CN210825446U - Cold hydrogenation slag slurry zero-emission treatment system - Google Patents
Cold hydrogenation slag slurry zero-emission treatment system Download PDFInfo
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Abstract
The utility model discloses a cold hydrogenation slag slurry zero-emission treatment system, which comprises a stirring tank, a dryer, a filter, a buffer tank, a flash evaporation kettle, a high-boiling-point substance storage tank, a condenser A, a condenser B, an intermediate storage tank A, an intermediate storage tank B, a rectifying tower, an acid-removing cooling machine and a high-boiling-point substance treatment device; the utility model has the advantages that: after liquid chlorosilane containing silicon powder from a cold hydrogenation device is treated by the system, the silicon powder is recovered and sold, and the recovered chlorosilane is reused in a polysilicon production system, so that raw materials for polysilicon production are saved, the yield of materials is improved, and the production cost of polysilicon is reduced; realizing zero discharge of the residual liquid of the high-boiling residues and reducing the influence on the environment.
Description
The technical field is as follows:
the utility model relates to a sediment thick liquid zero release processing system especially relates to cold hydrogenation sediment thick liquid zero release processing system.
Background art:
the improved Siemens process has the production process of synthesizing HCl with chlorine and hydrogen and SiHCl with HCl and metal silicon powder at certain temperature3Gas and synthesis gas are subjected to the processes of dust removal, washing, condensation and the like, and then chlorosilane liquid is sent to a TCS purification device. High-purity Trichlorosilane (TCS), Silicon Tetrachloride (STC) and Dichlorosilane (DCS) are separated in a TCS purification device by a rectification method. STC is sent to a cold hydrogenation device, is subjected to thermal decomposition and hydrogenation reaction under the conditions of high temperature and high pressure and a catalyst to obtain TCS, and is sent to a TCS purification device. And sending DCS to a reverse disproportionation device, mixing STC and DCS according to a certain proportion, sending to a disproportionation reactor, reacting under the action of a catalyst to generate TCS, and sending to a TCS purification device. And the TCS is sent to a reduction device and sent to a TCS vaporizer, and the TCS is vaporized and superheated by steam heating and enters a mixer together with the circulating hydrogen sent from the tail gas recovery workshop. After hydrogen and trichlorosilane are mixed in a certain proportion, the mixture is fed into each reduction furnace according to a program control appropriate flow, trichlorosilane is reduced into crystalline silicon on the surface of a silicon core (silicon rod) by hydrogen on the surface of a high-temperature silicon core (silicon rod) electrified in the furnace, the crystalline silicon is deposited on the surface of the silicon core (silicon rod), the diameter of the silicon rod is continuously increased until the silicon rod reaches a specified size, and the polysilicon rod is discharged by opening the furnace periodically. And conveying the polysilicon rod to a product finishing device, crushing, cleaning and packaging for sale.
The cold hydrogenation production process is to utilize hydrogen and vaporized silicon tetrachloride to carry out gas-solid phase reaction with metal silicon powder in a fluidized bed, and a cyclone separator is arranged at the top of the fluidized bed to recover the silicon powder in the reaction tail gas and return the silicon powder to the fluidized bed. Along with the reaction, the particles of the silicon powder gradually become smaller, the silicon powder is taken out from the top of the fluidized bed by reaction tail gas, enters a quenching tower, is sprayed, dedusted and trapped by chlorosilane, is discharged to a stripping tower, and is discontinuously discharged to a slurry stirring tank. In the production process, a large amount of silicon tetrachloride slag slurry waste containing more than 5 percent of silicon powder is discharged by the cold hydrogenation device every day and is directly discharged to pollute the environment. At present, polysilicon enterprises generally directly and properly dry the slag containing silicon powder to obtain muddy silicon slag, and then hydrolyze the muddy silicon slag by using lime milk. Discharging a large amount of hydrolysate containing slag after hydrolysis, performing filter pressing to separate silicon dioxide slag, and treating a large amount of wastewater containing high chloride ions and calcium ions. At present, no better treatment method exists, the environment protection situation is very severe, and normal production operation can be influenced at any time.
The utility model has the following contents:
an object of the utility model is to provide an improve the yield of material, reduce polycrystalline silicon manufacturing cost, realize the high thing raffinate zero release that boils, reduce the cold hydrogenation sediment thick liquid zero release processing system to the influence of environment.
The utility model discloses by following technical scheme implement: the cold hydrogenation slag slurry zero-emission treatment system comprises a stirring tank, a dryer, a filter, a buffer tank, a flash evaporation kettle, a high-boiling-point substance storage tank, a condenser A, a condenser B, an intermediate storage tank A, an intermediate storage tank B, a rectifying tower, an acid removal cooling machine and a high-boiling-point substance treatment device;
the silicon slurry outlet of the stirring tank is connected with the material inlet of the dryer, the material outlet of the dryer is connected with the feed inlet of the deacidification cooler, the gas outlet of the dryer is connected with the gas inlet of the condenser A, and the liquid outlet of the condenser A is connected with the inlet of the intermediate storage tank A;
the supernatant outlet of the stirring tank is connected with the inlet of the filter, the outlet of the filter is connected with the inlet of the buffer tank, the outlet of the buffer tank is connected with the inlet of the flash evaporation kettle, the high-boiling-point substance outlet of the flash evaporation kettle is connected with the inlet of the high-boiling-point substance storage tank, the gas-phase outlet of the flash evaporation kettle is connected with the inlet of the condenser B, the outlet of the condenser B is connected with the inlet of the intermediate storage tank B, and the outlet of the intermediate storage tank B is connected with the inlet of the rectifying tower; and the outlet of the high-boiling-point substance storage tank is connected with the inlet of the high-boiling-point substance treatment device.
Further, the high boiling substance treatment apparatus includes: the device comprises an aluminum ionic liquid stirring tank, an aluminum removal column, a vaporizer, a heater, a gas phase aluminum removal column, a separation tower and a cracking reaction kettle;
the outlet of the high-boiling-point substance storage tank is connected with the inlet of the aluminum ionic liquid stirring tank, the outlet of the aluminum ionic liquid stirring tank is connected with the inlet of the aluminum removing column, the outlet of the aluminum removing column is respectively connected with the inlet of the vaporizer and the inlet of the heater, the outlet of the heater is connected with the inlet of the aluminum ionic liquid stirring tank, the outlet of the vaporizer is connected with the inlet of the gas phase aluminum removing column, the outlet of the gas phase aluminum removing column is connected with the inlet of the separation tower, the high-boiling-point substance outlet of the separation tower is connected with the inlet of the cracking reaction kettle, and the outlet of the cracking reaction kettle is connected with the inlet of the separation tower; the top outlet of the separation tower 18 is connected with the inlet of the rectifying tower 11.
Further, a back-blowing inlet of the filter is connected with a chlorosilane pipeline without high-boiling residues, and a back-blowing material outlet of the filter is connected with an inlet of the stirring tank.
Further, a cooling jacket is arranged on the outer wall of the tank body of the stirring tank, a cooling medium inlet and a cooling medium outlet are arranged on the cooling jacket, and the cooling medium inlet is connected with a cooling medium inlet pipeline; the cooling medium outlet is connected with a cooling medium outlet pipeline.
The utility model has the advantages that after the liquid chlorosilane containing silicon powder from the cold hydrogenation device is processed by the system of the utility model, the silicon powder can be separately recycled for sale, thereby increasing the added value of the product; meanwhile, a large amount of chlorosilane is recovered after the processes of separation, drying, evaporation, condensation and the like are carried out; further removing aluminum chloride in the material system through aluminum removal and cracking processes, and cracking the high-boiling-point substances into chlorosilane such as trichlorosilane, silicon tetrachloride and the like; the recovered chlorosilane is reused in a polycrystalline silicon production system, so that polycrystalline silicon production raw materials are saved, the yield of materials is improved, and the production cost of polycrystalline silicon is reduced; realizing zero discharge of the residual liquid of the high-boiling residues and reducing the influence on the environment.
After the utility model is adopted, no waste water is generated, and the environmental protection pressure is reduced; chlorosilane is recycled, so that waste is changed into valuable, and the utilization rate of materials is improved; the process can also obtain the micro silicon powder, thereby generating certain economic value.
Description of the drawings:
FIG. 1 is a schematic view of a zero-emission treatment system for cold hydrogenation of slag slurry according to example 1.
The device comprises a stirring tank 1, a dryer 2, a filter 3, a buffer tank 4, a flash evaporation kettle 5, a high-boiling-point substance storage tank 6, a condenser A7, a condenser B8, an intermediate storage tank A9, an intermediate storage tank B10, a rectifying tower 11, an acid-removing cooler 12, an aluminum ion liquid stirring tank 13, an aluminum-removing column 14, a vaporizer 15, a heater 16, a gas-phase aluminum-removing column 17, a separation tower 18, a cracking reaction kettle 19 and a chlorosilane pipeline 20.
The specific implementation mode is as follows:
example 1: the zero-emission treatment system for the cold hydrogenation slag slurry is characterized by comprising a stirring tank 1, a dryer 2, a filter 3, a buffer tank 4, a flash evaporation kettle 5, a high-boiling-point substance storage tank 6, a condenser A7, a condenser B8, an intermediate storage tank A9, an intermediate storage tank B10, a rectifying tower 11, an acid removal cooler 12 and a high-boiling-point substance treatment device; the high boiling substance treatment apparatus comprises: an aluminum ionic liquid stirring tank 13, an aluminum removal column 14, a vaporizer 15, a heater 16, a gas phase aluminum removal column 17, a separation tower 18 and a cracking reaction kettle 19; a cooling jacket is arranged on the outer wall of the tank body of the stirring tank 1, a cooling medium inlet and a cooling medium outlet are arranged on the cooling jacket, and the cooling medium inlet is connected with a cooling medium inlet pipeline; the cooling medium outlet is connected with the cooling medium outlet pipeline.
A silicon slurry outlet of the stirring tank 1 is connected with a material inlet of a dryer 2, a material outlet of the dryer 2 is connected with a feed inlet of an acid removal cooler 12, a gas outlet of the dryer 2 is connected with a gas inlet of a condenser A7, and a liquid outlet of the condenser A7 is connected with an inlet of an intermediate storage tank A9;
a supernatant outlet of the stirring tank 1 is connected with an inlet of a filter 3, an outlet of the filter 3 is connected with an inlet of a buffer tank 4, a back-blowing gas inlet of the filter 3 is connected with a chlorosilane pipeline 20 without high-boiling residues, and a back-blowing material outlet of the filter 3 is connected with an inlet of the stirring tank 1;
the outlet of the intermediate storage tank A9 and the outlet of the buffer tank 4 are both connected with the inlet of the flash evaporation kettle 5, the high-boiling-point substance outlet of the flash evaporation kettle 5 is connected with the inlet of the high-boiling-point substance storage tank 6, the gas phase outlet of the flash evaporation kettle 5 is connected with the inlet of the condenser B8, the outlet of the condenser B8 is connected with the inlet of the intermediate storage tank B10, and the outlet of the intermediate storage tank B10 is connected with the inlet of the rectifying tower 11; the outlet of the high-boiling-point substance storage tank 6 is connected with the inlet of an aluminum ionic liquid stirring tank 13, the outlet of the aluminum ionic liquid stirring tank 13 is connected with the inlet of an aluminum removing column 14, the outlet of the aluminum removing column 14 is respectively connected with the inlet of a vaporizer 15 and the inlet of a heater 16, the outlet of the heater 16 is connected with the inlet of the aluminum ionic liquid stirring tank 13, the outlet of the vaporizer 15 is connected with the inlet of a gas-phase aluminum removing column 17, the outlet of the gas-phase aluminum removing column 17 is connected with the inlet of a separation tower 18, the high-boiling-point substance outlet of the separation tower 18 is connected with the inlet of a cracking reaction kettle 19, and the outlet of the cracking reaction kettle 19 is connected with the inlet of the separation tower 18; the top outlet of the separation tower 18 is connected with the inlet of the rectifying tower 11.
Liquid chlorosilane containing silicon powder from a cold hydrogenation device enters a stirring tank 1 with a cooling jacket for stirring and cooling, and then stands for layering. The method aims to cool the material, is beneficial to the separation of the silicon powder after the aggregation of the silicon powder, and obtains clean supernatant and slurry containing the silicon powder; the supernatant enters the filter 3 for filtration, and the filter 3 is provided with a back washing device, so that the filter 3 is prevented from being blocked due to long-term use. The supernatant further enters a flash evaporation kettle 5 to remove high-boiling-point substance impurities. Gas-phase chlorosilane evaporated from the flash evaporation kettle 5 is condensed by a condenser B8 to obtain chlorosilane, and the chlorosilane is returned to a rectifying tower 11 of the polysilicon production system for rectification.
And (3) drying the slurry containing the silicon powder in a dryer 2, feeding the dried silicon powder into an acid removal cooler 12, adding a proper amount of acid removal agent to remove residual chlorosilane, and packaging and selling the finished silicon powder. Liquid chlorosilane containing silicon powder is subjected to standing and layering in the stirring tank 1, a large amount of supernatant is separated, and the load of the dryer 2 can be greatly reduced. The gas phase chlorosilane evaporated by the drier 2 is condensed by a condenser A7 and then enters a flash evaporation kettle 5, and the gas phase chlorosilane and the supernatant are flashed together to remove high-boiling-point substance impurities in the chlorosilane.
High-boiling-point substance impurities separated from the flash evaporation kettle 5 enter a high-boiling-point substance storage tank 6 and then enter an aluminum ionic liquid stirring tank 13 through a raw material pump. The aluminum ion liquid stirring tank 13 is internally provided with a stirring device, and after the materials are heated and pressurized, the aluminum column 14 is removed through a high-temperature circulating pump. The aluminum removing column 14 is internally provided with an aluminum removing agent for liquid phase aluminum removal and filtering and trapping a solid phase generated in the aluminum removing process; a part of the materials after liquid phase aluminum removal are extracted and enter a vaporizer 15, and a part of the materials return to the aluminum ionic liquid stirring tank 13 after passing through a heater 16. The material entering the vaporizer 15 enters a gas phase aluminum removal column 17 after flash vaporization, the gas phase aluminum removal column 17 is of a tray structure, and an aluminum remover is placed on the tray. When the gas-phase chlorosilane passes through the tray, metal chlorides such as aluminum chloride and the like are captured by the ionic liquid, and the rest of the gas-phase chlorosilane is discharged from the top of the tower and enters the separation tower 18. The separation tower 18 adopts steam heating at the tower bottom and adopts circulating water and deep cooling two-stage condensation at the tower top. And chlorosilane such as trichlorosilane, silicon tetrachloride and the like is obtained at the tower top and is returned to the rectifying tower 11 of the polysilicon production system for rectification. The high-boiling residue obtained from the tower bottom enters a cracking reaction kettle 19 through a pump, chlorosilane in the cracking reaction kettle 19 reacts with hydrogen chloride to obtain a chlorosilane monomer, and the chlorosilane monomer returns to a separation tower 18 through the pump.
The agitator tank 1 that the embodiment relates to, desiccator 2, filter 3, buffer tank 4, flash distillation cauldron 5, high boiling thing storage tank 6, condenser A7, condenser B8, intermediate storage tank A9, intermediate storage tank B10, rectifying column 11, deacidification cooler 12, aluminium ion liquid agitator tank 13 removes aluminium column 14, vaporizer 15, heater 16, gaseous phase removes aluminium column 17, knockout tower 18, cracking reaction cauldron 19 is conventional equipment, and its specific structure is no longer repeated in this application. The aluminum removal column 14 and the vapor phase aluminum removal column 17 were fixed bed packed columns produced by Hubei Ribang Equipment Co., Ltd. The deacidification machine is produced by Changzhou Zhongshi Sanshui mechanical science and technology limited, and alkaline substances are added into the recycled micro silicon powder for mixing deacidification.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The zero-emission treatment system for the cold hydrogenation slag slurry is characterized by comprising a stirring tank, a dryer, a filter, a buffer tank, a flash evaporation kettle, a high-boiling-point substance storage tank, a condenser A, a condenser B, an intermediate storage tank A, an intermediate storage tank B, a rectifying tower, an acid-removing cooling machine and a high-boiling-point substance treatment device;
the silicon slurry outlet of the stirring tank is connected with the material inlet of the dryer, the material outlet of the dryer is connected with the feed inlet of the deacidification cooler, the gas outlet of the dryer is connected with the gas inlet of the condenser A, and the liquid outlet of the condenser A is connected with the inlet of the intermediate storage tank A;
the supernatant outlet of the stirring tank is connected with the inlet of the filter, the outlet of the filter is connected with the inlet of the buffer tank, the outlet of the buffer tank is connected with the inlet of the flash evaporation kettle, the high-boiling-point substance outlet of the flash evaporation kettle is connected with the inlet of the high-boiling-point substance storage tank, the gas-phase outlet of the flash evaporation kettle is connected with the inlet of the condenser B, the outlet of the condenser B is connected with the inlet of the intermediate storage tank B, and the outlet of the intermediate storage tank B is connected with the inlet of the rectifying tower; and the outlet of the high-boiling-point substance storage tank is connected with the inlet of the high-boiling-point substance treatment device.
2. The zero-emission treatment system for cold hydrogenation slag slurry as claimed in claim 1, wherein the high-boiling-point substance treatment device comprises: the device comprises an aluminum ionic liquid stirring tank, an aluminum removal column, a vaporizer, a heater, a gas phase aluminum removal column, a separation tower and a cracking reaction kettle;
the outlet of the high-boiling-point substance storage tank is connected with the inlet of the aluminum ionic liquid stirring tank, the outlet of the aluminum ionic liquid stirring tank is connected with the inlet of the aluminum removing column, the outlet of the aluminum removing column is respectively connected with the inlet of the vaporizer and the inlet of the heater, the outlet of the heater is connected with the inlet of the aluminum ionic liquid stirring tank, the outlet of the vaporizer is connected with the inlet of the gas phase aluminum removing column, the outlet of the gas phase aluminum removing column is connected with the inlet of the separation tower, the high-boiling-point substance outlet of the separation tower is connected with the inlet of the cracking reaction kettle, and the outlet of the cracking reaction kettle is connected with the inlet of the separation tower; the outlet of the separating tower (18) is connected with the inlet of the rectifying tower (11).
3. The cold hydrogenation slag slurry zero-emission treatment system according to claim 1 or 2, wherein a blowback gas inlet of the filter is connected with a chlorosilane pipeline without high-boiling residues, and a blowback material outlet of the filter is connected with an inlet of the stirring tank.
4. The cold hydrogenation slag slurry zero-emission treatment system according to claim 1 or 2, wherein a cooling jacket is arranged on the outer wall of the tank body of the stirring tank, a cooling medium inlet and a cooling medium outlet are arranged on the cooling jacket, and the cooling medium inlet is connected with a cooling medium inlet pipeline; the cooling medium outlet is connected with a cooling medium outlet pipeline.
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| CN201921720176.9U CN210825446U (en) | 2019-10-14 | 2019-10-14 | Cold hydrogenation slag slurry zero-emission treatment system |
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| CN201921720176.9U CN210825446U (en) | 2019-10-14 | 2019-10-14 | Cold hydrogenation slag slurry zero-emission treatment system |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905438A (en) * | 2020-09-01 | 2020-11-10 | 新疆协鑫新能源材料科技有限公司 | Process and device for drying and mixing residue and filter residue of slurry |
| CN112408396A (en) * | 2020-11-30 | 2021-02-26 | 天津大学 | Process and equipment for removing aluminum by chlorosilane complexation |
| WO2022041699A1 (en) * | 2020-08-24 | 2022-03-03 | 中国恩菲工程技术有限公司 | Silicon tetrachloride cold hydrogenation system |
| CN114590811A (en) * | 2022-03-10 | 2022-06-07 | 内蒙古新特硅材料有限公司 | Method and device for treating chlorosilane slurry |
| CN115650241A (en) * | 2022-10-28 | 2023-01-31 | 内蒙古通威高纯晶硅有限公司 | Polysilicon production slag slurry treatment process |
| CN116477631A (en) * | 2023-04-04 | 2023-07-25 | 青海黄河上游水电开发有限责任公司新能源分公司 | Polycrystalline silicon slag slurry recovery system |
-
2019
- 2019-10-14 CN CN201921720176.9U patent/CN210825446U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022041699A1 (en) * | 2020-08-24 | 2022-03-03 | 中国恩菲工程技术有限公司 | Silicon tetrachloride cold hydrogenation system |
| CN111905438A (en) * | 2020-09-01 | 2020-11-10 | 新疆协鑫新能源材料科技有限公司 | Process and device for drying and mixing residue and filter residue of slurry |
| CN112408396A (en) * | 2020-11-30 | 2021-02-26 | 天津大学 | Process and equipment for removing aluminum by chlorosilane complexation |
| CN114590811A (en) * | 2022-03-10 | 2022-06-07 | 内蒙古新特硅材料有限公司 | Method and device for treating chlorosilane slurry |
| CN115650241A (en) * | 2022-10-28 | 2023-01-31 | 内蒙古通威高纯晶硅有限公司 | Polysilicon production slag slurry treatment process |
| CN116477631A (en) * | 2023-04-04 | 2023-07-25 | 青海黄河上游水电开发有限责任公司新能源分公司 | Polycrystalline silicon slag slurry recovery system |
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