CN112390271A - Multi-dimensional salt separation system and multi-dimensional salt separation method - Google Patents
Multi-dimensional salt separation system and multi-dimensional salt separation method Download PDFInfo
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- 150000003839 salts Chemical class 0.000 title claims abstract description 121
- 238000000926 separation method Methods 0.000 title claims abstract description 58
- 238000001728 nano-filtration Methods 0.000 claims abstract description 302
- 238000002425 crystallisation Methods 0.000 claims abstract description 176
- 230000008025 crystallization Effects 0.000 claims abstract description 176
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 156
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 106
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 85
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 85
- 239000011780 sodium chloride Substances 0.000 claims abstract description 78
- 238000007710 freezing Methods 0.000 claims abstract description 69
- 230000008014 freezing Effects 0.000 claims abstract description 69
- 238000001704 evaporation Methods 0.000 claims abstract description 47
- 230000008020 evaporation Effects 0.000 claims abstract description 45
- 230000008018 melting Effects 0.000 claims abstract description 16
- 238000002844 melting Methods 0.000 claims abstract description 16
- 239000012452 mother liquor Substances 0.000 claims description 37
- 239000002351 wastewater Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- 239000010446 mirabilite Substances 0.000 claims description 10
- 238000011084 recovery Methods 0.000 claims description 8
- 238000000108 ultra-filtration Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- 230000003750 conditioning effect Effects 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000006227 byproduct Substances 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 238000001223 reverse osmosis Methods 0.000 description 7
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 239000003245 coal Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 238000000909 electrodialysis Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 235000010333 potassium nitrate Nutrition 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011552 falling film Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
-
- 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
- C02F1/22—Treatment of water, waste water, or sewage by freezing
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- 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
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
Abstract
The invention discloses a multi-dimensional salt separation system and a multi-dimensional salt separation method. The multi-dimensional salt separation system comprises a softening and desiliconizing device, a sodium chloride evaporation and crystallization device, a sodium sulfate freezing and crystallization device, a melting and crystallization device and a multi-stage nanofiltration device; the multistage nanofiltration device comprises a first-stage nanofiltration unit, a second-stage nanofiltration unit and a third-stage nanofiltration unit, wherein the first-stage nanofiltration unit, the second-stage nanofiltration unit and the third-stage nanofiltration unit are sequentially communicated in series, the first-stage nanofiltration unit is communicated with the third-stage nanofiltration unit to enable first-stage nanofiltration concentrated water of the first-stage nanofiltration unit to enter the third-stage nanofiltration unit, third-stage nanofiltration produced water of the third-stage nanofiltration unit also enters the second-stage nanofiltration unit, the softening and desiliconizing device is connected with the first-stage nanofiltration unit, the second-stage nanofiltration unit is connected with the sodium chloride evaporation crystallization device, the sodium sulfate freezing crystallization device is connected with the third-stage nanofiltration. The multi-dimensional salt separation system has the advantages of good salt separation effect, high purity of byproduct salt and low impurity salt rate.
Description
Technical Field
The invention relates to the technical field of water treatment and environmental protection, in particular to a multi-dimensional salt separation system and a multi-dimensional salt separation method.
Background
The scale of the high-salt-content wastewater in China is continuously increased, the high-salt-content wastewater mainly comes from coal chemical industry plants, textile plants, soda plants, pesticide plants, petroleum and natural gas acquisition and processing and other processes, and if a large amount of high-salt-content wastewater is not treated and directly discharged, a large amount of water resources are wasted, and huge damage is caused to the environment. At present, a membrane method and a distillation method become main technologies of high-salt-content wastewater, an evaporation and freezing salt separation technology is mainly adopted for evaporation and salt separation, the salt separation effect of the method is poor, the quality of crystallized salt is easily influenced by water quality fluctuation, the quality of sodium chloride and sewage sodium sulfate as byproducts is low, the impurity salt rate is high, and the impurity salt rate is more than 25%.
Disclosure of Invention
Therefore, a multidimensional salt separation system and a multidimensional salt separation method which have good salt separation effect, high purity of byproduct salt and small impurity salt rate are needed.
A multi-dimensional salt separation system comprises a multi-stage nanofiltration device, a sodium chloride evaporation crystallization device, a sodium sulfate freezing crystallization device and a melting crystallization device; the sodium chloride evaporative crystallization device and the sodium sulfate freezing crystallization device are respectively connected with the multistage nanofiltration device, the secondary nanofiltration water produced by the multistage nanofiltration device enters the sodium chloride evaporative crystallization device, the secondary nanofiltration concentrated water of the multistage nanofiltration device enters the sodium sulfate freezing crystallization device, the melting crystallization device is connected with the sodium sulfate freezing crystallization device, the sodium sulfate freezing crystallization device freezes and crystallizes to obtain mirabilite, the mirabilite is melted and crystallized by the melting crystallization device to obtain anhydrous sodium sulfate, and part of nanofiltration concentrated water of sodium sulfate crystallization mother liquor of the sodium sulfate freezing crystallization device after nanofiltration enters the miscellaneous salt evaporative crystallization device.
In one embodiment, the multistage nanofiltration device comprises a first-stage nanofiltration unit, a second-stage nanofiltration unit and a third-stage nanofiltration unit, wherein the first-stage nanofiltration unit, the second-stage nanofiltration unit and the third-stage nanofiltration unit are sequentially communicated in series, the first-stage nanofiltration unit is further communicated with the third-stage nanofiltration unit so as to enable first-stage nanofiltration concentrated water of the first-stage nanofiltration unit to enter the third-stage nanofiltration unit, third-stage nanofiltration concentrated water of the third-stage nanofiltration unit also enters the second-stage nanofiltration unit, the softening and desiliconization device is connected with the first-stage nanofiltration unit, the second-stage nanofiltration unit is connected with the sodium chloride evaporative crystallization device, the sodium sulfate frozen crystallization device is connected with the third-stage nanofiltration unit, and the melting crystallization device is connected with the sodium sulfate frozen crystallization device.
In one embodiment, the multidimensional salt separation system further comprises a high-pressure nanofiltration device, the high-pressure nanofiltration device is connected with the sodium sulfate freezing and crystallizing device, the high-pressure nanofiltration device is further connected with the primary nanofiltration unit, sodium sulfate crystallization mother liquor of the sodium sulfate freezing and crystallizing device enters the high-pressure nanofiltration device for nanofiltration, part of nanofiltration concentrated water of the high-pressure nanofiltration device enters the mixed salt evaporation and crystallization device, and nanofiltration produced water of the high-pressure nanofiltration device enters the primary nanofiltration unit.
In one embodiment, the multidimensional salt separation system further comprises a mixed salt evaporative crystallization device, the mixed salt evaporative crystallization device is connected with the sodium chloride evaporative crystallization device, and the mixed salt evaporative crystallization device is used for receiving part of sodium chloride crystallization mother liquor from the sodium chloride evaporative crystallization device and evaporating mixed salt.
In one embodiment, the sodium chloride evaporative crystallization device is further connected with the sodium sulfate freezing crystallization device, and part of sodium chloride crystallization mother liquor of the sodium chloride evaporative crystallization device enters the sodium sulfate freezing crystallization device for freezing crystallization.
In one embodiment, the multidimensional salt separation system further comprises a first concentration device connected in series between the secondary nanofiltration unit and the sodium chloride evaporative crystallization device.
In one embodiment, the multidimensional salt separation system further comprises a second concentration device connected in series between the three-stage nanofiltration unit and the sodium sulfate freezing and crystallizing device.
In one embodiment, the multidimensional salt separation system further comprises a high-pressure nanofiltration device, the high-pressure nanofiltration device is connected in series between the sodium sulfate freezing and crystallizing device and the mixed salt evaporation device, the high-pressure nanofiltration device is further connected with the primary nanofiltration unit, sodium sulfate crystallization mother liquor of the sodium sulfate freezing and crystallizing device enters the high-pressure nanofiltration device for nanofiltration, part of nanofiltration concentrated water of the high-pressure nanofiltration device enters the mixed salt evaporation and crystallization device, and nanofiltration produced water of the high-pressure nanofiltration device enters the primary nanofiltration unit for connection.
In one embodiment, the high-pressure nanofiltration device is further connected with the second concentration device, and part of nanofiltration concentrated water of the high-pressure nanofiltration device also enters the second concentration device.
In one embodiment, the multidimensional salt separation system further comprises a regulating tank which is connected to the front end of the softening and desiliconizing device.
In one embodiment, the softening and silicon-removing device comprises one or more of a silicon-removing high-density tank, a V-shaped filter tank and an ultrafiltration device.
In one embodiment, the first-stage nanofiltration unit is a high-efficiency He nanofiltration unit;
and/or the secondary nanofiltration unit is a high-interception Hr nanofiltration unit;
and/or the third-stage nanofiltration unit is a high-recovery Hc nanofiltration unit.
A multi-dimensional salt separation method comprises the following steps:
the method comprises the following steps that high-salinity wastewater is softened and desilicated by a softening desiliconization device and then enters a multi-stage nanofiltration device for nanofiltration treatment, first-stage nanofiltration concentrated water of a first-stage nanofiltration unit enters a third-stage nanofiltration unit, first-stage nanofiltration produced water of the first-stage nanofiltration unit enters a second-stage nanofiltration unit, second-stage nanofiltration concentrated water of the second-stage nanofiltration unit enters the third-stage nanofiltration unit, second-stage nanofiltration produced water of the second-stage nanofiltration unit enters a sodium chloride evaporation crystallization device for evaporation and crystallization to obtain sodium chloride, second-stage nanofiltration concentrated water of the third-stage nanofiltration unit enters a sodium sulfate freezing crystallization device for freezing and crystallization to obtain sodium sulfate, and second-stage nanofiltration produced water of the third-stage nanofiltration unit flows back.
In one embodiment, the multi-dimensional salt separation method further comprises the following steps:
part of sodium chloride crystals in the sodium chloride evaporative crystallization device enter a mixed salt evaporative crystallization device and are evaporated and crystallized to obtain mixed salt;
and/or, part of sodium chloride crystallization mother liquor of the sodium chloride evaporation crystallization device enters the sodium sulfate freezing crystallization device to be frozen and crystallized to obtain sodium sulfate;
and/or part of nanofiltration concentrated water of sodium sulfate crystallization mother liquor of the sodium sulfate freezing crystallization device after nanofiltration by the high-pressure nanofiltration device enters the mixed salt evaporation crystallization device and is evaporated and crystallized to obtain mixed salt, the other part of nanofiltration concentrated water flows back to the second concentration device, and nanofiltration produced water of the high-pressure nanofiltration device flows back to the first-stage nanofiltration unit.
In one embodiment, the multi-dimensional salt separation method further comprises the following steps: and the sodium sulfate freezing and crystallizing device freezes and crystallizes the obtained mirabilite, and the sodium sulfate is melted and crystallized by the melting and crystallizing device to obtain anhydrous sodium sulfate.
The multistage nanofiltration device provided by the invention comprises three groups of nanofiltration units, so that the recovery rate is ensured, the sulfate radical is high in retention rate, chloride ions and the sulfate radical are better separated, and the purity of byproduct salt is ensured.
Compared with the prior art, the invention creatively and organically combines 3 methods of evaporation, freezing and high-pressure nanofiltration, and aims at the NaCl solution and Na separated by a multi-stage nanofiltration device system2SO4And (3) producing high-purity sodium chloride from the solution through an evaporation crystallization device, and producing high-purity anhydrous sodium sulfate through freezing and melting crystallization. Wherein, part of evaporation mother liquor flows back to a freezing crystallization device to improve the output of mirabilite, sodium sulfate crystallization mother liquor is subjected to secondary separation by high-pressure nanofiltration, NaCl in the sodium sulfate crystallization mother liquor is recovered, and Na is treated2SO4Concentrating and refluxing, and leaving a small amount of sodium sulfate crystallization mother liquor and chlorineDischarging the sodium chloride crystallization mother liquor to a mixed salt evaporation crystallization device to produce mixed salt. The multidimensional salt separation system greatly improves the quality of sodium chloride (the purity of the sodium chloride is more than 97%) and the quality of anhydrous sodium sulfate (the purity of the anhydrous sodium sulfate is more than 97%) by flexibly combining evaporation, refrigeration and high-pressure nanofiltration, and reduces the impurity salt rate which is less than 15%.
Drawings
FIG. 1 is a schematic view of a multi-dimensional salt separation system according to an embodiment of the present invention;
fig. 2 is a schematic view of a multi-stage nanofiltration device of the multi-dimensional salt separation system shown in fig. 1.
Description of the reference numerals
10. A multi-dimensional salt separation system; 100. a multi-stage nanofiltration device; 110. a first-stage nanofiltration unit; 120. a secondary nanofiltration unit; 130. a third nanofiltration unit; 200. a softening and silicon-removing device; 300. a sodium chloride evaporation crystallization device; 400. a sodium sulfate freezing and crystallizing device; 500. a melt crystallization device; 600. a miscellaneous salt evaporation crystallization device; 700. a first concentration device; 800. a second concentration device; 900. a high pressure nanofiltration device; 1000. and (4) a regulating reservoir.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
In the description of the present invention, it should be understood that the terms used in the present invention are used in the description of the present invention, and it should be understood that the directions or positional relationships indicated by the terms "center", "upper", "lower", "bottom", "inner", "outer", etc. in the present invention are based on the directions or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element referred to 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.
It should be understood that the terms "first", "second", etc. are used herein to describe various information, but the information should not be limited to these terms, which are only used to distinguish one type of information from another. For example, "first" information may also be referred to as "second" information, and similarly, "second" information may also be referred to as "first" information, without departing from the scope of the present invention.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected" and "connected" are to be interpreted broadly, e.g., as being fixed or detachable or integrally connected; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening elements, or they may be in communication within two elements, i.e., when an element is referred to as being "secured to" another element, it may 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 specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
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 invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1 and 2 together, one embodiment of the present invention provides a multi-dimensional salt separation system 10.
A multi-dimensional salt separation system 10 comprises a softening and desiliconizing device 200, a sodium chloride evaporation and crystallization device 300, a sodium sulfate freezing and crystallization device 400, a melting and crystallization device 500 and a multi-stage nanofiltration device 100.
Referring to fig. 2, the multi-stage nanofiltration device 100 includes a first nanofiltration unit 110, a second nanofiltration unit 120, and a third nanofiltration unit 130. The first-stage nanofiltration unit 110, the second-stage nanofiltration unit 120 and the third-stage nanofiltration unit 130 are sequentially communicated in series, the first-stage nanofiltration unit 110 is further communicated with the third-stage nanofiltration unit 130 to enable first-stage nanofiltration concentrated water of the first-stage nanofiltration unit 110 to enter the third-stage nanofiltration unit 130, third-stage nanofiltration concentrated water of the third-stage nanofiltration unit 130 also enters the second-stage nanofiltration unit 120, second-stage nanofiltration concentrated water of the second-stage nanofiltration unit 120 is used for entering the sodium chloride evaporative crystallization device 300, and third-stage nanofiltration concentrated water of the third-stage nanofiltration unit 130 is used for entering the sodium sulfate freezing crystallization device.
The multistage nanofiltration device 100 comprises three groups of nanofiltration units, ensures the recovery rate, has high retention rate on sulfate radicals, and better separates chloride ions from the sulfate radicals to ensure the purity of byproduct salt.
The softening and desiliconizing device 200 is connected with the first-stage nanofiltration unit 110, the second-stage nanofiltration unit 120 is connected with the sodium chloride evaporative crystallization device 300, the sodium sulfate freezing crystallization device 400 is connected with the third-stage nanofiltration unit 130, and the melting crystallization device 500 is connected with the sodium sulfate freezing crystallization device 400.
In one particular embodiment, the first stage nanofiltration unit 110 is a high efficiency He nanofiltration unit.
In one particular embodiment, the secondary nanofiltration unit 120 is a high rejection Hr nanofiltration unit.
In one particular embodiment, tertiary nanofiltration unit 130 is a high recovery Hc nanofiltration unit.
In one embodiment, the multi-dimensional salt separation system 10 further comprises a miscellaneous salt evaporative crystallization device 600. The mixed salt evaporative crystallization device 600 is connected with the sodium chloride evaporative crystallization device 300, and the mixed salt evaporative crystallization device 600 is used for receiving part of sodium chloride crystallization mother liquor from the sodium chloride evaporative crystallization device 300 and evaporating mixed salt. Preferably, the miscellaneous salt evaporative crystallization apparatus 600 may be a single effect evaporative system.
In one embodiment, the sodium chloride evaporative crystallization device 300 is further connected to the sodium sulfate freezing crystallization device 400, and a part of the sodium chloride crystallization mother liquor of the sodium chloride evaporative crystallization device 300 enters the sodium sulfate freezing crystallization device 400 for freezing crystallization.
In one embodiment, the multi-dimensional salt separation system 10 further includes a first concentration device 700. The first concentration device 700 is connected in series between the secondary nanofiltration unit 120 and the sodium chloride evaporative crystallization device 300. The first concentration device 700 may be a high pressure reverse osmosis concentration device.
Preferably, the first concentration device 700 may be one or more of reverse osmosis, high pressure reverse osmosis, DTRO, electrodialysis, and MVR.
In one embodiment, the multi-dimensional salt separation system 10 further includes a second concentration device 800. The second concentration device 800 is connected in series between the three-stage nanofiltration unit 130 and the sodium sulfate freezing and crystallizing device 400. The second concentration device 800 may be a reverse osmosis concentration device.
Preferably, the second concentration device 800 may be one or more of reverse osmosis, high pressure reverse osmosis, DTRO, electrodialysis, and MVR.
Preferably, the sodium chloride evaporative crystallization apparatus 300 may be one or more selected from the group consisting of a falling film evaporator, a rising film evaporator, TVR, MVR, single effect evaporation, and multiple effect evaporation.
The sodium sulfate freezing and crystallizing device 400 can be any one or more selected from OSLO evaporative crystallizer, DTB evaporative crystallizer, FC evaporative crystallizer, multi-effect evaporative crystallizer, and the like.
In one particular embodiment, the multi-dimensional salt separation system 10 further includes a high pressure nanofiltration device 900. The high-pressure nanofiltration device 900 is connected in series between the sodium sulfate freezing crystallization device 400 and the mixed salt evaporation device, the high-pressure nanofiltration device 900 is also connected with the primary nanofiltration unit 110, sodium sulfate crystallization mother liquor of the sodium sulfate freezing crystallization device 400 enters the high-pressure nanofiltration device 900 for nanofiltration, part of nanofiltration concentrated water of the high-pressure nanofiltration device 900 enters the mixed salt evaporation crystallization device 600, and nanofiltration produced water of the high-pressure nanofiltration device 900 enters the primary nanofiltration unit 110 for connection.
In one embodiment, the high-pressure nanofiltration device 900 is further connected to the second concentration device 800, and a part of the nanofiltration concentrated water of the high-pressure nanofiltration device 900 is further introduced into the second concentration device 800.
In one embodiment, the multi-dimensional salt separation system 10 further comprises a conditioning tank 1000, and the conditioning tank 1000 is connected to the front end of the softening and desiliconizing device 200.
In one embodiment, the softening and silicon-removing device 200 comprises one or more of a silicon-removing high-density tank, a V-shaped filter tank and an ultrafiltration device.
A multi-dimensional salt separation method comprises the following steps:
the high-salinity wastewater is softened and desilicated by a softening desiliconization device 200 and then enters a multi-stage nanofiltration device 100 for nanofiltration treatment, first-stage nanofiltration concentrated water of a first-stage nanofiltration unit 110 enters a third-stage nanofiltration unit 130, first-stage nanofiltration produced water of the first-stage nanofiltration unit 110 enters a second-stage nanofiltration unit 120, second-stage nanofiltration concentrated water of the second-stage nanofiltration unit 120 enters the third-stage nanofiltration unit 130, second-stage nanofiltration produced water of the second-stage nanofiltration unit 120 enters a sodium chloride evaporation crystallization device 300 for evaporation crystallization to obtain sodium chloride, second-stage nanofiltration concentrated water of the third-stage nanofiltration unit 130 enters a sodium sulfate freezing crystallization device 400 for freezing crystallization to obtain sodium sulfate, and second-stage nanofiltration produced water of the third-stage nanofiltration unit 130 flows back to.
In one embodiment, the multi-dimensional salt separation method further comprises the following steps:
part of the sodium chloride crystals in the sodium chloride evaporative crystallization device 300 enter the miscellaneous salt evaporative crystallization device 600 and are evaporated and crystallized to obtain miscellaneous salts.
In one embodiment, a part of the mother liquor of sodium chloride crystallization in the sodium chloride evaporative crystallization device 300 enters the sodium sulfate freezing crystallization device 400 for freezing crystallization to obtain sodium sulfate.
In a specific embodiment, a part of nanofiltration concentrated water of the sodium sulfate crystallization mother liquor of the sodium sulfate freezing crystallization device 400 after nanofiltration by the high-pressure nanofiltration device 900 enters the mixed salt evaporation crystallization device 600 and is evaporated and crystallized to obtain mixed salt, another part of nanofiltration concentrated water flows back to the second concentration device 800, and nanofiltration produced water of the high-pressure nanofiltration device 900 flows back to the first-stage nanofiltration unit 110.
In one embodiment, the multi-dimensional salt separation method further comprises the following steps: the sodium sulfate freezing and crystallizing device 400 freezes and crystallizes to obtain mirabilite, and the mirabilite is melted and crystallized by the melting and crystallizing device 500 to obtain anhydrous sodium sulfate.
Compared with the prior art, the invention innovatively and organically combines 3 methods of evaporation, freezing and high-pressure nanofiltration, and aims at the NaCl solution and Na separated by the multi-stage nanofiltration device 100 system2SO4And (3) producing high-purity sodium chloride from the solution through an evaporation crystallization device, and producing high-purity anhydrous sodium sulfate through freezing and melting crystallization. Wherein, part of evaporation mother liquor flows back to a freezing crystallization device to improve the output of mirabilite, sodium sulfate crystallization mother liquor is subjected to secondary separation by high-pressure nanofiltration, NaCl in the sodium sulfate crystallization mother liquor is recovered, and Na is treated2SO4Concentrating and refluxing, and discharging a small amount of residual sodium sulfate crystallization mother liquor and sodium chloride crystallization mother liquor to a mixed salt evaporation crystallization device 600 to produce mixed salt. The multidimensional salt separation system 10 greatly improves the quality of sodium chloride (the purity of the sodium chloride is more than 97%) and the quality of anhydrous sodium sulfate (the purity of the anhydrous sodium sulfate is more than 97%) by flexibly combining evaporation, refrigeration and high-pressure nanofiltration, and reduces the impurity salt rate which is less than 15%.
Example 1
The embodiment provides a multi-dimensional salt separation method.
The multidimensional salt separation method is used for treating high-salt-content wastewater in certain coal chemical industry.
The coal chemical industry high salt content waste water is detected, and the water quality condition is as follows: pH: 6-8, COD: 110.0mg/L, TOC: 25.0mg/L, Ca2+：0.6mg/L，Mg2+：0.4mg/L，NH4 +：3.0mg/L，Na+：6692.5mg/L，K+：131.5mg/L，Cl-：4970.6mg/L，SO4 2-：7271.4mg/L，NO3 -：122.1mg/L，HCO3-：76.5mg/L，CO3 2-：4.0mg/L，SiO2：31.7mg/L，TDS：19304.2mg/L。
The coal chemical industry high-salt-content wastewater is recycled by a multi-dimensional salt separation method, and comprises the following steps:
(1) the high-salt-content wastewater firstly enters an adjusting tank 1000, and the water inlet flow of the adjusting tank 1000 is 97.5m3The residence time was 4 h.
(2) The wastewater with high salt content enters the softening and desiliconization device 200 after being regulated by the regulating reservoir 1000, the softening and desiliconization device 200 in the embodiment comprises a desiliconization high-density pool, a V-shaped filter pool and an ultrafiltration device, and SiO in the wastewater with high salt content is treated by the softening and desiliconization device 2002Reducing the concentration to 10.0mg/L, and filtering by a V-shaped filter tank and an ultrafiltration device to reduce the SDI of the high-salt wastewater to below 3 and reduce the turbidity to below 1 NTU.
(3) After being treated by the softening and desiliconizing device 200, the wastewater with high salt content enters the multi-stage nanofiltration device 100. The recovery rate of the first-stage nanofiltration unit 110 of the multi-stage nanofiltration device 100 is 73%, the recovery rate of the second-stage nanofiltration unit 120 is 84%, the recovery rate of the third-stage nanofiltration unit 130 is 70%, and the water quality of the multi-stage nanofiltration device 100 is as shown in table 1 below.
TABLE 1
As shown in the above table, the water produced by the secondary nanofiltration unit 120 is the secondary nanofiltration water Cl-/SO4 2-5917.3/73.5, saltpeter ratio (NaCl/Na)2SO4) 89.6/1, three-stage nanofiltration concentrated water Cl of the three-stage nanofiltration unit 130-/SO4 2-1204.8/53114.5, saltpeter ratio (NaCl/Na)2SO4)＝1/39.6。
(4) The final produced water of the multi-stage nanofiltration device 100, that is, the secondary nanofiltration produced water of the secondary nanofiltration unit 120, and the final concentrated water of the multi-stage nanofiltration device 100, that is, the tertiary nanofiltration concentrated water of the tertiary nanofiltration unit 130, both enter the concentration device, so as to reduce the scale of sodium chloride and sodium sulfate crystals. In this embodiment, the concentration device respectively adopts a first concentration device 700 and a second concentration device 800, wherein the first concentration device 700 is a high-pressure reverse osmosis concentration device, and after the second-stage nanofiltration produced water is concentrated by the first concentration device 700, the concentrated water side of the first concentration device 700 has the following water quality: pH: 6-8, COD: 388.0mg/L, TOC: 88.2mg/L, Ca2+：0.5mg/L、Mg2+：0.4mg/L、NH4 +：11.6mg/L、Na+：18348.4mg/L、K+：628.2mg/L、Cl-：27732.5mg/L、SO4 2-：344.7mg/L、NO3 -：893.3mg/L、HCO3-：640.5mg/L、CO3 2-：38.3mg/L、SiO2：120.4mg/L、TDS：48758.7mg/L。
After the three-stage nanofiltration concentrated water of the multi-stage nanofiltration device 100 passes through the second concentration device 800, the concentrated water side of the second concentration device 800 has the following water quality: pH: 6-8, COD: 2482.3.0mg/L, TOC: 564.2mg/L, Ca2+：19.9mg/L、Mg2+：13.2mg/L、NH4 +：72.6mg/L、Na+：41985.6mg/L、K+：2821.5mg/L、Cl-：1682.3mg/L、SO4 2-：88019.1mg/L、NO3 -：236.7mg/L、HCO3-：1131.9mg/L、CO3 2-：13.3mg/L、SiO2：248.1mg/L、TDS：136244.4mg/L。
(5) The final produced water of the multi-stage nanofiltration device 100, that is, the concentrated water of the second-stage nanofiltration produced water of the second-stage nanofiltration unit 120, concentrated by the first concentration device 700, enters the sodium chloride evaporative crystallization device 300. In this embodiment, the sodium chloride evaporative crystallization device 300 may be an MVR evaporator, it is understood that in other embodiments, the MVR evaporator may be replaced by a single-effect evaporator, a TVR evaporator or a multiple-effect evaporator, and the sodium chloride evaporative crystallization device 300 produces 0.72t/h of sodium chloride, purity: 97.2 percent and 4.7 percent of water. Residual sodium chloride crystallization mother liquor 0.5m3H, wherein 0.3m3Refluxing for h till sodium sulfate freezing crystallization mother liquor enters water, and enabling the rest sodium chloride crystallization mother liquor to enter a miscellaneous salt evaporation crystallization device 600, wherein the water quality of the sodium chloride crystallization mother liquor is as follows: pH: 6-8, COD: 2482.3mg/L, TOC: 564.2mg/L, Ca2+：19.9mg/L、Mg2+：13.2mg/L、NH4 +：72.6mg/L、Na+：41985.6mg/L、K+：2821.5mg/L、Cl-：1682.3mg/L、SO4 2-：88019.1mg/L、NO3 -：236.7mg/L、HCO3-：1131.9mg/L、CO3 2-：13.3mg/L、SiO2：248.1mg/L、TDS：136244.4mg/L。
(6) The final concentrate of the multi-stage nanofiltration device 100 is alsoNamely, the three-stage nanofiltration concentrated water is concentrated by the first concentration device 700 and then enters the sodium sulfate freezing crystallization mother liquor, the sodium sulfate freezing crystallization mother liquor produces 0.91t/h of sodium sulfate, the purity is 99 percent, the water content is 4.6 percent, and the water quality of the sodium sulfate crystallization mother liquor is as follows: pH: 6-8, COD: 3032.0mg/L, TOC: 687.0mg/L, Ca2+：22.3mg/L、Mg2+：14.9mg/L、NH4 +：92.2mg/L、Na+：17969.9mg/L、K+：3783.1mg/L、Cl-：7336.0mg/L、SO4 2-：30000.0mg/L、NO3 -：1255.1mg/L、HCO3-：1951.0mg/L、CO3 2-：57.3mg/L、SiO2: 405.4mg/L, TDS: 62887.1mg/L, the sodium sulfate crystallization mother liquor enters a high-pressure nanofiltration device 900.
(7) Nanofiltration water produced by the high-pressure nanofiltration device 900 flows back to the water inlet end of the first-stage nanofiltration unit 110 of the multi-stage nanofiltration device 100, part of nanofiltration concentrated water of the high-pressure nanofiltration device 900 enters the mixed salt evaporation crystallization device 600, part of the nanofiltration concentrated water of the high-pressure nanofiltration device 900 flows back to the second concentration device 800, and the nanofiltration concentrated water of the high-pressure nanofiltration device 900 has the following water quality: pH: 6-8, COD: 7255.14mg/L, TOC: 1648.9mg/L, Ca2+：63.9mg/L、Mg2+：42.6mg/L、NH4 +：221.4mg/L、Na+：40621.3mg/L、K+：8551.7mg/L、Cl-：489.1mg/L、SO4 2-：93000.0mg/L、NO3 -：1196.5mg/L、HCO3-：3084.3mg/L、CO3 2-：37.2mg/L、SiO2：405.4mg/L、TDS：148154.0mg/L。
(8) The sodium chloride crystallization mother liquor and the nanofiltration concentrated water of the high-pressure nanofiltration device 900 enter the mixed salt evaporation crystallization device 600 together, and the mixed salt evaporation crystallization device 600 uses a single-effect evaporation system in the embodiment. The final production of the miscellaneous salt is 0.21t/h, the integral miscellaneous salt rate of the project is 11.3 percent, and the treatment cost of hazardous waste is greatly reduced.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (16)
1. A multi-dimensional salt separation system is characterized by comprising a multi-stage nanofiltration device, a sodium chloride evaporation crystallization device, a sodium sulfate freezing crystallization device and a melting crystallization device; the sodium chloride evaporative crystallization device and the sodium sulfate freezing crystallization device are respectively connected with the multistage nanofiltration device, the secondary nanofiltration water produced by the multistage nanofiltration device enters the sodium chloride evaporative crystallization device, the secondary nanofiltration concentrated water of the multistage nanofiltration device enters the sodium sulfate freezing crystallization device, the melting crystallization device is connected with the sodium sulfate freezing crystallization device, the sodium sulfate freezing crystallization device freezes and crystallizes to obtain mirabilite, the mirabilite is melted and crystallized by the melting crystallization device to obtain anhydrous sodium sulfate, and part of nanofiltration concentrated water of sodium sulfate crystallization mother liquor of the sodium sulfate freezing crystallization device after nanofiltration enters the miscellaneous salt evaporative crystallization device.
2. The multi-dimensional salt separation system of claim 1, wherein the multi-stage nanofiltration device comprises a primary nanofiltration unit, a secondary nanofiltration unit, and a tertiary nanofiltration unit, the first-stage nanofiltration unit, the second-stage nanofiltration unit and the third-stage nanofiltration unit are sequentially communicated in series, the first-stage nanofiltration unit is also communicated with the third-stage nanofiltration unit so as to realize that first-stage nanofiltration concentrated water of the first-stage nanofiltration unit enters the third-stage nanofiltration unit, the water produced by the third-stage nanofiltration of the third-stage nanofiltration unit also enters the second-stage nanofiltration unit, the softening and desiliconization device is connected with the first-stage nanofiltration unit, the second-stage nanofiltration unit is connected with the sodium chloride evaporative crystallization device, the sodium sulfate freezing crystallization device is connected with the third-stage nanofiltration unit, and the melting crystallization device is connected with the sodium sulfate freezing crystallization device.
3. The multidimensional salt separation system according to claim 2, further comprising a high-pressure nanofiltration device, wherein the high-pressure nanofiltration device is connected with the sodium sulfate freezing crystallization device, the high-pressure nanofiltration device is further connected with the primary nanofiltration unit, sodium sulfate crystallization mother liquor of the sodium sulfate freezing crystallization device enters the high-pressure nanofiltration device for nanofiltration, part of nanofiltration concentrated water of the high-pressure nanofiltration device enters the miscellaneous salt evaporation crystallization device, and nanofiltration produced water of the high-pressure nanofiltration device enters the primary nanofiltration unit.
4. The multidimensional salt separation system as recited in claim 3, further comprising a miscellaneous salt evaporative crystallization device connected with the sodium chloride evaporative crystallization device, the miscellaneous salt evaporative crystallization device being configured to receive a portion of the sodium chloride crystallization mother liquor from the sodium chloride evaporative crystallization device and evaporate miscellaneous salts.
5. The multi-dimensional salt separation system according to claim 2, wherein the sodium chloride evaporative crystallization device is further connected with the sodium sulfate freezing crystallization device, and a part of sodium chloride crystallization mother liquor of the sodium chloride evaporative crystallization device enters the sodium sulfate freezing crystallization device for freezing crystallization.
6. The multi-dimensional salt separating system according to any one of claims 3-5, further comprising a first concentration device connected in series between the secondary nanofiltration unit and the sodium chloride evaporative crystallization device.
7. The multi-dimensional salt separating system according to any one of claims 4-5, further comprising a second concentration device connected in series between the three-stage nanofiltration unit and the sodium sulfate freezing and crystallizing device.
8. The multi-dimensional salt separation system according to claim 7, wherein the high-pressure nanofiltration device is connected in series between the sodium sulfate freezing crystallization device and the miscellaneous salt evaporation device, and part of the nanofiltration concentrated water of the high-pressure nanofiltration device enters the miscellaneous salt evaporation crystallization device.
9. The multi-dimensional salt separation system according to claim 8, wherein the high-pressure nanofiltration device is further connected to the second concentration device, and part of the nanofiltration concentrated water of the high-pressure nanofiltration device further enters the second concentration device.
10. The multi-dimensional salt separating system according to any one of claims 2-5, further comprising a conditioning tank connected to the front end of the softening and desiliconizing device.
11. A multi-dimensional salt separation system according to any one of claims 2 to 5, wherein the softening and desiliconizing device comprises one or more of a high density pond, a filter pond and an ultrafiltration device.
12. The multi-dimensional salt separation system according to any one of claims 2-5, wherein the primary nanofiltration unit is a high efficiency He nanofiltration unit;
and/or the secondary nanofiltration unit is a high-interception Hr nanofiltration unit;
and/or the third-stage nanofiltration unit is a high-recovery Hc nanofiltration unit.
13. The multi-dimensional salt separation system according to any one of claims 1 to 5, further comprising a softening and silicon-removing device connected to the multi-stage nanofiltration device.
14. A multi-dimensional salt separation method is characterized by comprising the following steps:
the method comprises the following steps that high-salinity wastewater is softened and desilicated by a softening desiliconization device and then enters a multi-stage nanofiltration device for nanofiltration treatment, first-stage nanofiltration concentrated water of a first-stage nanofiltration unit enters a third-stage nanofiltration unit, first-stage nanofiltration produced water of the first-stage nanofiltration unit enters a second-stage nanofiltration unit, second-stage nanofiltration concentrated water of the second-stage nanofiltration unit enters the third-stage nanofiltration unit, second-stage nanofiltration produced water of the second-stage nanofiltration unit enters a sodium chloride evaporation crystallization device for evaporation and crystallization to obtain sodium chloride, second-stage nanofiltration concentrated water of the third-stage nanofiltration unit enters a sodium sulfate freezing crystallization device for freezing and crystallization to obtain sodium sulfate, and second-stage nanofiltration produced water of the third-stage nanofiltration unit flows back.
15. The multi-dimensional salt splitting method according to claim 14, further comprising the steps of:
part of sodium chloride crystals in the sodium chloride evaporative crystallization device enter a mixed salt evaporative crystallization device and are evaporated and crystallized to obtain mixed salt;
and/or, part of sodium chloride crystallization mother liquor of the sodium chloride evaporation crystallization device enters the sodium sulfate freezing crystallization device to be frozen and crystallized to obtain sodium sulfate;
and/or part of nanofiltration concentrated water of sodium sulfate crystallization mother liquor of the sodium sulfate freezing crystallization device after nanofiltration by the high-pressure nanofiltration device enters the mixed salt evaporation crystallization device and is evaporated and crystallized to obtain mixed salt, the other part of nanofiltration concentrated water flows back to the second concentration device, and nanofiltration produced water of the high-pressure nanofiltration device flows back to the first-stage nanofiltration unit.
16. The multi-dimensional salt splitting method according to claim 14 or 15, further comprising the steps of: and the sodium sulfate freezing and crystallizing device freezes and crystallizes the obtained mirabilite, and the sodium sulfate is melted and crystallized by the melting and crystallizing device to obtain anhydrous sodium sulfate.
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