CN113493213A - Process and equipment for recycling and zero discharge of wastewater containing sodium chloride and sodium sulfate - Google Patents
Process and equipment for recycling and zero discharge of wastewater containing sodium chloride and sodium sulfate Download PDFInfo
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- CN113493213A CN113493213A CN202110877646.8A CN202110877646A CN113493213A CN 113493213 A CN113493213 A CN 113493213A CN 202110877646 A CN202110877646 A CN 202110877646A CN 113493213 A CN113493213 A CN 113493213A
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- forced circulation
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 128
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 title claims abstract description 121
- 239000011780 sodium chloride Substances 0.000 title claims abstract description 56
- 229910052938 sodium sulfate Inorganic materials 0.000 title claims abstract description 56
- 235000011152 sodium sulphate Nutrition 0.000 title claims abstract description 56
- 239000002351 wastewater Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title claims abstract description 25
- 238000004064 recycling Methods 0.000 title claims abstract description 15
- 238000001704 evaporation Methods 0.000 claims abstract description 139
- 230000008020 evaporation Effects 0.000 claims abstract description 136
- 150000003839 salts Chemical group 0.000 claims abstract description 90
- 238000007710 freezing Methods 0.000 claims abstract description 87
- 230000008014 freezing Effects 0.000 claims abstract description 87
- 238000002425 crystallisation Methods 0.000 claims abstract description 22
- 230000008025 crystallization Effects 0.000 claims abstract description 22
- 239000012452 mother liquor Substances 0.000 claims description 95
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 92
- 239000012153 distilled water Substances 0.000 claims description 51
- 239000010446 mirabilite Substances 0.000 claims description 47
- 239000007788 liquid Substances 0.000 claims description 44
- 239000002562 thickening agent Substances 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 36
- 238000002844 melting Methods 0.000 claims description 23
- 230000008018 melting Effects 0.000 claims description 22
- 230000000694 effects Effects 0.000 claims description 21
- 239000013078 crystal Substances 0.000 claims description 20
- 238000010992 reflux Methods 0.000 claims description 20
- 238000000926 separation method Methods 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 17
- 229910002651 NO3 Inorganic materials 0.000 claims description 16
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 13
- 238000012546 transfer Methods 0.000 claims description 13
- 239000003507 refrigerant Substances 0.000 claims description 12
- 238000009835 boiling Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000007701 flash-distillation Methods 0.000 claims description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 230000009290 primary effect Effects 0.000 claims description 2
- 230000009291 secondary effect Effects 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 12
- 238000011161 development Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 10
- 239000011552 falling film Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000007832 Na2SO4 Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000012946 outsourcing Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
-
- 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
Abstract
The invention discloses a process and equipment for recycling and zero discharge of wastewater containing sodium chloride and sodium sulfate, which comprises a one-effect evaporation concentration unit, a nitrate-side double-effect evaporation sodium sulfate unit, a salt-side double-effect evaporation sodium chloride unit, a salt-side triple-effect evaporation miscellaneous salt unit, a nitrate-side triple-effect flash evaporation concentration unit and a freezing crystallization unit, wherein the process adopts two parallel-connection triple-effect evaporation technologies, namely secondary steam generated by the one-effect evaporation concentration is divided into two paths: the sodium chloride production method has the advantages that the occupied area of equipment is small, the investment is low, the production efficiency is high, the operation flexibility is large, the operation is a self-balancing process, the operation is simple, the automation degree is high, the process flow is simple and controllable, the sustainable development requirement is met, and the sodium chloride production method can be widely applied to the actual industrial production process.
Description
Technical Field
The invention relates to the technical field of treatment of wastewater containing sodium chloride and sodium sulfate, in particular to a process and equipment for recycling and zero discharge of wastewater containing sodium chloride and sodium sulfate.
Background
In recent years, with the rapid development of industry, the variety and the quantity of waste water are rapidly increased, the pollution to water bodies is more and more extensive and serious, the health and the safety of the water bodies are threatened, how to recycle industrial wastewater resources and realize zero discharge becomes a big problem which troubles industrial enterprises, in the industrial wastewater zero discharge process of salt chemical industry, chlor-alkali chemical industry, coal chemical industry, wet smelting, pharmacy and other industries, wastewater containing sodium chloride and sodium sulfate is often encountered, if the waste water directly enters an evaporative crystallization system to generate mixed salt, the waste water can not be recycled, but a large amount of solid waste can be generated, and the treatment is carried out qualitatively according to dangerous waste or solid waste, the treatment cost is high, the economy is poor, and the project progress of enterprises can be seriously influenced by the high cost, such as improper treatment of mixed salt, leaching and seepage when meeting water and risk of secondary pollution.
Generally, in the sodium chloride and sodium sulfate salt separation technology, there are two types, namely a hot method and a cold method, and the quality of sodium sulfate obtained by thermal crystallization cannot be guaranteed generally, so that in order to obtain a high-quality sodium sulfate product, a freezing crystallization technology is required, mirabilite is firstly separated out, and then hot melting recrystallization is carried out to obtain the sodium sulfate product.
The MVR technology can be selected as the evaporation unit, but the treatment units of the sodium chloride and sodium sulfate salt separation technology are more, and meanwhile, the MVR technology is not suitable for all the evaporation units, such as an impurity salt evaporation unit and a mirabilite hot melting evaporation unit, the MVR technology is selected with large investment, large occupied area, small operation flexibility and high maintenance cost of the compressor, if the MVR technology and a single-effect or multi-effect evaporation technology are selected, the system is complex, the operability is poor, the system is more complex by selecting the traditional multi-effect evaporation as the evaporation unit, and the energy-saving effect is better than the effect of the invention.
Disclosure of Invention
The invention mainly aims to provide a process and equipment for recycling and zero discharge of wastewater containing sodium chloride and sodium sulfate, which can effectively solve the problems in the background art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a process for recycling and zero emission of wastewater containing sodium chloride and sodium sulfate comprises the following steps:
s1, performing primary evaporation concentration treatment on the materials in a primary effect concentration unit;
s2, transferring the concentrated solution obtained in the step S1 to a nitro side triple-effect flash evaporation concentration unit for secondary flash evaporation concentration treatment;
s3, sending the concentrated solution obtained in the step S2 to a freezing crystallization unit for freezing crystallization treatment, separating out mirabilite crystals by freezing crystallization, and obtaining mirabilite solid salt and cold mother liquor by solid-liquid separation;
s4, sending the mirabilite obtained in the step S3 to a mirabilite side double-effect evaporation sodium sulfate unit for mirabilite hot melting and sodium sulfate evaporation treatment, centrifugally separating to separate out sodium sulfate product salt and centrifugal mother liquor, and periodically returning the centrifugal mother liquor to a freezing and crystallizing unit;
s5, sending the cold mother liquor obtained in the step S3 to a salt side double-effect evaporation sodium chloride unit for sodium chloride evaporation treatment, and centrifugally separating out sodium chloride product salt and centrifugal mother liquor; returning a part of the centrifugal mother liquor to continue evaporating the sodium chloride product;
and S6, sending the other part of the centrifugal mother liquor obtained in the step S5 to a salt side triple-effect miscellaneous salt evaporation unit for miscellaneous salt evaporation treatment, centrifugally separating and precipitating miscellaneous salts and high-concentration mother liquor, carrying out miscellaneous salt removal treatment, and periodically burning or removing high-concentration mother liquor.
Preferably, the step S1 specifically includes: send the material to distilled water preheater, first secondary steam preheater, bright steam condensate water preheater afterwards and get into first separator, the material is squeezed into first forced circulation heat exchanger by first forced circulation pump with the material and is carried out the heat transfer, and the material heaies up to the boiling point, gets back to at last and carries out the flash distillation in the first separator, so circulation, reaches the effect of evaporative concentration.
Preferably, the step S2 specifically includes: and (4) sending the concentrated solution generated in the step S1 to a fifth separator of a nitrate-side triple-effect flash evaporation concentration unit for flash evaporation, pumping the materials which are not subjected to flash evaporation into a fifth forced circulation heat exchanger for heat exchange by a fifth forced circulation pump, heating the materials to a boiling point, and finally returning the materials to the fifth separator for flash evaporation, so that circulation is carried out, and the effect of secondary evaporation concentration is achieved.
Preferably, the step S3 specifically includes: and (2) the concentrated material obtained in the step (S2) is firstly and secondly sent to a circulating water precooler and a cold mother liquor precooler of a freezing and crystallizing unit for precooling, the precooled material and the circulating cold material are pumped into a freezing heat exchanger for cold exchange by a freezing forced circulation pump, and finally the material and the circulating cold material enter the freezing crystallizer from a central downcomer for crystal growing, small-particle mirabilite flows upwards along with circulating liquid, large-particle mirabilite is deposited at the bottom of the freezing crystallizer, large-particle mirabilite crystal slurry is sent to a fourth thickener by a freezing discharge pump, the volume ratio of the solid is improved, then solid-liquid separation is carried out to obtain mirabilite solid and cold mother liquor, one part of the cold mother liquor returns to the freezing and crystallizing unit, and the other part of the cold mother liquor enters a salt side double-effect sodium chloride evaporation unit after passing through the cold mother liquor precooler and a second secondary steam preheater.
Preferably, the step S4 specifically includes: and (2) conveying the mirabilite obtained in the step (S3) to a mirabilite hot melting tank of a mirabilite side double-effect evaporation sodium sulfate unit through a screw conveyor, conveying the hot-melted material to a first thickener through a mirabilite hot melting pump, increasing the volume ratio of solids, then carrying out centrifugal separation to obtain a sodium sulfate product and saturated sodium sulfate mother liquor, continuously carrying out evaporation concentration on the saturated mother liquor to separate out sodium sulfate solids, conveying the separated sodium sulfate crystal slurry to the first thickener through a discharge pump, carrying out centrifugal separation together with sodium sulfate crystal slurry formed by mirabilite hot melting, circulating in the way, continuously carrying out evaporation crystallization, continuously enriching entrained miscellaneous salts, and returning a part of the centrifugal mother liquor to the freezing crystallization unit after concentrating to a certain multiple.
Preferably, the step S5 specifically includes: and (3) sending the cold mother liquor preheated in the step (S3) to a third separator of a salt side double-effect evaporation sodium chloride unit, then pumping the cold mother liquor into a third forced circulation pump to force a third circulation heat exchanger to exchange heat, returning the cold mother liquor to the third separator to carry out flash evaporation, circulating in the way, concentrating to a certain multiple, sending the separated sodium chloride crystal slurry to a third thickener, increasing the volume ratio of solids, then carrying out solid-liquid separation to obtain a sodium chloride product and a mother liquor, returning one part of the mother liquor to the salt side double-effect evaporation sodium chloride unit to continue evaporation, and directly returning the other part of the mother liquor to the salt side triple-effect evaporation miscellaneous salt unit.
Preferably, the step S6 includes: step S5, the centrifugal mother liquor enters a fourth separator of a salt side triple-effect evaporation miscellaneous salt unit for flash evaporation, then is injected into a fourth forced circulation heat exchanger for heat exchange through a fourth forced circulation pump, and returns to the fourth separator for flash evaporation, the circulation is carried out, after the centrifugal mother liquor is concentrated to a certain multiple, the separated miscellaneous salt crystal slurry is sent to a third thickener, the volume ratio of the solid is improved, then solid-liquid separation is carried out, miscellaneous salt and high-concentration mother liquor are obtained, miscellaneous salt is subjected to external treatment, part of the high-concentration mother liquor returns to the triple-effect evaporation miscellaneous salt unit for continuous evaporation, and part of the high-concentration mother liquor is periodically burnt or subjected to external treatment.
Preferably, the secondary steam generated in the step S1 has two directions, one part is used as a heat source of a sodium sulfate double-effect evaporation unit on a nitrate side, and the other part is used as a heat source of a sodium chloride double-effect evaporation unit on a salt side; the secondary steam generated in the step S4 is used as a heat source of a nitrate side triple-effect flash evaporation concentration unit; the secondary steam generated in the step S5 is divided to be used as a heat source of a salt side triple-effect evaporation miscellaneous salt unit; the secondary steam generated in the step S2 is used as a heat source for preheating cold mother liquor, the rest uncondensed secondary steam is used for condensation in a vacuum condenser, the secondary steam generated in the step S6 is used as a heat source for hot melting of mirabilite, and the rest uncondensed secondary steam is used for condensation in the vacuum condenser.
The equipment comprises a one-effect evaporation concentration unit, a saltpeter-side double-effect evaporation sodium sulfate unit, a salt-side double-effect evaporation sodium chloride unit, a salt-side triple-effect evaporation miscellaneous salt unit, a saltpeter-side triple-effect flash evaporation concentration unit and a freezing crystallization unit.
Preferably, the first-effect evaporation concentration unit comprises a raw material tank, a feed pump, a distilled water preheater, a first secondary steam preheater, a fresh steam condensate water tank, a fresh steam condensate water pump, a first separator, a first forced circulation pump, a first forced circulation heat exchanger and a first discharge pump, wherein the raw material tank is connected with the distilled water preheater through the feed pump, the distilled water preheater is connected with the fresh steam condensate water preheater through the first secondary steam preheater, the fresh steam condensate water preheater is connected with the fresh steam condensate water tank through the fresh steam condensate water pump, the fresh steam condensate water tank is connected with the first separator through the first forced circulation heat exchanger, and the output end of the first forced circulation heat exchanger is provided with the first forced circulation pump and the first discharge pump; the sodium sulfate unit for the two-effect evaporation at the nitrate side comprises a second forced circulation pump, a second discharge pump, a fourth mother liquor tank, a first mother liquor reflux pump, a sodium sulfate hot melting tank, a first distilled water buffer tank, a first distilled water transfer pump, a distilled water tank, a second forced circulation heat exchanger, a second separator, a first thickener and a first centrifugal machine, wherein the second forced circulation heat exchanger is connected with the second forced circulation pump through the second separator, the second separator is connected with the first thickener through the second discharge pump, the first centrifuge is arranged at the lower end of the first thickener, the first thickener is connected with the first mother liquor reflux pump through the fourth mother liquor tank, the first thickener is connected with the sodium sulfate tank through the sodium sulfate hot melting pump, the hot melting tank is connected with the first distilled water transfer pump through the first distilled water buffer tank, the first distilled water transferring pump is connected with a distilled water pump through a distilled water tank, and the distilled water tank is connected with a distilled water preheater through a distilled water pump; the salt side secondary-effect evaporation sodium chloride unit comprises a third forced circulation pump, a second mother liquid reflux pump, a third discharge pump, a first mother liquid tank, a first mother liquid discharge pump, a third forced circulation heat exchanger, a third separator, a second centrifuge and a second thickener, wherein the third forced circulation heat exchanger is connected with the third forced circulation pump through the third separator; the nitrate side triple-effect flash evaporation concentration unit comprises a fifth forced circulation pump, a fifth discharge pump, a fifth forced circulation heat exchanger, a fifth separator, a second secondary steam preheater and a steam-water separator, wherein the fifth forced circulation heat exchanger is connected with the second secondary steam preheater through the fifth separator, the second secondary steam preheater is connected with the steam-water separator, the fifth forced circulation pump is connected with the fifth forced circulation heat exchanger and the fifth separator, and the fifth discharge pump is arranged at the lower end of the fifth separator; the freezing and crystallizing unit comprises a circulating water precooler, a freezing forced circulation pump, a freezing crystallizer, a freezing heat exchanger, a freezing discharge pump, a fourth mother liquid reflux pump, a second mother liquid discharge pump, a fourth centrifuge, a third mother liquid tank, a cold mother liquid precooler, a freezing unit, a refrigerant lifting pump, a refrigerant storage tank, an auxiliary circulation pump and a fourth thickener, wherein the circulating water precooler and the cold mother liquid precooler are connected with the freezing heat exchanger through the freezing forced circulation pump, the freezing forced circulation pump is connected with the freezing crystallizer, one end of the freezing heat exchanger, far away from the freezing forced circulation pump, is connected with the freezing crystallizer in an inserting manner, the freezing heat exchanger is connected with the fourth thickener through the freezing discharge pump, the fourth thickener is connected with the third mother liquid tank through the fourth centrifuge, the lower end of the third mother liquid tank is provided with the fourth mother liquid reflux pump and the second mother liquid discharge pump, one end of the fourth mother liquid reflux pump, which is far away from the third mother liquid tank, is connected with a freezing heat exchanger, one end of the second mother liquid discharge pump, which is far away from the third mother liquid tank, is connected with a circulating water precooler, the fourth thickener is connected with a freezing crystallizer through a freezing discharge pump, one side of the freezing heat exchanger is connected with a refrigerating unit, the refrigerating unit is connected with a refrigerant storage tank through a refrigerant lifting pump, an auxiliary circulating pump is connected between the refrigerant storage tank and the freezing heat exchanger, and one end of the refrigerating unit is connected with the freezing heat exchanger; salt side triple effect evaporation miscellaneous salt unit: comprises a fourth forced circulation pump, a fourth discharge pump, a third mother liquor reflux pump, a second mother liquor tank, a second distilled water transfer pump, a second distilled water buffer tank, a fourth forced circulation heat exchanger, a fourth separator, a third centrifuge and a third thickener, the fourth forced circulation pump is connected with the fourth forced circulation heat exchanger through a fourth separator, the fourth separator is connected with a third thickener through a fourth discharge pump, the lower end of the third thickener is fixedly connected with a third centrifuge, the third centrifuge is connected with a third mother liquor reflux pump through a second mother liquor tank, the second distilled water transfer pump is connected with a fourth forced circulation heat exchanger through a second distilled water buffer tank, one end of the second distilled water transferring pump is connected with the distilled water tank, and one end of the second distilled water buffer tank is connected with the fifth forced circulation heat exchanger.
Compared with the prior art, the invention has the following beneficial effects:
1. the evaporation form of the step S1 of the invention can be flexibly used, and when the water quality of the wastewater can meet the conditions of falling film evaporation, falling film evaporation concentration can also be selected, so that the energy consumption of falling film evaporation is lower.
2. The step S2 of the present invention has three advantages: the first is to use the secondary steam of the nitrate side double effect as the heat source, and simultaneously, because the pressure of the triple effect is low, the effect of flash evaporation cooling can be achieved, not only can the concentration be further carried out, but also the material temperature can be reduced, the energy can be fully recovered, and simultaneously, the precooling load of the freezing crystallization system can be reduced.
3. The step S3 of the invention adopts a freezing crystallization technology, and because the freezing temperature is about-5 ℃, the solubility of sodium sulfate is about 0.7, and the solubility of sodium chloride is about 25, the influence of sodium sulfate on the quality of sodium chloride is greatly reduced.
4. In the step S4, a mirabilite hot-melting recrystallization technology is adopted, the mirabilite is dissolved by using the bound water of the mirabilite, the effect of washing the sodium sulfate is achieved, the quality of the sodium sulfate crystal salt obtained by centrifugal separation is high, and the purpose of recycling the wastewater is realized.
5. In step S5 of the invention, as the rear end is provided with a mixed salt evaporation unit, the external discharge amount of the sodium chloride mother liquor is determined by the content of the mixed salt, thereby ensuring the quality of the sodium chloride salt.
6. The step S6 of the present invention is a key unit for realizing zero emission of the whole system.
7. In the invention, a proper evaporation unit can be selected according to the water quality condition of the wastewater, such as: when the nitrate content is not high and the content of the miscellaneous salt is high, the salt side triple effect evaporation miscellaneous salt unit can be interchanged with the nitrate side evaporation sodium sulfate unit, and the like.
8. In the invention, the nitrate side double effect is communicated with the salt side double effect in pressure, and the nitrate side triple effect is communicated with the salt side triple effect in pressure, thus realizing self-distribution and self-balance of steam.
Drawings
FIG. 1 is a schematic diagram of the apparatus for recycling and zero-emission process of wastewater containing sodium chloride and sodium sulfate according to the implementation of the invention;
FIG. 2 is a data diagram of the overall process flow of the process for recycling and zero discharge of wastewater containing sodium chloride and sodium sulfate.
In the figure: a one-effect evaporation concentration unit: 1. a raw material tank; 2. a feed pump; 3. a distilled water preheater; 4. a fresh steam condensate pump; 5. a fresh steam condensate tank; 6. a first forced circulation pump; 7. a first discharge pump; 40. a first secondary steam preheater; 41. a fresh steam condensate preheater; 42. a first forced circulation heat exchanger; 43. a first separator;
nitrate side double effect evaporation sodium sulfate unit: 8. a second forced circulation pump; 9. a second discharge pump; 10. a fourth mother liquor tank; 11. a first mother liquor reflux pump; 12. a mirabilite hot melting pump; 13. a mirabilite hot melting tank; 14. a first distilled water buffer tank; 15. a first distilled water transfer pump; 16. a distilled water pump; 17. a distilled water tank; 44. a second forced circulation heat exchanger; 45. a second separator; 46. a first thickener; 47. a first centrifuge;
salt side double effect evaporation sodium chloride unit: 18. a third forced circulation pump; 19. a second mother liquor reflux pump; 20. a third discharge pump; 21. a first mother liquor tank; 22. a first mother liquor efflux pump; 48. a third forced circulation heat exchanger; 49. a third separator; 50. a second centrifuge; 51. a second thickener;
salt side triple effect evaporation miscellaneous salt unit: 23. a fourth forced circulation pump; 24. a fourth discharge pump; 25. a third mother liquor reflux pump; 26. a second mother liquor tank; 27. a second distilled water transfer pump; 28. a second distilled water buffer tank; 52. a fourth forced circulation heat exchanger; 53. a fourth separator; 54. a third centrifuge; 55. a third thickener;
nitrate side triple-effect flash evaporation concentration unit: 29. a fifth forced circulation pump; 30. a fifth discharge pump; 56. a fifth forced circulation heat exchanger; 57. a fifth separator; 58. a second secondary steam preheater; 59. a steam-water separator;
a freezing and crystallizing unit: 31. a circulating water precooler; 32. a refrigeration forced circulation pump; 33. a freezing crystallizer; 34. a freezing heat exchanger; 35. a freezing discharge pump; 36. a fourth mother liquor reflux pump; 37. a second mother liquor efflux pump; 38. a fourth centrifuge; 39. a third mother liquor tank; 60. a cold mother liquor precooler; 61. a refrigerating unit; 62. a refrigerant lift pump; 63. a refrigerant storage tank; 64. an auxiliary circulation pump; 65. and a fourth thickener.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The process for recycling and zero discharge of wastewater containing sodium chloride and sodium sulfate comprises the following steps:
s1, performing primary evaporation concentration treatment on the materials in a primary evaporation concentration unit, wherein the treatment capacity of the wastewater in the implementation is 10000kg/h (wherein the treatment capacity of Na2SO 4: 10%, NaCl: 5%, and other impurities: 0.2%), preheating the wastewater to about 110 ℃ in three stages, and then performing evaporation concentration in an evaporator, wherein the evaporation capacity of the unit is as follows: 3400kg/h, material transfer amount 6600k/h (wherein Na2SO 4: 15.15%, NaCl:7.58, other impurities: 0.30%), boiling point about 110 deg.C.
S2, transferring the concentrated solution obtained in the step S1 to a nitro-side triple-effect flash evaporation concentration unit for secondary flash evaporation concentration treatment, wherein the feeding amount of the wastewater in the implementation is 6600kg/h (wherein the Na2SO 4: 15.15%, NaCl: 7.57%, and other impurities: 0.3%), and the evaporation amount of the unit is as follows: 2300kg/h, a material transferring amount of 4300k/h (wherein Na2SO 4: 23.26NaCl: 11.63%, other impurities: 0.46%), a boiling point of about 75 deg.C.
S3, sending the concentrated solution obtained in the step S2 to a freezing and crystallizing unit for freezing and crystallizing, wherein the feeding amount of the wastewater in the implementation is 4300k/h (Na 2SO 4: 23.26, NaCl: 11.63% and other impurities: 0.46%), carrying out secondary cooling to about 40 ℃, then carrying out freezing and crystallizing to separate out mirabilite crystals, and carrying out solid-liquid separation to obtain 2300kg/h of mirabilite solid salt and 2000kg/h of cold mother liquor (wherein the Na2SO 4: 1.10%, NaCl: 24.00% and other impurities: 0.96%), wherein the freezing temperature is about-5 ℃.
And S4, conveying the mirabilite obtained in the step S3 to a mirabilite side double-effect evaporation sodium sulfate unit for mirabilite hot melting and sodium sulfate evaporation treatment, wherein the feeding amount of the mirabilite is 2300k/h (the mirabilite water content is about 5%), performing hot melting treatment, raising the temperature to about 45 ℃, then conveying the mirabilite into an evaporator for evaporation crystallization, the evaporation amount is 1250kg/h, performing thickening and centrifugal separation on crystal slurry to obtain a sodium sulfate product 1050kg/h (the sodium sulfate water content is about 8%), and returning the centrifugal mother liquor to the freezing crystallization unit periodically, and the boiling point is about 90 ℃.
S5, sending the cold mother liquor obtained in the step S3 to a salt side double-effect evaporation sodium chloride unit for sodium chloride evaporation treatment, wherein the feeding amount of the waste water in the implementation is 2000k/h (wherein the Na2SO4 is 1.10%, the NaCl is 24.00%, and other impurities are 0.96%), heating to about 60% after secondary preheating, then sending the waste water into an evaporator for evaporation crystallization, wherein the evaporation amount is 1100kg/h, thickening and centrifugally separating the crystal slurry to obtain 350kg/h (wherein the water content of the sodium chloride is about 5%) of a sodium chloride product and 550kg/h (wherein the Na2SO4 is 4.00%, the NaCl is 25.00%, and other impurities are 3.48%) of a centrifugal mother liquor, and the boiling point is about 95 ℃.
S6, conveying the centrifugal mother liquor obtained in the step S5 to a salt side triple-effect evaporation miscellaneous salt unit for carrying out evaporation miscellaneous salt treatment, wherein the feeding amount of the waste water is 550k/h (the Na2SO 4: 4.00%, the NaCl: 25.00% and the other impurities: 3.26%) in the implementation, the evaporation amount is 360kg/h, the centrifugal separation is carried out to separate out miscellaneous salt at 190kg/h (the water content of the miscellaneous salt is 5%), the miscellaneous salt is subjected to outsourcing treatment, and the high-concentration mother liquor is periodically incinerated or subjected to outsourcing treatment.
By combining the data analysis, when the contents of sodium chloride and miscellaneous salts are high and the content of sodium sulfate is low, the sodium sulfate unit for double-effect evaporation on the nitrate side and the miscellaneous salt unit for triple-effect evaporation on the salt side can be exchanged; if the contents of miscellaneous salt and sodium sulfate are high and the content of sodium chloride is low, the salt side double-effect evaporation sodium chloride unit and the salt side triple-effect evaporation miscellaneous salt unit can be exchanged.
The invention is a device for recycling and zero-discharge process of wastewater containing sodium chloride and sodium sulfate, preheating raw materials in a raw material tank 1 by a one-effect evaporation concentration unit, then introducing the raw materials into a first separator 43, then repeatedly flashing the materials by a first forced circulation pump 6, sending the concentrated solution to a fifth separator 57 of a nitrate-side three-effect flash evaporation concentration unit for flashing, evaporating to improve the concentration of sodium chloride and sodium sulfate, sending the concentrated materials into a circulating water precooler 31 and a cold mother liquor precooler 60 of a freezing crystallization unit for precooling, after precooling, introducing the concentrated materials into a freezing heat exchanger 34 for cold exchange by a freezing forced circulation pump 32, finally introducing the concentrated materials into a freezing crystallizer 33 for crystal growth, sending large-particle mirabilite crystal slurry into a fourth thickener 65 by a freezing discharge pump 35, improving the volume ratio of solids, then carrying out solid-liquid separation to obtain mirabilite solid and cold mother liquor, thereby changing the temperature of the solution, changing the solubility of sodium chloride and sodium sulfate, leading one salt to be precipitated in a saturated way, leading the other salt not to reach a saturated state, and realizing the purpose of recycling the wastewater; meanwhile, the high-concentration mother liquor with complex and various components is evaporated to generate miscellaneous salt by utilizing redundant secondary steam, and a zero-emission technology is realized.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A process for recycling and zero emission of wastewater containing sodium chloride and sodium sulfate is characterized by comprising the following steps:
s1, performing primary evaporation concentration treatment on the materials in a primary effect concentration unit;
s2, transferring the concentrated solution obtained in the step S1 to a nitro side triple-effect flash evaporation concentration unit for secondary flash evaporation concentration treatment;
s3, sending the concentrated solution obtained in the step S2 to a freezing crystallization unit for freezing crystallization treatment, separating out mirabilite crystals by freezing crystallization, and obtaining mirabilite solid salt and cold mother liquor by solid-liquid separation;
s4, sending the mirabilite obtained in the step S3 to a mirabilite side double-effect evaporation sodium sulfate unit for mirabilite hot melting and sodium sulfate evaporation treatment, centrifugally separating to separate out sodium sulfate product salt and centrifugal mother liquor, and periodically returning the centrifugal mother liquor to a freezing and crystallizing unit;
s5, sending the cold mother liquor obtained in the step S3 to a salt side double-effect evaporation sodium chloride unit for sodium chloride evaporation treatment, and centrifugally separating out sodium chloride product salt and centrifugal mother liquor; returning a part of the centrifugal mother liquor to continue evaporating the sodium chloride product;
and S6, sending the other part of the centrifugal mother liquor obtained in the step S5 to a salt side triple-effect miscellaneous salt evaporation unit for miscellaneous salt evaporation treatment, centrifugally separating and precipitating miscellaneous salts and high-concentration mother liquor, carrying out miscellaneous salt removal treatment, and periodically burning or removing high-concentration mother liquor.
2. The resource-based and zero-emission process of wastewater containing sodium chloride and sodium sulfate according to claim 1, wherein the step S1 specifically comprises: send the material to distilled water preheater, first secondary steam preheater, bright steam condensate water preheater afterwards and get into first separator, the material is squeezed into first forced circulation heat exchanger by first forced circulation pump with the material and is carried out the heat transfer, and the material heaies up to the boiling point, gets back to at last and carries out the flash distillation in the first separator, so circulation, reaches the effect of evaporative concentration.
3. The resource-based and zero-emission process of wastewater containing sodium chloride and sodium sulfate according to claim 1, wherein the step S2 specifically comprises: and (4) sending the concentrated solution generated in the step S1 to a fifth separator of a nitrate-side triple-effect flash evaporation concentration unit for flash evaporation, pumping the materials which are not subjected to flash evaporation into a fifth forced circulation heat exchanger for heat exchange by a fifth forced circulation pump, heating the materials to a boiling point, and finally returning the materials to the fifth separator for flash evaporation, so that circulation is carried out, and the effect of secondary evaporation concentration is achieved.
4. The resource-based and zero-emission process of wastewater containing sodium chloride and sodium sulfate according to claim 1, wherein the step S3 specifically comprises: and (2) the concentrated material obtained in the step (S2) is firstly and secondly sent to a circulating water precooler and a cold mother liquor precooler of a freezing and crystallizing unit for precooling, the precooled material and the circulating cold material are pumped into a freezing heat exchanger for cold exchange by a freezing forced circulation pump, and finally the material and the circulating cold material enter the freezing crystallizer from a central downcomer for crystal growing, small-particle mirabilite flows upwards along with circulating liquid, large-particle mirabilite is deposited at the bottom of the freezing crystallizer, large-particle mirabilite crystal slurry is sent to a fourth thickener by a freezing discharge pump, the volume ratio of the solid is improved, then solid-liquid separation is carried out to obtain mirabilite solid and cold mother liquor, one part of the cold mother liquor returns to the freezing and crystallizing unit, and the other part of the cold mother liquor enters a salt side double-effect sodium chloride evaporation unit after passing through the cold mother liquor precooler and a second secondary steam preheater.
5. The resource-based and zero-emission process of wastewater containing sodium chloride and sodium sulfate according to claim 1, wherein the step S4 specifically comprises: and (2) conveying the mirabilite obtained in the step (S3) to a mirabilite hot melting tank of a mirabilite side double-effect evaporation sodium sulfate unit through a screw conveyor, conveying the hot-melted material to a first thickener through a mirabilite hot melting pump, increasing the volume ratio of solids, then carrying out centrifugal separation to obtain a sodium sulfate product and saturated sodium sulfate mother liquor, continuously carrying out evaporation concentration on the saturated mother liquor to separate out sodium sulfate solids, conveying the separated sodium sulfate crystal slurry to the first thickener through a discharge pump, carrying out centrifugal separation together with sodium sulfate crystal slurry formed by mirabilite hot melting, circulating in the way, continuously carrying out evaporation crystallization, continuously enriching entrained miscellaneous salts, and returning a part of the centrifugal mother liquor to the freezing crystallization unit after concentrating to a certain multiple.
6. The resource-based and zero-emission process of wastewater containing sodium chloride and sodium sulfate according to claim 1, wherein the step S5 specifically comprises: and (3) sending the cold mother liquor preheated in the step (S3) to a third separator of a salt side double-effect evaporation sodium chloride unit, then pumping the cold mother liquor into a third forced circulation pump to force a third circulation heat exchanger to exchange heat, returning the cold mother liquor to the third separator to carry out flash evaporation, circulating in the way, concentrating to a certain multiple, sending the separated sodium chloride crystal slurry to a third thickener, increasing the volume ratio of solids, then carrying out solid-liquid separation to obtain a sodium chloride product and a mother liquor, returning one part of the mother liquor to the salt side double-effect evaporation sodium chloride unit to continue evaporation, and directly returning the other part of the mother liquor to the salt side triple-effect evaporation miscellaneous salt unit.
7. The recycling and zero-emission process of wastewater containing sodium chloride and sodium sulfate as claimed in claim 1, wherein the step S6 comprises: step S5, the centrifugal mother liquor enters a fourth separator of a salt side triple-effect evaporation miscellaneous salt unit for flash evaporation, then is injected into a fourth forced circulation heat exchanger for heat exchange through a fourth forced circulation pump, and returns to the fourth separator for flash evaporation, the circulation is carried out, after the centrifugal mother liquor is concentrated to a certain multiple, the separated miscellaneous salt crystal slurry is sent to a third thickener, the volume ratio of the solid is improved, then solid-liquid separation is carried out, miscellaneous salt and high-concentration mother liquor are obtained, miscellaneous salt is subjected to external treatment, part of the high-concentration mother liquor returns to the triple-effect evaporation miscellaneous salt unit for continuous evaporation, and part of the high-concentration mother liquor is periodically burnt or subjected to external treatment.
8. The process of claim 1, wherein the secondary steam generated in step S1 has two directions, one is used as a heat source of a sodium sulfate unit for the double-effect evaporation on the nitrate side, and the other is used as a heat source of a sodium chloride unit for the double-effect evaporation on the salt side; the secondary steam generated in the step S4 is used as a heat source of a nitrate side triple-effect flash evaporation concentration unit; the secondary steam generated in the step S5 is divided to be used as a heat source of a salt side triple-effect evaporation miscellaneous salt unit; the secondary steam generated in the step S2 is used as a heat source for preheating cold mother liquor, the rest uncondensed secondary steam is used for condensation in a vacuum condenser, the secondary steam generated in the step S6 is used as a heat source for hot melting of mirabilite, and the rest uncondensed secondary steam is used for condensation in the vacuum condenser.
9. The equipment for the sodium chloride and sodium sulfate-containing wastewater recycling and zero-emission process according to any one of claims 1 to 8, which comprises a single-effect evaporation concentration unit, a saltpeter-side double-effect evaporation sodium sulfate unit, a saltpeter-side double-effect evaporation sodium chloride unit, a saltpeter-side triple-effect evaporation miscellaneous salt unit, a saltpeter-side triple-effect flash evaporation concentration unit and a freezing crystallization unit.
10. The equipment for the resource and zero discharge process of the wastewater containing sodium chloride and sodium sulfate according to claim 9, it is characterized in that the first-effect evaporation concentration unit comprises a raw material tank, a feed pump, a distilled water preheater, a first secondary steam preheater, a fresh steam condensate water tank, a fresh steam condensate water pump, a first separator, a first forced circulation pump, a first forced circulation heat exchanger and a first discharge pump, the raw material tank is connected with a distilled water preheater through a feed pump, the distilled water preheater is connected with a fresh steam condensate water preheater through a first secondary steam preheater, the fresh steam condensate water preheater is connected with the fresh steam condensate water tank through a fresh steam condensate water pump, the fresh steam condensate water tank is connected with the first separator through the first forced circulation heat exchanger, the output end of the first forced circulation heat exchanger is provided with a first forced circulation pump and a first discharge pump; the sodium sulfate unit for the two-effect evaporation at the nitrate side comprises a second forced circulation pump, a second discharge pump, a fourth mother liquor tank, a first mother liquor reflux pump, a sodium sulfate hot melting tank, a first distilled water buffer tank, a first distilled water transfer pump, a distilled water tank, a second forced circulation heat exchanger, a second separator, a first thickener and a first centrifugal machine, wherein the second forced circulation heat exchanger is connected with the second forced circulation pump through the second separator, the second separator is connected with the first thickener through the second discharge pump, the first centrifuge is arranged at the lower end of the first thickener, the first thickener is connected with the first mother liquor reflux pump through the fourth mother liquor tank, the first thickener is connected with the sodium sulfate tank through the sodium sulfate hot melting pump, the hot melting tank is connected with the first distilled water transfer pump through the first distilled water buffer tank, the first distilled water transferring pump is connected with a distilled water pump through a distilled water tank, and the distilled water tank is connected with a distilled water preheater through a distilled water pump; the salt side secondary-effect evaporation sodium chloride unit comprises a third forced circulation pump, a second mother liquid reflux pump, a third discharge pump, a first mother liquid tank, a first mother liquid discharge pump, a third forced circulation heat exchanger, a third separator, a second centrifuge and a second thickener, wherein the third forced circulation heat exchanger is connected with the third forced circulation pump through the third separator; the nitrate side triple-effect flash evaporation concentration unit comprises a fifth forced circulation pump, a fifth discharge pump, a fifth forced circulation heat exchanger, a fifth separator, a second secondary steam preheater and a steam-water separator, wherein the fifth forced circulation heat exchanger is connected with the second secondary steam preheater through the fifth separator, the second secondary steam preheater is connected with the steam-water separator, the fifth forced circulation pump is connected with the fifth forced circulation heat exchanger and the fifth separator, and the fifth discharge pump is arranged at the lower end of the fifth separator; the freezing and crystallizing unit comprises a circulating water precooler, a freezing forced circulation pump, a freezing crystallizer, a freezing heat exchanger, a freezing discharge pump, a fourth mother liquid reflux pump, a second mother liquid discharge pump, a fourth centrifuge, a third mother liquid tank, a cold mother liquid precooler, a freezing unit, a refrigerant lifting pump, a refrigerant storage tank, an auxiliary circulation pump and a fourth thickener, wherein the circulating water precooler and the cold mother liquid precooler are connected with the freezing heat exchanger through the freezing forced circulation pump, the freezing forced circulation pump is connected with the freezing crystallizer, one end of the freezing heat exchanger, far away from the freezing forced circulation pump, is connected with the freezing crystallizer in an inserting manner, the freezing heat exchanger is connected with the fourth thickener through the freezing discharge pump, the fourth thickener is connected with the third mother liquid tank through the fourth centrifuge, the lower end of the third mother liquid tank is provided with the fourth mother liquid reflux pump and the second mother liquid discharge pump, one end of the fourth mother liquid reflux pump, which is far away from the third mother liquid tank, is connected with a freezing heat exchanger, one end of the second mother liquid discharge pump, which is far away from the third mother liquid tank, is connected with a circulating water precooler, the fourth thickener is connected with a freezing crystallizer through a freezing discharge pump, one side of the freezing heat exchanger is connected with a refrigerating unit, the refrigerating unit is connected with a refrigerant storage tank through a refrigerant lifting pump, an auxiliary circulating pump is connected between the refrigerant storage tank and the freezing heat exchanger, and one end of the refrigerating unit is connected with the freezing heat exchanger; salt side triple effect evaporation miscellaneous salt unit: comprises a fourth forced circulation pump, a fourth discharge pump, a third mother liquor reflux pump, a second mother liquor tank, a second distilled water transfer pump, a second distilled water buffer tank, a fourth forced circulation heat exchanger, a fourth separator, a third centrifuge and a third thickener, the fourth forced circulation pump is connected with the fourth forced circulation heat exchanger through a fourth separator, the fourth separator is connected with a third thickener through a fourth discharge pump, the lower end of the third thickener is fixedly connected with a third centrifuge, the third centrifuge is connected with a third mother liquor reflux pump through a second mother liquor tank, the second distilled water transfer pump is connected with a fourth forced circulation heat exchanger through a second distilled water buffer tank, one end of the second distilled water transferring pump is connected with the distilled water tank, and one end of the second distilled water buffer tank is connected with the fifth forced circulation heat exchanger.
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| CN114275837A (en) * | 2021-12-28 | 2022-04-05 | 江苏卓生源环保科技有限公司 | Freezing crystallization processing system |
| CN114394706A (en) * | 2021-12-07 | 2022-04-26 | 陕西航天机电环境工程设计院有限责任公司 | Evaporation-freezing coupling high-concentration salt wastewater treatment method and system based on heat pump |
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