CN117602646A - Comprehensive recovery zero-emission system for high-salt wastewater generated in polysilicon production - Google Patents
Comprehensive recovery zero-emission system for high-salt wastewater generated in polysilicon production Download PDFInfo
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- CN117602646A CN117602646A CN202311421725.3A CN202311421725A CN117602646A CN 117602646 A CN117602646 A CN 117602646A CN 202311421725 A CN202311421725 A CN 202311421725A CN 117602646 A CN117602646 A CN 117602646A
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- 239000002351 wastewater Substances 0.000 title claims abstract description 120
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 31
- 238000011084 recovery Methods 0.000 title claims abstract description 17
- 229920005591 polysilicon Polymers 0.000 title claims description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 143
- 238000001704 evaporation Methods 0.000 claims abstract description 140
- 230000008020 evaporation Effects 0.000 claims abstract description 136
- 239000012452 mother liquor Substances 0.000 claims abstract description 48
- 238000002425 crystallisation Methods 0.000 claims abstract description 38
- 230000008025 crystallization Effects 0.000 claims abstract description 38
- 238000001816 cooling Methods 0.000 claims abstract description 32
- 230000008676 import Effects 0.000 claims abstract description 21
- 150000003839 salts Chemical class 0.000 claims abstract description 20
- 238000004064 recycling Methods 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 82
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 abstract description 45
- 239000001110 calcium chloride Substances 0.000 abstract description 43
- 229910001628 calcium chloride Inorganic materials 0.000 abstract description 43
- 239000011780 sodium chloride Substances 0.000 abstract description 38
- 238000007701 flash-distillation Methods 0.000 abstract description 20
- 238000004065 wastewater treatment Methods 0.000 abstract description 16
- 238000005265 energy consumption Methods 0.000 abstract description 15
- 239000002699 waste material Substances 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 44
- 238000000034 method Methods 0.000 description 20
- 230000008569 process Effects 0.000 description 17
- 238000000926 separation method Methods 0.000 description 9
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/007—Energy recuperation; Heat pumps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
- B01D3/065—Multiple-effect flash distillation (more than two traps)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
- B01D5/009—Collecting, removing and/or treatment of the condensate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/32—Purification
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/06—Flash evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/346—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from semiconductor processing, e.g. waste water from polishing of wafers
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/10—Energy recovery
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The application relates to a zero release system is synthesized to polycrystalline silicon production high salt waste water, the concentrated export of first flash distillation cauldron links to each other with the waste water import of second flash distillation cauldron, the concentrated export of second flash distillation cauldron links to each other with the import of centrifuge, the mother liquor export of centrifuge links to each other with the waste water import of third flash distillation cauldron, the concentrated export of third flash distillation cauldron links to each other with cooling crystallization device's import, cooling crystallization device's mother liquor export links to each other with the waste water import of first flash distillation cauldron, electric heater's export links to each other with the heating import of third flash distillation cauldron, the heating export and/or the steam export of third flash distillation cauldron links to each other with the heating import of second flash distillation cauldron, the heating export and/or the steam export of second flash distillation cauldron link to each other with the heating import of first flash distillation cauldron. The system can realize the separate recovery of calcium chloride and sodium chloride in the high-salt wastewater, does not generate any wastewater and waste residues, has zero emission, can save steam required by heating of the first flash evaporation kettle and the second flash evaporation kettle, and reduces the operation energy consumption of high-salt wastewater treatment.
Description
Technical Field
The application relates to the technical field of high-salt wastewater treatment in the production process of polycrystalline silicon, in particular to a comprehensive recovery zero-emission system for high-salt wastewater in the production process of polycrystalline silicon.
Background
Polysilicon is a very important intermediate product in the silicon product industry chain, is a main raw material for manufacturing silicon polished wafers, solar cells and high-purity silicon products, and is a raw material for information industry and new energy foundation. In general, currently the main conventional processes for the international production of polysilicon are the modified siemens process, the silane process and the fluidized bed process. Wherein the polysilicon produced by the modified siemens process has the greatest productivity. A great amount of high-salt wastewater mainly containing calcium chloride and sodium chloride is generated in the production process of the polysilicon produced by the current improved Siemens technology, and the direct discharge can seriously pollute the environment.
The currently adopted treatment method is shown in fig. 1, firstly, high-salt wastewater generated in the production process of polysilicon sequentially passes through a first flash evaporation kettle 10, a second flash evaporation kettle 20 and a third flash evaporation kettle 30 to be heated, evaporated and concentrated, then concentrated wastewater after the evaporation and concentration passes through a cooling crystallization device 40 to obtain mixed salt solid waste of calcium chloride and sodium chloride, mother liquor returns to the first flash evaporation kettle 10 to be evaporated and concentrated again, steam generated in the evaporation and concentration process is recycled after condensation, and in total, the salt in the high-salt wastewater is enriched and removed by utilizing the evaporation crystallization technology, so that the treatment of the high-salt wastewater is realized.
However, the above process cannot realize separate recovery of calcium chloride and sodium chloride, that is, the above process cannot separate and recover calcium chloride and sodium chloride to obtain calcium chloride salt with higher purity and sodium chloride salt with higher purity, respectively, and the salt obtained after the cooling crystallization is a mixed salt of calcium chloride and sodium chloride, which cannot be recycled, and needs to be treated as solid waste, resulting in additional increase of treatment cost for solid waste. Meanwhile, in the high-salt wastewater treatment process, a large amount of high-salt wastewater is required to be directly evaporated and crystallized, the process is required to be carried out at a high temperature, the whole system is required to be kept at a high temperature, and all three flash evaporation kettles are required to be heated by a large amount of steam, so that the heating steam consumption is huge, that is, the energy consumption of electric energy and the like is more, the operation energy consumption of high-salt wastewater treatment is greatly increased, the treatment cost is high, and the production cost of polysilicon is greatly increased.
Disclosure of Invention
Based on the above, it is necessary to separately recover the calcium chloride and the sodium chloride in the high-salt wastewater at present when the high-salt wastewater is treated, so that the obtained salts are mixed salts of the calcium chloride and the sodium chloride, and the obtained salts are required to be used as solid waste treatment, so that the treatment cost of the solid waste is additionally increased. The application provides a zero release system is retrieved in polycrystalline silicon production high salt waste water synthesis, can realize that calcium chloride and sodium chloride are retrieved alone respectively in the high salt waste water, and the purity is higher, avoid retrieving and obtain mixed salt and lead to extra increase to give up useless processing cost, changing waste into valuables, increase additional economic benefits, whole system can realize the whole recovery of high salt waste water, do not produce any waste water waste residue, zero release, realize the green clean processing of high salt waste water, simultaneously, utilize third flash distillation cauldron and second flash distillation cauldron evaporation concentration in-process exhaust vapor, and utilize heating third flash distillation cauldron and second flash distillation cauldron back exhaust vapor, can save energy such as electric energy that first flash distillation cauldron and second flash distillation cauldron heating are required, thereby can reduce the production and supply steam to consume outward, reduce high salt waste water treatment's operation energy consumption, greatly reduced high salt waste water processing cost, and then reduce polycrystalline silicon manufacturing cost.
The utility model provides a zero release system is retrieved in polycrystalline silicon production high salt waste water synthesis, includes 60 ℃ to 70 ℃ first flash tank, 90 ℃ to 100 ℃ second flash tank, 120 ℃ to 130 ℃ third flash tank, cooling crystallization device, centrifuge and electric heater, the waste water import of first flash tank is connected with high salt waste water pipeline, its concentrated export with the waste water import of second flash tank links to each other, the concentrated export of second flash tank links to each other with the import of centrifuge, the mother liquor export of centrifuge links to each other with the waste water import of third flash tank, the concentrated export of third flash tank links to each other with cooling crystallization device's import, cooling crystallization device's mother liquor export links to each other with the waste water import of first flash tank, electric heater's heating temperature is 150 ℃ to 170 ℃, and its export links to each other with the heating import of third flash tank, the heating export and/or the steam export of third flash tank link to each other with the heating import of second flash tank, the heating export and the steam export of second flash tank link to each other with the heating import of first flash tank.
The technical scheme that this application adopted can reach following beneficial effect:
according to the high-salt wastewater comprehensive recovery zero-emission system for the production of the polycrystalline silicon, high-salt wastewater generated in the production process of the polycrystalline silicon sequentially passes through a first flash evaporation kettle and a second flash evaporation kettle to be evaporated and concentrated, sodium chloride in the high-salt wastewater is saturated in solubility, and then the high-salt wastewater is introduced into a centrifugal machine, under the centrifugal separation effect of the centrifugal machine, saturated sodium chloride is subjected to crystallization separation to obtain sodium chloride with purity higher than 90%, then centrifugal mother liquor is introduced into a third flash evaporation kettle to be continuously evaporated and crystallized, and then the high-salt wastewater is introduced into a cooling crystallization device, so that calcium chloride in the centrifugal mother liquor is crystallized to be separated, the calcium chloride in the centrifugal mother liquor is separated, and the mother liquor after cooling crystallization is introduced into the first flash evaporation kettle to be mixed with the high-salt wastewater, and evaporated and concentrated along with the high-salt wastewater, so that the sodium chloride and the calcium chloride in the high-salt wastewater are completely separated and recovered, and the calcium chloride in the high-salt wastewater are separately recovered, the purity of the calcium chloride and the sodium chloride is higher, the waste is sold, the waste is prevented from being subjected to reinforcement treatment, the waste is increased, the waste water is completely produced, the waste water is not is completely recycled, and the waste water is clean, and the waste water is not polluted, and the waste water is completely is recycled.
Meanwhile, the steam discharged from the heating outlet and/or the steam outlet of the third flash evaporation kettle is introduced into the heating jacket of the second flash evaporation kettle and used for heating the second flash evaporation kettle, the steam discharged from the heating outlet and/or the steam outlet of the second flash evaporation kettle is introduced into the heating jacket of the first flash evaporation kettle and used for heating the first flash evaporation kettle, so that the heat in the steam is utilized, the first flash evaporation kettle and the second flash evaporation kettle do not need to be externally supplied with steam, the steam required by heating the first flash evaporation kettle and the second flash evaporation kettle can be saved, the externally supplied steam can be reduced, the steam discharged after heating the first flash evaporation kettle and the steam generated in the evaporation concentration process of the first flash evaporation kettle are heated to about 150 ℃ through an electric heater and used for heating the third flash evaporation kettle, compared with the steam obtained by heating and evaporating normal-temperature water to be 150 ℃, the steam at about 150 ℃ through heating the steam at about 60 ℃, the heat required by heating of the system can be reduced, the consumption of externally supplied steam is reduced, the electric energy consumption of the externally supplied steam is reduced, the energy consumption of the production is reduced, the energy consumption of the water is greatly reduced, the production cost is greatly reduced, the cost is high, and the production cost is greatly reduced, and the cost is high, and high in salt is and high, and the cost is low.
Drawings
FIG. 1 is a schematic diagram of a high-salt wastewater treatment system in a silicon material production process in the prior art;
FIG. 2 is a schematic diagram of a comprehensive recovery zero-emission system for high-salt wastewater from polysilicon production disclosed in an embodiment of the present application;
FIG. 3 is another schematic diagram of a comprehensive recovery zero-emission system for high-salinity wastewater from polysilicon production disclosed in an embodiment of the present application;
fig. 4 is a schematic diagram of a system for comprehensively recycling high-salt wastewater in polysilicon production according to an embodiment of the present application.
Description of the drawings: a first flash tank 10, a second flash tank 20, a third flash tank 30, and a cooling crystallization device 40;
a first flash tank 100, a second flash tank 200, a third flash tank 300, a cooling crystallization device 400, a centrifuge 500, an electric heater 600, and a high-salt wastewater pipe 700.
Description of the embodiments
In order that the present application may be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments that are illustrated in the appended drawings. Preferred embodiments of this application are given in the examples. This application may, however, be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "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. The terms "vertical," "horizontal," "left," "right," "top," "bottom," "top," and the like are used herein for illustrative purposes only and are not meant to be the only embodiment.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 2 to 4, the embodiment of the application discloses a comprehensive recovery zero-emission system for high-salt wastewater generated in polysilicon production, which comprises a first flash tank 100, a second flash tank 200, a third flash tank 300, a cooling crystallization device 400, a centrifuge 500 and an electric heater 600, wherein:
the first flash tank 100, the second flash tank 200 and the third flash tank 300 all have jacket structures for heating, and the temperature of heating steam in the jacket structures of the first flash tank 100 is about 90 ℃ so as to heat the high-salt wastewater in the first flash tank 100 to 60 ℃ to 70 ℃ for evaporation concentration, that is, the working temperature of the first flash tank 100 is 60 ℃ to 70 ℃; the temperature of the heating steam in the jacket structure of the second flash evaporation kettle 200 is about 120 ℃ so as to heat the high-salt wastewater in the second flash evaporation kettle 200 to 90 ℃ to 100 ℃ for evaporation concentration, namely, the working temperature of the second flash evaporation kettle 200 is 90 ℃ to 100 ℃; the heating steam temperature in the jacket structure of the third flash tank 300 is about 150 ℃ to heat the high-salt wastewater in the third flash tank 300 to 120 ℃ to 130 ℃ for evaporation concentration, that is, the working temperature of the third flash tank 300 is 120 ℃ to 130 ℃.
The waste water inlet of the first flash tank 100 is connected with a high-salt waste water pipeline 700 to enable the high-salt waste water generated in the production process of polysilicon to be introduced into the first flash tank 100, the high-salt waste water is evaporated and concentrated at the temperature of 60 ℃ to 70 ℃, the concentration outlet of the first flash tank 100 is connected with the waste water inlet of the second flash tank 200, the high-salt waste water obtained after the evaporation and concentration of the first flash tank 100 is introduced into the second flash tank 200 for continuous evaporation and concentration, in the second flash tank 200, the high-salt waste water is required to be evaporated and concentrated until sodium chloride reaches saturation, that is, the sodium chloride in the high-salt waste water obtained after the evaporation and concentration of the second flash tank 200 reaches the solubility saturation, and because the temperature of the second flash tank 200 is higher than that of the first flash tank 100, calcium chloride in the high-salt waste water can be continuously dissolved, that is, the dissolution saturation of calcium chloride is not reached, in general, after the evaporation and concentration of the second flash tank 200, the sodium chloride in the high-salt wastewater reaches the solubility saturation, the calcium chloride does not reach the solubility saturation, the concentration outlet of the second flash evaporation kettle 200 is connected with the inlet of the centrifugal machine 500, the high-salt wastewater after the evaporation concentration of the second flash evaporation kettle 200 is introduced into the centrifugal machine 500, as the sodium chloride reaches the solubility saturation, the saturated sodium chloride is crystallized and separated under the centrifugal separation action of the centrifugal machine 500 to obtain the sodium chloride with the purity higher than 90 percent, and the calcium chloride does not reach the solubility saturation, so that the calcium chloride in the high-salt wastewater is not crystallized and separated under the centrifugal action of the centrifugal machine 500, and remains in the centrifugal mother liquor, that is, the saturated sodium chloride in the high-salt wastewater is crystallized and separated after the high-salt wastewater is centrifuged by the centrifugal machine 500, and the unsaturated calcium chloride remains in the centrifugal mother liquor, and enters the next working procedure along with the centrifugal mother liquor.
The mother liquor outlet of the centrifuge 500 is connected with the waste water inlet of the third flash evaporation kettle 300, so that the centrifugal mother liquor is led into the third flash evaporation kettle 300 for evaporation and crystallization, at this time, most of the centrifugal mother liquor is calcium chloride, the content of the calcium chloride in the centrifugal mother liquor is about 60% after the centrifugal mother liquor is evaporated and concentrated by the third flash evaporation kettle 300, the calcium chloride reaches the dissolution saturation state, and part of the calcium chloride is in the melt precipitation state. The concentrated outlet of the third flash evaporation kettle 300 is connected with the inlet of the cooling crystallization device 400, the centrifugal mother liquor after the third flash evaporation kettle 300 is evaporated and concentrated is introduced into the cooling crystallization device 400, and the solubility of calcium chloride in the centrifugal mother liquor is reduced along with the reduction of the temperature of the centrifugal mother liquor, so that the calcium chloride in the centrifugal mother liquor is crystallized and separated, and the calcium chloride in the centrifugal mother liquor is separated. After the centrifugal mother liquor is cooled and crystallized, although the content of sodium chloride and calcium chloride in the mother liquor is low, a small amount of sodium chloride and calcium chloride exist, so that the mother liquor after cooling and crystallization cannot be discharged, the mother liquor outlet of the cooling and crystallizing device 400 is connected with the waste water inlet of the first flash kettle 100, so that the mother liquor after cooling and crystallization is introduced into the first flash kettle 100 to be mixed with high-salt waste water, and the high-salt waste water is subjected to evaporation concentration and separation again along with the high-salt waste water, so that the circulation is realized, the sodium chloride and the calcium chloride in the high-salt waste water are completely separated and recycled, waste water cannot be generated, and meanwhile, the water in the high-salt waste water is evaporated into water vapor for recycling.
Thus, firstly, the high-salt wastewater after the second flash evaporation kettle 200 is evaporated and concentrated is subjected to separation of sodium chloride by the centrifuge 500, then the centrifugal mother liquor is evaporated and concentrated by the third flash evaporation kettle 300, and then calcium chloride is separated by the cooling crystallization device 400, so that the calcium chloride and the sodium chloride in the high-salt wastewater are respectively and independently recovered, and the purity of the calcium chloride and the sodium chloride which are respectively separated and recovered is higher, the calcium chloride and the sodium chloride can be sold, waste materials are changed into valuable materials, and additional economic benefits are increased. In general, sodium chloride and calcium chloride in the high-salt wastewater are all separated and recycled, water in the high-salt wastewater is evaporated into water vapor for recycling, the whole system can realize the whole recycling of the high-salt wastewater, no waste water and waste residues are generated, zero emission is realized, and the green clean treatment of the high-salt wastewater is realized.
Since the third flash tank 300 needs to be heated with steam of about 150 ℃ to heat the high-salt wastewater in the third flash tank 300 to 120 ℃ to 130 ℃ for evaporation concentration, the third flash tank 300 needs to be provided with steam of about 150 ℃, specifically, the heating temperature of the electric heater 600 is 150 ℃ to 170 ℃, the outlet of the electric heater 600 is connected with the heating inlet of the third flash tank 300, the electric heater 600 is used for heating to obtain water vapor of about 150 ℃, then the water vapor of about 150 ℃ is introduced into the heating jacket of the third flash tank 300 for heating the third flash tank 300, the evaporation concentration temperature in the third flash tank 300 is heated to about 120 ℃ to 130 ℃ for evaporation concentration of the high-salt wastewater (the above centrifugal mother liquor) in the third flash tank 300, and the water vapor is discharged through the heating outlet of the third flash tank 300 after heating the third flash tank 300.
The temperature of the vapor discharged from the heating outlet of the third flash evaporation kettle 300 is about 120 ℃, if the vapor is directly cooled to be condensed water for recovery, the waste of heat in the vapor is caused, meanwhile, the third flash evaporation kettle 300 is heated by the vapor at about 150 ℃, the working temperature of the third flash evaporation kettle 300 is about 120 ℃ to 130 ℃, the vapor temperature discharged from the third flash evaporation kettle 300 is about 120 ℃, if the vapor is directly cooled to be condensed water for recovery, the waste of heat in the vapor is also caused, therefore, the heating outlet and/or the vapor outlet of the third flash evaporation kettle 300 are connected with the heating inlet of the second flash evaporation kettle 200, the vapor discharged from the heating outlet and/or the vapor outlet of the third flash evaporation kettle 300 is introduced into the heating jacket of the second flash evaporation kettle 200 for heating the second flash evaporation kettle 200, the vapor required by the vapor discharged from the heating outlet and/or the vapor outlet of the third flash evaporation kettle 300 is about 120 ℃, the heat consumption of the vapor required by the second flash evaporation kettle 200 is reduced, and the consumption of the vapor required by the second flash evaporation kettle is reduced, and the heat consumption of the vapor is reduced from the heating outlet and the second flash evaporation kettle 200 is reduced, and the like.
The second flash tank 200 is heated by the steam of about 120 ℃ and then discharged from the heating outlet of the second flash tank 200, the operating temperature of the second flash tank 200 is 90 ℃ to 100 ℃, so that the temperature of the steam discharged from the heating outlet of the second flash tank 200 is about 90 ℃, if the steam is directly cooled to condensate water for recovery, the waste of heat in the steam is caused, at the same time, the operating temperature of the second flash tank 200 is 90 ℃ to 100 ℃ by the steam of about 120 ℃, the temperature of the steam discharged from the second flash tank 200 by evaporation is about 90 ℃, if the steam is directly cooled to condensate water for recovery, the waste of heat in the steam is also caused, therefore, the heating outlet and/or steam outlet of the second flash tank 200 is connected with the heating inlet of the first flash tank 100, the steam discharged from the heating outlet and/or the steam outlet of the second flash tank 200 is introduced into the heating jacket of the first flash tank 100 to heat the first flash tank 100, and the steam discharged from the heating outlet and/or the steam outlet of the second flash tank 200 is about 90 ℃, and the temperature of the steam required by the first flash tank 100 is exactly about 90 ℃, so that the first flash tank 100 is heated by using the heat in the steam discharged from the heating outlet and/or the steam outlet of the second flash tank 200, and at this time, the first flash tank 100 does not need to be externally supplied with steam about 90 ℃, so that the steam required by the first flash tank 100 can be saved, the externally supplied steam can be reduced, and energy sources such as electric energy consumed by producing externally supplied steam can be reduced, and the energy consumption of electric energy and the like can be reduced.
As described above, the first flash tank 100 and the second flash tank 200 do not need external steam, but the third flash tank 300 needs the electric heater 600 to provide 150 ℃ steam, in general, the 150 ℃ steam is obtained by heating normal temperature water by the electric heater 600, the process needs to evaporate the normal temperature water to obtain 150 ℃ steam by heating by the electric heater 600, more heat is needed to be consumed, and more energy sources such as consumed electric energy are needed, therefore, in the application, the heating outlet and the steam outlet of the first flash tank 100 are connected with the inlet of the electric heater 600, after the first flash tank 100 is heated by the 90 ℃ steam, the temperature is reduced to about 60 ℃, the steam is discharged from the heating outlet of the first flash tank 100, meanwhile, high-salt wastewater is discharged from the steam outlet of the first flash tank 100 in the evaporation concentration process, the water vapor at about 60 ℃ is generated, the steam at about 60 ℃ is introduced into the electric heater 600 to be heated to about 150 ℃, and then the heating jacket is introduced into the heating tank 300 to the heating temperature, and the energy consumption of the water is greatly reduced by the heating jacket at about 150 ℃ after the heating, and the water at about 150 ℃ is further reduced by the heating energy sources such as the heating jacket. And the two parts of water vapor with the temperature of about 60 ℃ are introduced into the electric heater 600, so that a sufficient water source can be provided for the electric heater 600, the need of additional supplement of warm water is avoided, the water vapor with the temperature of about 60 ℃ is used for replacing the warm water for supplement, and the heat required by heating can be saved and reduced.
According to the high-salt wastewater comprehensive recovery zero-emission system for producing the polycrystalline silicon, disclosed by the embodiment of the application, high-salt wastewater generated in the production process of the polycrystalline silicon sequentially passes through the first flash evaporation kettle 100 and the second flash evaporation kettle 200 to be evaporated and concentrated, sodium chloride in the high-salt wastewater is saturated in solubility, and then is introduced into the centrifugal machine 500, under the centrifugal separation effect of the centrifugal machine 500, saturated sodium chloride is subjected to crystallization separation, so that sodium chloride with purity higher than 90% is obtained, then the centrifugal mother liquor is introduced into the third flash evaporation kettle 300 to be subjected to continuous evaporation and crystallization, and then is introduced into the cooling crystallization device 400, so that calcium chloride in the centrifugal mother liquor is crystallized to be separated, and the mother liquor after cooling crystallization is introduced into the first flash evaporation kettle 100 to be mixed with the high-salt wastewater, and is evaporated and concentrated again along with the high-salt wastewater, so that the circulation is realized, the sodium chloride in the high-salt wastewater and the calcium chloride are completely separated and recovered, and the saturated sodium chloride are respectively and independently recovered, the calcium chloride and the sodium chloride are separated respectively, the purity of the sodium chloride and the sodium chloride are higher can be obtained, the centrifugal mother liquor is introduced into the third flash evaporation kettle 300, the waste water is completely, the waste water is not polluted, the waste water is recovered, the waste water is completely is recovered, the waste water is purified, and the waste water is polluted, and the waste water is generated, and the waste water is purified, and the waste water is completely, and the waste water is not polluted, and the waste water is recycled.
Meanwhile, the steam discharged from the heating outlet and/or the steam outlet of the third flash tank 300 is introduced into the heating jacket of the second flash tank 200 for heating the second flash tank 200, the steam discharged from the heating outlet and/or the steam outlet of the second flash tank 200 is introduced into the heating jacket of the first flash tank 100 for heating the first flash tank 100, so that the heat in the steam is utilized, the first flash tank 100 and the second flash tank 200 do not need to be externally supplied with steam, the steam required for heating the first flash tank 100 and the second flash tank 200 can be saved, the externally supplied steam can be reduced, the steam discharged after heating the first flash tank 100 and the steam generated in the evaporation concentration process of the first flash tank 100 are heated to about 150 ℃ through the electric heater 600, the third flash tank 300 is heated, compared with the steam obtained by evaporating the normal-temperature water by heating to about 150 ℃, the steam at about 60 ℃, the heat required by the system heating is reduced, the externally supplied steam is reduced, the consumption of the water is greatly reduced, the energy consumption of the water is greatly reduced, the production cost is greatly reduced, and the waste water consumption is greatly reduced, and the production cost is greatly reduced.
Further, the heating outlet of the third flash tank 300 is connected to the heating inlet of the second flash tank 200, the heating outlet of the second flash tank 200 is connected to the heating inlet of the first flash tank 100, and the steam outlet of the third flash tank 300 and the steam outlet of the second flash tank 200 are also connected to the inlet of the electric heater 600. In the evaporation and concentration process of the high-salt wastewater in the second flash evaporation kettle 200, water vapor at about 90 ℃ is generated and discharged, and the water vapor is also introduced into the electric heater 600 for heating, and the water vapor at about 90 ℃ is used for heating to about 150 ℃, so that the heat required by heating can be further reduced, the consumed energy sources such as electric energy and the like are further reduced, the operation energy consumption of high-salt wastewater treatment is further reduced, and the high-salt wastewater treatment cost is greatly reduced. In the evaporation and concentration process of the centrifugal mother liquor in the third flash evaporation kettle 300, water vapor at about 120 ℃ is generated and discharged, and the water vapor is also introduced into the electric heater 600 for heating, and the water vapor at about 120 ℃ is used for heating to about 150 ℃, so that the heat required by heating can be further reduced, the consumed energy sources such as electric energy and the like are further reduced, the operation energy consumption of high-salt wastewater treatment is further reduced, and the high-salt wastewater treatment cost is greatly reduced.
In this application, the steam discharged from the heating outlet or the steam outlet of the third flash tank 300 is introduced into the heating jacket of the second flash tank 200, and is used for heating the second flash tank 200, so as to ensure that the second flash tank 200 is sufficiently heated, avoid that the second flash tank 200 is insufficiently heated due to insufficient steam, and prevent that the second flash tank 200 cannot reach the working temperature thereof, and based on this, optionally, the heating outlet and the steam outlet of the third flash tank 300 are both connected with the heating inlet of the second flash tank 200, so that the second flash tank 200 is heated by two parts of steam, so that the heating of the second flash tank 200 is sufficiently ensured, and further, the second flash tank 200 is sufficiently heated, and avoid that the second flash tank 200 cannot reach the working temperature thereof and affect the evaporation concentration result due to insufficient steam.
Similarly, the steam discharged from the heating outlet or steam outlet of the second flash tank 200 is introduced into the heating jacket of the first flash tank 100 to heat the first flash tank 100, so as to ensure that the first flash tank 100 is sufficiently heated, avoid insufficient heating of the first flash tank 100 due to insufficient steam, and prevent the first flash tank 100 from reaching the working temperature thereof, and based on this, optionally, the heating outlet and steam outlet of the second flash tank 200 are both connected with the heating inlet of the first flash tank 100, so that the first flash tank 100 is heated by two parts of steam, and the heating of the first flash tank 100 is sufficiently ensured, so that the first flash tank 100 is sufficiently heated, and avoid insufficient heating of the first flash tank 100 due to insufficient steam, and the first flash tank 100 is not reaching the working temperature thereof to affect the evaporation and concentration result.
Preferably, the steam outlet of the third flash evaporation kettle 300 is connected with the heating inlet of the second flash evaporation kettle 200, the steam outlet of the second flash evaporation kettle 200 is connected with the heating inlet of the first flash evaporation kettle 100, the heating outlet of the third flash evaporation kettle 300 and the heating outlet of the second flash evaporation kettle 200 are also connected with the inlet of the electric heater 600, the temperature of the water vapor at about 120 ℃ is reduced to about 90 ℃ after the second flash evaporation kettle 200 is heated, the water vapor is discharged from the heating outlet of the second flash evaporation kettle 200, and the water vapor at about 90 ℃ is used for heating to about 150 ℃, so that the heat required by heating can be further reduced, the consumed energy sources such as electric energy and the like can be further reduced, the operation energy consumption of high-salt wastewater treatment can be further reduced, and the high-salt wastewater treatment cost is greatly reduced. After the third flash evaporation kettle 300 is heated by the water vapor with the temperature of about 150 ℃, the temperature is reduced to about 120 ℃, the water vapor is discharged from a heating outlet of the third flash evaporation kettle 300, and the water vapor with the temperature of about 120 ℃ is used for heating to about 150 ℃, so that the heat required by heating can be further reduced, the consumed energy sources such as electric energy and the like can be further reduced, the operation energy consumption of high-salt wastewater treatment can be further reduced, and the high-salt wastewater treatment cost can be greatly reduced.
In a preferred embodiment, the steam outlet of the third flash tank 300 is connected to the heating inlet of the second flash tank 200, the steam outlet of the second flash tank 200 is connected to the heating inlet of the first flash tank 100, the heating outlet of the third flash tank 300 and the heating outlet of the second flash tank 200 are also connected to the inlet of the electric heater 600, and the steam outlet of the first flash tank 100 and the heating outlet of the first flash tank 100 are connected to the air cooler to recover condensed water. In this scheme, the steam with the heating outlet of the second flash evaporation kettle 200 and the heating outlet of the third flash evaporation kettle 300 having the discharge temperature higher than 60 ℃ is introduced into the electric heater 600 to heat for providing heating steam for the third flash evaporation kettle 300, and the steam with the lower discharge temperature of the steam outlet of the first flash evaporation kettle 100 and the heating outlet of the first flash evaporation kettle 100 is directly condensed to recover water resources, that is, the high-temperature steam is used for heating for providing heating steam for the third flash evaporation kettle 300, the low-temperature steam is condensed to recover, the classification treatment is realized, the mixing temperature is prevented from being reduced due to the mixing of the steam, the heating amount is larger, the heat required by heating is more, and the cascade utilization of the heat in the steam is realized.
As described above, the centrifugal mother liquor evaporated and concentrated by the third flash evaporation kettle 300 is introduced into the cooling crystallization device 400 to cool, crystallize and separate calcium chloride, and the temperature of the evaporated and concentrated by the third flash evaporation kettle 300 is 120 ℃ to 130 ℃, so that the temperature of the evaporated and concentrated centrifugal mother liquor of the third flash evaporation kettle 300 is also 120 ℃ to 130 ℃, if the evaporated and concentrated centrifugal mother liquor of the third flash evaporation kettle 300 is directly cooled, heat waste in the part of high-temperature centrifugal mother liquor is likely to be caused, and a large amount of cold energy is consumed by the cooling crystallization device 400 for cooling the part of high-temperature centrifugal mother liquor. Based on this, optionally, the system disclosed in the application may further include a heat exchanger, the concentrated outlet of the third flash tank 300 is connected to the shell side inlet of the heat exchanger, the shell side outlet of the heat exchanger is connected to the inlet of the cooling crystallization device 400, the heating outlet and the steam outlet of the first flash tank 100 are both connected to the tube side inlet of the heat exchanger, the tube side outlet of the heat exchanger is connected to the inlet of the electric heater 600, so that the centrifugal mother liquor at 120 ℃ to 130 ℃ exchanges heat with the steam (about 60 ℃) discharged from the heating outlet and the steam outlet of the first flash tank 100 in the heat exchanger, the heat in the centrifugal mother liquor is recovered, the waste is avoided, the temperature of the part of steam can be increased, the part of steam is heated to about 150 ℃ by the electric heater 600, the heat required by the heating of the electric heater 600 can be reduced, the consumed energy sources such as electric energy can be further reduced, the running energy consumption of high-salt wastewater treatment can be greatly reduced, and the cost of high-salt wastewater treatment can be greatly reduced.
In this application, let in cooling crystallization device 400 with the centrifugal mother liquor after the evaporation concentration of third flash distillation cauldron 300, with the calcium chloride separation in the centrifugal mother liquor, if with the whole direct cooling of centrifugal mother liquor after the evaporation concentration of third flash distillation cauldron 300, then can obtain massive calcium chloride crystal, be unfavorable for transportation and storage, follow-up still need smash, the extra process that increases, based on this, optionally, cooling crystallization device 400 is rotary drum crystallization slicer, let in rotary drum crystallization slicer with the centrifugal mother liquor after the evaporation concentration of third flash distillation cauldron 300, can obtain powdery calcium chloride crystal through rotary drum crystallization slicer, thereby need not to smash, be convenient for transport and store.
In order to ensure that the purity of the sodium chloride obtained by centrifuging the centrifuge 500 is higher, optionally, the working temperature of the centrifuge 500 is 90 ℃ to 100 ℃, so that the high-salt wastewater obtained by evaporating and concentrating the second flash evaporation kettle 200 is prevented from being saturated due to the fact that the temperature of the wastewater is reduced in the centrifuge 500, and is mixed in the sodium chloride due to the fact that the calcium chloride is separated under the action of the centrifuge 500, the high-salt wastewater obtained by evaporating and concentrating the second flash evaporation kettle 200 is ensured not to be mixed in the sodium chloride due to the fact that the working temperature of the centrifuge 500 is 90 ℃ to 100 ℃, so that the solubility of each component in the centrifuging mother liquor is ensured to be in a stable state, namely, the sodium chloride is saturated in solubility, and the calcium chloride is not saturated in dissolution, so that only the separation of the sodium chloride is ensured under the action of the centrifuge 500, and the purity of the sodium chloride obtained by centrifuging the centrifuge 500 is ensured to be higher.
In order to improve the evaporation and concentration efficiency of the first flash evaporation kettle 100, the second flash evaporation kettle 200 and the third flash evaporation kettle 300, optionally, the first flash evaporation kettle 100, the second flash evaporation kettle 200 and the third flash evaporation kettle 300 are all spray evaporators, the water vapor flowing upwards is evaporated to meet the high-salt wastewater sprayed downwards, the water vapor fully contacts with heat exchange, and the high-temperature water vapor can take away a part of water, so that the evaporation of the high-salt wastewater is accelerated, the evaporation and concentration efficiency of the first flash evaporation kettle 100, the second flash evaporation kettle 200 and the third flash evaporation kettle 300 is improved, and the evaporation and concentration rate is greatly improved.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples only represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the claims. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.
Claims (8)
1. The utility model provides a high salt waste water comprehensive recovery zero release system for polycrystalline silicon production, which is characterized in that, including 60 ℃ to 70 ℃ first flash kettle (100), 90 ℃ to 100 ℃ second flash kettle (200), 120 ℃ to 130 ℃ third flash kettle (300), cooling crystallization device (400), centrifuge (500) and electric heater (600), the waste water inlet of first flash kettle (100) is connected with high salt waste water pipeline (700), its concentrated export links to each other with the waste water inlet of second flash kettle (200), the concentrated export of second flash kettle (200) links to each other with the import of centrifuge (500), the mother liquor export of centrifuge (500) links to each other with the waste water inlet of third flash kettle (300), the concentrated export of third flash kettle (300) links to each other with the import of cooling crystallization device (400), the mother liquor export of cooling crystallization device (400) links to each other with the waste water inlet of first flash kettle (100), the heating temperature of electric heater (600) is 150 ℃ to 170 ℃, and its export links to each other with the heating kettle of third flash kettle (300) or the import of heating kettle (300) and the import of heating kettle (200), the heating outlet and the steam outlet of the first flash kettle (100) are connected with the inlet of the electric heater (600).
2. The system for comprehensively recycling high-salt wastewater and zero discharge of polysilicon production according to claim 1, wherein a heating outlet of the third flash evaporation kettle (300) is connected with a heating inlet of the second flash evaporation kettle (200), a heating outlet of the second flash evaporation kettle (200) is connected with a heating inlet of the first flash evaporation kettle (100), and a steam outlet of the third flash evaporation kettle (300) and a steam outlet of the second flash evaporation kettle (200) are also connected with an inlet of the electric heater (600).
3. The system for comprehensively recycling high-salt wastewater and zero discharge of polycrystalline silicon production according to claim 1, wherein a heating outlet and a steam outlet of the third flash evaporation kettle (300) are connected with a heating inlet of the second flash evaporation kettle (200), and a heating outlet and a steam outlet of the second flash evaporation kettle (200) are connected with a heating inlet of the first flash evaporation kettle (100).
4. The system for comprehensively recycling high-salt wastewater and zero discharge of polysilicon production according to claim 1, wherein a steam outlet of the third flash evaporation kettle (300) is connected with a heating inlet of the second flash evaporation kettle (200), a steam outlet of the second flash evaporation kettle (200) is connected with a heating inlet of the first flash evaporation kettle (100), and a heating outlet of the third flash evaporation kettle (300) and a heating outlet of the second flash evaporation kettle (200) are also connected with an inlet of the electric heater (600).
5. The comprehensive recovery zero-emission system for high-salt wastewater generated in polysilicon production according to claim 1, further comprising a heat exchanger, wherein a concentrated outlet of the third flash tank (300) is connected with a shell side inlet of the heat exchanger, a shell side outlet of the heat exchanger is connected with an inlet of the cooling crystallization device (400), a heating outlet and a steam outlet of the first flash tank (100) are both connected with a tube side inlet of the heat exchanger, and a tube side outlet of the heat exchanger is connected with an inlet of the electric heater (600).
6. The system for comprehensively recovering and zero-discharging high-salt wastewater generated in the production of polycrystalline silicon according to claim 1, wherein the cooling crystallization device (400) is a rotary drum type crystallization slicer.
7. The system for comprehensively recovering and zero-discharging high-salt wastewater generated in the production of polycrystalline silicon according to claim 1, wherein the working temperature of the centrifuge (500) is 90-100 ℃.
8. The system for comprehensively recovering and zero-discharging high-salt wastewater generated in the production of polycrystalline silicon according to claim 1, wherein the first flash tank (100), the second flash tank (200) and the third flash tank (300) are all spray evaporators.
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| CN116839009A (en) * | 2023-08-22 | 2023-10-03 | 山蓝(山东)节能环保科技有限公司 | Device and method for preparing steam by utilizing waste heat |
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| US20130048562A1 (en) * | 2011-08-31 | 2013-02-28 | Prochemtech International, Inc. | Treatment of gas well production wastewaters |
| CN208716886U (en) * | 2018-08-24 | 2019-04-09 | 石家庄鼎威化工设备工程有限公司 | A kind of high calcium high sodium waste-water evaporating |
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