after the reaction is discharged to the atmosphere through a water seal device, water supplemented by a system flows into the alkali liquor configuration device from the water seal device, waste residue generated by the secondary hydrolysis neutralization device and the alkali liquor enter the primary hydrolysis neutralization device, and slag-containing sewage generated by the primary hydrolysis neutralization device enters a cooling crystallization device to be crystallized, the low-temperature saturated solution of the crystallization device is heated by a solution heating device (the temperature of the second-stage hydrolysis neutralization device is raised according to the temperature of the second-stage hydrolysis neutralization device, the temperature of the second-stage hydrolysis neutralization device needs to be 20-100 ℃ higher than that of the low-temperature crystallization removal solution), and then the low-temperature saturated solution and alkali liquor (such as calcium oxide, sodium hydroxide and the like) are prepared and returned to the first-stage hydrolysis neutralization device and the second-stage hydrolysis neutralization device for use, and crystallized filter residues can be recycled as materials for paving building materials and the like.
The utility model provides a thought and a method of a chlorosilane tail gas cooling crystallization treatment system, and a method and a way for realizing the technical scheme are many, the above description is only a preferred embodiment of the utility model, and it should be noted that, for a person skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the utility model, and the improvements and decorations should also be regarded as the protection scope of the utility model. All the components not specified in the present embodiment can be realized by the prior art.
Claims (6)
1. A chlorosilane tail gas cooling crystallization treatment system is characterized by comprising a hydrolysis neutralization device, a temperature reduction cooling crystallization device, an alkali liquor preparation device and a water seal device;
the slag discharging outlet of the hydrolysis neutralization device is connected with the temperature-reducing cooling crystallization device, and the generated slag-containing solution is sent into the temperature-reducing cooling crystallization device for crystallization; an exhaust port of the hydrolysis neutralization device is connected with a water seal device, and gas generated in the hydrolysis neutralization process is sent into the water seal device to be treated and then is exhausted into the atmosphere;
the water seal device is connected with the alkali liquor configuration device, and redundant make-up water in the water seal device is sent into the alkali liquor configuration device to be used as configuration water;
a liquid outlet of the alkali liquor configuration device is connected to the hydrolysis neutralization device, and alkali liquor is supplemented to the hydrolysis neutralization device for neutralization reaction;
and a liquid outlet of the temperature-reducing cooling crystallization device is connected to the alkali liquor preparation device, and the solution generated in the temperature-reducing cooling crystallization process is sent to the alkali liquor preparation device for reuse.
2. The chlorosilane tail gas cooling and crystallizing treatment system as claimed in claim 1, wherein the hydrolysis and neutralization devices are in a group and are sequentially connected in series; discharging the slag-containing alkali liquor generated by the upper stage hydrolysis neutralization device into the next stage hydrolysis neutralization device for further treatment, and sending the gas generated by the lower stage hydrolysis neutralization device into the upper stage hydrolysis neutralization device for further treatment.
3. The chlorosilane tail gas cooling crystallization treatment system as claimed in claim 1, further comprising a solution heating device connected between the temperature-reducing cooling crystallization device and the alkali liquor preparation device, wherein the solution generated in the temperature-reducing cooling crystallization process is heated and then sent into the alkali liquor preparation device.
4. The chlorosilane tail gas cooling and crystallizing treatment system as claimed in claim 1, wherein the hydrolysis neutralization device is any one of a hydrolysis neutralization tank, a reaction kettle, a reaction tank, a reaction tower and a washing tower with stirring or mixing functions.
5. The chlorosilane tail gas cooling crystallization treatment system as claimed in claim 1, wherein the temperature-reducing cooling crystallization device is any one of an internal circulation cooling type crystallizer, an external circulation cooling type crystallizer, a rotary drum cooling crystallizer, a cooling crystallization pool and a cooling crystallization tank.
6. The chlorosilane tail gas cooling and crystallizing treatment system according to claim 1, wherein the water sealing device is any one of a power wave type water sealing device, a water sealing tank and a water sealing tank.
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| CN202220375317.3U CN216935386U (en) | 2022-02-23 | 2022-02-23 | Chlorosilane tail gas cooling crystallization treatment system |
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| CN202220375317.3U CN216935386U (en) | 2022-02-23 | 2022-02-23 | Chlorosilane tail gas cooling crystallization treatment system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116102018A (en) * | 2022-11-11 | 2023-05-12 | 石河子大学 | Method for separating hexachlorodisilane from polysilicon byproduct oligomeric chlorosilane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116102018A (en) * | 2022-11-11 | 2023-05-12 | 石河子大学 | Method for separating hexachlorodisilane from polysilicon byproduct oligomeric chlorosilane |
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