CN107324581A - The device of sub-prime salt manufacturing and the method for sub-prime salt manufacturing - Google Patents
The device of sub-prime salt manufacturing and the method for sub-prime salt manufacturing Download PDFInfo
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- CN107324581A CN107324581A CN201710786980.6A CN201710786980A CN107324581A CN 107324581 A CN107324581 A CN 107324581A CN 201710786980 A CN201710786980 A CN 201710786980A CN 107324581 A CN107324581 A CN 107324581A
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- mother liquor
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- salt manufacturing
- sodium chloride
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- 150000003839 salts Chemical class 0.000 title claims abstract description 82
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 41
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 102
- 238000000926 separation method Methods 0.000 claims abstract description 62
- 239000013078 crystal Substances 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 239000011780 sodium chloride Substances 0.000 claims abstract description 49
- 230000003647 oxidation Effects 0.000 claims abstract description 46
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 46
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 41
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 23
- 238000001728 nano-filtration Methods 0.000 claims abstract description 22
- 239000012452 mother liquor Substances 0.000 claims description 79
- 239000012141 concentrate Substances 0.000 claims description 49
- 239000012528 membrane Substances 0.000 claims description 30
- 150000002500 ions Chemical class 0.000 claims description 29
- 239000002351 wastewater Substances 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 11
- 239000005416 organic matter Substances 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 16
- 230000008901 benefit Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 6
- 238000010276 construction Methods 0.000 abstract description 5
- 235000002639 sodium chloride Nutrition 0.000 description 110
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 47
- 238000002425 crystallisation Methods 0.000 description 15
- 230000008025 crystallization Effects 0.000 description 14
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 13
- 239000010442 halite Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 238000001764 infiltration Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 235000011152 sodium sulphate Nutrition 0.000 description 5
- 239000012267 brine Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 4
- 241000628997 Flos Species 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- -1 Fe2+) Chemical class 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 206010039509 Scab Diseases 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 238000009287 sand filtration Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- 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
- 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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- 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
- C02F1/445—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by forward osmosis
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/20—Total organic carbon [TOC]
-
- 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
- C02F2301/04—Flow arrangements
- C02F2301/046—Recirculation with an external loop
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/22—Eliminating or preventing deposits, scale removal, scale prevention
Abstract
The device for the sub-prime salt manufacturing that the present invention is provided and the method for sub-prime salt manufacturing, are related to sub-prime salt manufacturing production technical field, and the device of the sub-prime salt manufacturing includes：Pretreatment unit, separate oxidation unit, upgrading unit, sulfate crystal device and sodium chloride crystallizer；The pretreatment unit, separate oxidation unit and sulfate crystal device are sequentially connected, and the separate oxidation unit includes the nanofiltration separation device and oxidation unit being sequentially connected；The upgrading unit includes the first reverse osmosis enrichment facility being sequentially connected and just oozes enrichment facility, and the first reverse osmosis enrichment facility is connected with the nanofiltration separation device, and the enrichment facility that just oozing is connected with the sodium chloride crystallizer.The purity of divalence crystal salt in sulfate crystal device is further increased in the device for the sub-prime salt manufacturing that the present invention is provided, the first separating liquid is further concentrated using upgrading unit, the effect high to the salt rate of recovery is reached, has the advantages that simple in construction and economizes on resources.
Description
Technical field
The present invention relates to sub-prime salt manufacturing production technical field, device and sub-prime salt manufacturing more particularly, to a kind of sub-prime salt manufacturing
Method.
Background technology
The high saliferous discharged during the project constructions such as papermaking, printing and dyeing, desalinization, electric power, oil and coal chemical industry gives up
Contain multiple inorganic ions and organic matter in water, the sodium chloride of higher concentration is usually contained, therefore, in the processing of this kind of waste water
In, desalination difficulty is larger, and resource utilization degree is low.
In recent years, as environmental protection is increasingly paid attention to by the mankind, " zero-emission " or " nearly zero-emission of high slat-containing wastewater
Put " turn into the requirement of more and more Enterprise Projects, therefore a kind of reliable, economic, efficient, energy-conservation high strong brine " zero-emission of exploitation
Put " system, and realize high strong brine maximum resource using emphasis and difficult point of the chemical conversion for current field of industrial waste water treatment.
At present, domestic most enterprises handle high strong brine using evaporative crystallization method, i.e. Halite water is dense via evaporator
Evaporation pond is delivered to after contracting and is evaporated or delivers to crystallizer crystallization generation carnallite.Carnallite complicated components, and can only enter as dangerous waste
Row landfill disposal, the method not only a large amount of occupied grounds, is also easily lost in, salinization to environment structure grave danger, salt and impurity
Surrounding soil, jeopardizes vegetation around, and rivers, water source, rice field to surrounding etc. are polluted.
In traditional sub-prime salt technique, one is directly by evaporative crystallization and freezing and crystallizing system by not separated carnallite
Salt, or purified the relatively low crystal salt of purity again by recrystallization method.But the investment of both approaches is big, operating cost
Height, the rate of recovery is low, and the purity of obtained salt is low, is not appropriate for extensive use.
With constantly bringing forth new ideas and progressive, the technique mesh that a kind of concentration of ionic membrane point salt is combined with crystallization salt manufacturing for embrane method technology
It is preceding just expanded, and may though high slat-containing wastewater can be carried out initial gross separation by this technique by the method for ion UF membrane
The sodium chloride salt of higher degree is obtained, but this system is adding investment and operating cost, and also the pure salt rate of recovery is low, causes money
Source is wasted.
It can be seen that, the dual treatment method for high slat-containing wastewater mainly will separation embrane method and evaporative crystallization in the prior art
Simply combined, but this combination is not only saved to energy consumption and not helped significantly, while again virtually
Cost of investment is added, and guarantee in high yield with high-purity can not be reached to final product salt.
The content of the invention
It is an object of the present invention to provide a kind of device of sub-prime salt manufacturing, to solve existing sub-prime salt manufacturing to energy consumption
Saving is not helped significantly, and technical problem in high yield with high-purity can not be reached to final product salt.
It is another object of the present invention to provide a kind of method of sub-prime salt manufacturing, using the sub-prime salt manufacturing of above-mentioned offer
Device.
In order to solve the above technical problems, present invention employs following technical scheme；The sub-prime that first aspect present invention is provided
The device of salt manufacturing, wherein, including：Pretreatment unit, separate oxidation unit, upgrading unit, sulfate crystal device and sodium chloride knot
Brilliant device；
The pretreatment unit, separate oxidation unit and sulfate crystal device are sequentially connected, the separate oxidation unit bag
Include the nanofiltration separation device and oxidation unit being sequentially connected；
The upgrading unit includes the first reverse osmosis enrichment facility being sequentially connected and just oozes enrichment facility, first reverse osmosis
Enrichment facility is connected with the nanofiltration separation device, and the enrichment facility that just oozing is connected with the sodium chloride crystallizer.
In any of the above-described technical scheme, further, in addition to mother liquor separating and reclaiming device, the sulfate crystal device
On be provided with the second mother liquor outlet being connected with the mother liquor separating and reclaiming device.
In any of the above-described technical scheme, further, the mother liquor separating and reclaiming device includes and second mother liquor
The ion membrane separation device of connection is exported, the ion membrane separation device is connected with the sodium chloride crystallizer.
In any of the above-described technical scheme, further, the mother liquor separating and reclaiming device also includes being arranged at described the
Heat exchanger between two mother liquor outlets and ion membrane separation device.
In any of the above-described technical scheme, further, the first mother liquor outlet, institute are provided with the sodium chloride crystallizer
The first mother liquor outlet is stated to be connected with the sulfate crystal device.
In any of the above-described technical scheme, further, the upgrading unit also includes connecting with the enrichment facility that just oozing
The the second reverse osmosis enrichment facility connect, for recycling the second separating liquid in the second reverse osmosis enrichment facility.
The present invention also provides a kind of method of sub-prime salt manufacturing, wherein, comprise the following steps：
S1, waste water carry out pretreating process, and the easy scale-forming ion and organic matter in waste water are removed substantially；
S2, pretreated waste water obtain the first separating liquid and the first concentrate by nanofiltration separation device；
S31, the first separating liquid are condensed into the second separating liquid and the second concentrate by upgrading unit separation；
S32, the first concentrate are evaporated into sulfate crystal device after oxidation unit and obtain divalence crystal salt；
S4, the second concentrate are evaporated into sodium chloride crystallizer obtains monovalence crystal salt.
In any of the above-described technical scheme, further, the second separating liquid returns to upgrading unit and circulated in step S31
Utilize.
In any of the above-described technical scheme, further, processing of first concentrate in sulfate crystal device in step S32
During the second mother liquor for producing recycled by mother liquor separating and reclaiming device into sodium chloride crystallizer.
In any of the above-described technical scheme, further, processing of second concentrate in sodium chloride crystallizer in step S4
During the first mother liquor for producing enter sulfate crystal device and recycled.
Using above-mentioned technical proposal, the present invention has the advantages that：
Halite water is carried out at separation oxidation using separate oxidation unit in the device for the sub-prime salt manufacturing that the present invention is provided
Reason, further increases the purity of divalence crystal salt in sulfate crystal device, and the first separating liquid is entered to advance using upgrading unit
One step is concentrated, and reaches the effect high to the salt rate of recovery, is had the advantages that simple in construction and is economized on resources.
Further, in addition to mother liquor separating and reclaiming device, it is provided with the sulfate crystal device and the mother liquor point
The second mother liquor outlet connected from retracting device.
Further, be provided with the first mother liquor outlet in the sodium chloride crystallizer, first mother liquor outlet with it is described
Sulfate crystal device is connected.
The additional aspect and advantage of the present invention will become obvious in following description section, or pass through the practice of the present invention
Recognize.
Brief description of the drawings
Below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The accompanying drawing used required in embodiment or description of the prior art is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the positive structure schematic of the device for the sub-prime salt manufacturing that the embodiment of the present invention one is provided.
Reference：
101：Inlet water tank；102：Pretreatment unit；103：Separate oxidation unit；
104：Nanofiltration separation device；105：Oxidation unit；106：Upgrading unit；
107：First reverse osmosis enrichment facility；108：Just ooze enrichment facility；
109：Second reverse osmosis enrichment facility；110：Sulfate crystal device；
111：Sodium chloride crystallizer；112：Heat exchanger；113：Ion membrane separation device；
114：Mother liquor separating and reclaiming device.
Embodiment
Technical scheme is clearly and completely described below in conjunction with accompanying drawing, it is clear that described implementation
Example is a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
It should be noted that in the case where not conflicting, the feature in embodiments herein and embodiment can be mutually combined.
In the description of the invention, it is necessary to explanation, term " " center ", " on ", " under ", "left", "right", " vertical ",
The orientation or position relationship of the instruction such as " level ", " interior ", " outer " be based on orientation shown in the drawings or position relationship, merely to
Be easy to the description present invention and simplify description, rather than indicate or imply signified device or element must have specific orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.In addition, term " first ", " second ",
" the 3rd " is only used for describing purpose, and it is not intended that indicating or implying relative importance.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected, or be integrally connected；Can
To be mechanical connection or electrical connection；Can be joined directly together, can also be indirectly connected to by intermediary, Ke Yishi
The connection of two element internals.For the ordinary skill in the art, with concrete condition above-mentioned term can be understood at this
Concrete meaning in invention.
With reference to specific embodiment the present invention will be further explained explanation.
As shown in figure 1, the device for the sub-prime salt manufacturing that the embodiment of first aspect present invention is provided, including：Pretreatment unit
102nd, separate oxidation unit 103, upgrading unit 106, sulfate crystal device 110 and sodium chloride crystallizer 111；
The pretreatment unit 102, separate oxidation unit 103 and sulfate crystal device 110 are sequentially connected, the separation oxygen
Change nanofiltration separation device 104 and oxidation unit 105 that unit 103 includes being sequentially connected；
The upgrading unit 106 includes the first reverse osmosis enrichment facility 107 being sequentially connected and just oozes enrichment facility 108, institute
The first reverse osmosis enrichment facility 107 is stated to be connected with the nanofiltration separation device 104, it is described just to ooze enrichment facility 108 and the chlorination
Sodium crystallizer 111 is connected.
Separation oxidation is carried out to Halite water using separate oxidation unit 103 in the device for the sub-prime salt manufacturing that the present invention is provided
Processing, further increases the purity of divalence crystal salt in sulfate crystal device 110, utilizes 106 pair of first separation of upgrading unit
Liquid is further concentrated, and reaches the effect high to the salt rate of recovery, is had the advantages that simple in construction and is economized on resources.
Pretreatment unit 102 in the present invention, with water inlet and softened water delivery port；
Oxidation treatment device is separated, described with its water inlet connection of water inlet, discharge channel and concentrated solution outlet
The delivery port of pretreatment unit 102；Upgrading unit 106, the separating liquid of the described separation oxidation treatment device of its water inlet connection
Outlet；The device of sulfate crystal device 110, the concentrated solution outlet of the described separation oxidation treatment device of its water inlet connection and chlorination
The mother liquor floss hole of sodium crystallizer 111；The device of sodium chloride crystallizer 111, the concentration of the described upgrading unit 106 of its water inlet connection
Liquid is exported and mother liquor separates and recovers the discharge channel of processing unit；Disposing mother liquor processing unit, its water inlet connects described
The mother liquor floss hole of sulfate crystal device 110.
The separate oxidation unit 103 includes being used for the first water inlet, the first separating liquid of the high slat-containing wastewater after softening
Outlet and the first concentrated solution outlet after advanced oxidation；The upgrading unit 106 includes second for the first separating liquid
Water inlet, the second concentrated solution outlet and the second discharge channel；The sodium chloride crystallizer 111 includes being used for sodium chloride salt concentration
The 3rd water inlet, sodium chloride salt slurry outlet and the first mother liquor outlet；The sulfate crystal device 110 includes being used for sodium sulfate salt
The 4th water inlet, the outlet of sodium sulphate salt slurry and the second mother liquor outlet of concentration；The mother liquor separating and reclaiming device 114 includes being used for
The 5th water inlet, the outlet of final separation liquid and the final outer row's mother liquor outlet of second mother liquor separation.
Wherein, first discharge channel connects second water inlet, second concentrate and final separation liquid
Outlet connection the 3rd water inlet, first concentrate and the first mother liquor outlet connect the 4th water inlet, and second is female
Liquid outlet connection the 5th water inlet.
The NF membrane rate of recovery in separate oxidation unit 103 can adjust intake pressure and recovery according to specific Water-quality control
Rate, oxidation unit 105 is only handled nanofiltration concentrated water, and processing water is only 20%~50% that separation oxidation is always intake；
Upgrading unit 106 is using counter-infiltration with just permeating the processing unit being combined, and Halite water is by counter-infiltration and just
The priority processing sequence of permeable membrane device can according to specific influent quality and family demand carry out permutation and combination, the reverse osmosis
The enrichment facility permeated thoroughly and just may be designed as single-stage or multistep treatment to adjust cycles of concentration；
Also include：First centrifugal drying device, its be arranged at the first crystallization apparatus bottom slurry export be connected；The
Two centrifugal drying devices, its be arranged at the second crystallization apparatus bottom magma export be connected；
Mother liquor separating and reclaiming device 114, in addition to：Heat exchanger 112, its hot side import and the sulfate crystal device 110
Mother liquor floss hole be connected, outlet be connected with the water inlet of mother liquor membrane separation device, cold side import and export is connected with cooling medium.
The present invention also provides a kind of method of sub-prime salt manufacturing, wherein, comprise the following steps：
S1, waste water carry out pretreating process, and the easy scale-forming ion and organic matter in waste water are removed substantially；
S2, pretreated waste water obtain the first separating liquid and the first concentrate by nanofiltration separation device；
S31, the first separating liquid are condensed into the second separating liquid and the second concentrate by upgrading unit separation；
S32, the first concentrate are evaporated into sulfate crystal device after oxidation unit and obtain divalence crystal salt；
S4, the second concentrate are evaporated into sodium chloride crystallizer obtains monovalence crystal salt.
In any of the above-described technical scheme, further, the second separating liquid returns to upgrading unit and circulated in step S31
Utilize.
In any of the above-described technical scheme, further, processing of first concentrate in sulfate crystal device in step S32
During the second mother liquor for producing recycled by mother liquor separating and reclaiming device into sodium chloride crystallizer.
In any of the above-described technical scheme, further, processing of second concentrate in sodium chloride crystallizer in step S4
During the first mother liquor for producing enter sulfate crystal device and recycled.
Pretreating process：Using handling process such as dosing softening, coagulation clarification, tubular type micro-filtrations by Ca2+, Mg2 in raw water
+, easily scale-forming ion and the organic matter such as Si remove, and reduce the parameter such as COD, TOC in raw water substantially.
Separate oxidation technology：Halite water after sofening treatment is arrived first enters nano filter membrance device, nanofiltration separation device 104
For tubular nanofiltration membrane separator, tubular nanofiltration membrane separator carries out membrane filtration separation to it, because haline water is in charged membrane
In the southern effect in road, it is divalence that the first separating liquid being filtrated to get comprises only most of salt in monovalent salt, the first concentrate substantially
Ion, and contain organic matter in water inlet etc.；The first concentrate that nanofiltration is obtained is handled into oxidation unit 105, is passed through
The high-level oxidation technologies such as Fenton reduce its organic matter, COD, TOC and some specific divalent ions (such as Fe2+), by separation
The first concentrate that oxidation processes are obtained, enters eventually into sulfate crystal device 110 and is handled.
Concentration technology：The first separating liquid obtained in separation oxidation technology is initially entered in the first reverse osmosis enrichment facility 107
Preliminary concentrate is carried out, the first-stage reverse osmosis concentrated water waited until obtains the second concentrate by the processing of positive permeability apparatus, its salt content
Highest can be concentrated into 240,000mg/L；First reverse osmosis produced water is re-introduced into the second reverse osmosis enrichment facility with positive infiltration production water
109 are refined, and two-pass reverse osmosis concentrated water continues cycling through processing；The second separating liquid finally given by upgrading unit 106 is made
For production Water circulation, the second concentrate is handled into sodium chloride crystallizer 111.
Economic benefits and social benefits crystallization processes：Second concentrate is produced in the processing procedure of sodium chloride crystallizer 111, quantitatively
Sulfate crystal device 110 is drained into outside one mother liquor, so as to obtain the monovalence crystal salt of high-purity；First concentrate and the first mother liquor exist
During sodium chloride crystallizer 111 is evaporated crystallization treatment, is quantitatively produced the second mother liquor and quantitatively drain into mother liquor outside
Separating and reclaiming device 114, so as to obtain the divalence crystal salt of high-purity；The steam condensate (SC) that economic benefits and social benefits crystallizer is produced will be returned and used
In production.
Mother liquor process for separating and recovering, including heat exchanger 112 and ion membrane separation device 113：Second mother liquor passes through heat exchanger
112 by a kind of ion membrane separation device 113 with after cooling water heat exchange, then being handled and obtaining being finally recovered liquid and final concentrate；Its
In, the final separation liquid containing most monovalent ions is back to sodium chloride crystallizer 111 and crystallized, it is very small amount of most
Whole concentrate is discharged as outer row's mother liquor.
In any of the above-described technical scheme, further, in addition to mother liquor separating and reclaiming device 114, the sodium sulphate knot
The second mother liquor outlet being connected with the mother liquor separating and reclaiming device 114 is provided with brilliant device 110.
In any of the above-described technical scheme, further, the mother liquor separating and reclaiming device 114 includes and the described second mother
The ion membrane separation device 113 of liquid outlet connection, the ion membrane separation device 113 is connected with the sodium chloride crystallizer 111.
In any of the above-described technical scheme, further, the mother liquor separating and reclaiming device 114 is also described including being arranged at
Heat exchanger 112 between second mother liquor outlet and ion membrane separation device 113.
In any of the above-described technical scheme, further, in the sodium chloride crystallizer 111 it is provided with the first mother liquor and goes out
Mouthful, first mother liquor outlet is connected with the sulfate crystal device 110.
In any of the above-described technical scheme, further, the upgrading unit 106 also includes just oozing enrichment facility with described
Second reverse osmosis enrichment facility 109 of 108 connections, for recycling the second separation in the second reverse osmosis enrichment facility 109
Liquid.
In any of the above-described technical scheme, further, in addition to centrifugal drying device, the sulfate crystal device 110
Slurry outlet is respectively arranged with the bottom of sodium chloride crystallizer 111, the centrifugal drying device corresponds to the slurry outlet and set.
In any of the above-described technical scheme, further, first outlet is respectively arranged with the nanofiltration separation device 104
And second outlet, the first outlet is connected with the oxidation unit 105, and the second outlet is concentrated with first reverse osmosis and filled
Put 107 connections.
The present invention also provides a kind of sub-prime salt making system, wherein, include the device of sub-prime salt manufacturing as described above.
In any of the above-described technical scheme, further, in addition to the inlet water tank being connected with the pretreatment unit 102
101。
Using NF membrane to bivalent ions high rejection in Halite water, it can both ensure the high-purity of monovalence crystal salt
Degree, efficiently can be separated one, divalent ion under relatively low investment and operating cost again, complete the sub-prime of high-purity
Processing.
Separation oxidation processes are carried out to Halite water using separate oxidation unit 103, reduces in the first concentrate and pollutes
Content of material, the problems such as both effectively eliminating the fouling of follow up device, scab, further improves sulfate crystal device 110
The purity of middle divalence crystal salt.
Further concentrated using 106 pair of first separating liquid of upgrading unit, not only operational efficiency is high, cost of investment is low,
The water for eventually entering into sodium chloride crystallizer 111 is also substantially reduced, and improves its salt content of intaking simultaneously, is greatly reduced
The investment of follow-up sodium chloride crystallizer 111 and operating cost.
Described economic benefits and social benefits crystallization apparatus production intensity is big, efficiency high, in crystallization, passes through quantitatively outer row's mother liquor
Method make the monovalence finally obtained and divalence product salt quality good, purity is high, and mother liquor is separated using follow up device
The method of recovery ensure that the rate of recovery of salt.
The mother liquor separating and reclaiming device 114, employs a kind of ion membrane separation device 113 of low energy consumption, and it will be last
Separate the monovalence salting liquid containing high concentration and high-purity and be back to sodium chloride crystallizer 111, both enhance salt separation effect
Really, organic efficiency is improved, the cost of mother liquid disposal is reduced again, the energy has been saved.
The disposing mother liquor processing unit, is the coupling apparatus of a kind of heat exchanger 112 and ion membrane separation process, existing skill
Record is had no in art.
A, first by pretreatment unit 102 remove strong brine in easily fouling ion such as calcium, magnesium；Wrapped in step A
Include sand filtration, multi-medium filtering, tubular type micro-filtration, coagulation clarification method processing in one or more of methods combination
B, softened water are handled by nanofiltration separation device 104 and obtain the first separating liquid and the first concentrate；
C, the first separating liquid carry out separation concentration by enrichment facility, obtain the second concentrate and the second separating liquid, second
Separating liquid is returned for producing；
D, the first concentrate enter sulfate crystal device 110 after catalysis oxidation, and the second concentrate enters sodium chloride knot
Brilliant device 111 is evaporated crystallization treatment；
The first mother liquor that E, the second concentrate are produced in the processing procedure of sodium chloride crystallizer 111 enters sodium sulphate knot
Brilliant device 110, the second mother liquor that the first concentrate is produced in the processing procedure of sodium sulphate sodium crystallizer is separated and recovered into mother liquor
Device 114；
After F, the second mother liquor are by heat exchanger 112 and cooling water heat exchange, are handled and obtained by a kind of ion membrane separation device 113
It is finally recovered liquid and final concentrate；
G, final separation liquid are back to sulfate crystal device 110 and crystallized, and very small amount of final concentrate is as outer
Arrange mother liquor discharge；
H, final sodium chloride crystallizer 111 and sulfate crystal device 110 respectively obtain high yield and purity monovalence and
Divalence solid salt, the condensed water that two sets of crystallizers are produced is returned for producing.
Following process step is included in the step B-D：
Handled first with nanofiltration separation device 104 and obtain the first separating liquid and the first concentrate；
First concentrate is handled after catalysis oxidation into sulfate crystal device 110；
The enrichment facility (MBC) that first separating liquid enters positive infiltration and counter-infiltration combination carries out decrement concentration to water again
Obtain the second separating liquid and the second concentrate；
Second separating liquid is returned for producing；
Second concentrate is evaporated crystallization treatment into sodium chloride crystallizer 111.
The outer row's mother liquor amount of sodium chloride crystallizer 111 can be to ensure monovalence crystal salt purity requirement by calculating in step E
Minimum Mother liquid.
Following process step is included between step F and the step G：
Second mother liquor is exchanged heat by heat exchanger 112 and cooling water first to cool；
Then in the step F, the second mother liquor, which is entered back into membrane separation device, to be separated, and obtains being finally recovered liquid and most
Whole concentrate；
Then in the step G, it is finally recovered liquid and the second separating liquid is mixed into sodium chloride crystallizer 111, so that greatly
The big rate of recovery for improving sodium chloride crystal salt；
Preferentially, in the step F, final concentrate continuous circulation and stress in membrane separation device, finally according to calculating
The outer discharge capacity of final concentrate of minimum is drawn, to ensure the final purity of product salt and reach the highest rate of recovery.
Described NF membrane major function is salt separation function, its retention to organic matter (COD), divalence and high valence ion
Rate can reach more than 95%, and have preferable permeability to monovalention such as Na+, Cl- etc..
The nanofiltration device and ion membrane separation device 113, its operating pressure is generally in 0.2~4.0MPa, and its form can
One section of one-level of selection, two sections of one-level or multistage multisection type are required according to processing water, water quality and aquifer yield etc..
It by UF membrane and mother liquor recovering device, can respectively reach the brilliant salt of sodium chloride and the sulfate crystal salt rate of recovery
More than 90%, sodium chloride crystallization purity salt reaches more than 98.5%, and sulfuric acid crystallization purity salt reaches more than 95%.
The specific workflow of the sub-prime salt treatment device of this example is：Certain chemical production wastewater (120m3/ h) through pre- place
Manage after the sofening treatment of device 102, handled into separate oxidation unit 103, the first separating liquid of nanofiltration device enters concentration
Unit 106 completes further concentration, and the second concentrate of generation is only 15.2m3/ h, TDS reach 210,000ppm or so, wherein
Sodium chloride content is 19% or so, and sodium sulphate content is 0.2% or so, and the second concentrate enters the device of sodium chloride crystallizer 111
After progress, calculated according to model, the first mother liquor that sodium chloride crystallizer 111 is produced drains into sulfate crystal device 110 and is about
0.8m3/ h or so；The first concentrate separated after oxidation processes is about 28m3/h, and TDS is about 120,000ppm or so, wherein
Sodium sulphate content is 9.5% or so, and sodium chloride content is 2% or so, is calculated according to model, the second mother liquor drains into mother liquor and separated back
The flow of receiving apparatus 114 is about 2.2m3/h or so；Second mother liquor enters ion membrane separation device by the cooling of heat exchanger 112
113, it can reach more than 85% to the sodium chloride salt rate of recovery in the second mother liquor, produces final separation liquid and is back to sodium chloride knot
The brilliant device of device 111；Final sodium chloride crystal salt overall recovery can reach more than 90%, and purity is 98.5% or so, sodium sulphate knot
Brilliant salt overall recovery can reach more than 90%, and purity is 95% or so.
In summary, Halite water is divided using separate oxidation unit in the device for the sub-prime salt manufacturing that the present invention is provided
From oxidation processes, the purity of divalence crystal salt in sulfate crystal device is further increased, is separated using upgrading unit to first
Liquid is further concentrated, and reaches the effect high to the salt rate of recovery, is had the advantages that simple in construction and is economized on resources.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.Although in addition, it will be appreciated by those of skill in the art that some embodiments described herein include other implement
Included some features rather than further feature in example, but the combination of the feature of be the same as Example does not mean in the present invention
Within the scope of and form different embodiments.For example, in superincumbent claims, embodiment claimed
It is one of any mode to use in any combination.
Claims (10)
1. a kind of device of sub-prime salt manufacturing, it is characterised in that including：Pretreatment unit, separate oxidation unit, upgrading unit, sulphur
Sour sodium crystallizer and sodium chloride crystallizer；
The pretreatment unit, separate oxidation unit and sulfate crystal device are sequentially connected, the separate oxidation unit include according to
The nanofiltration separation device and oxidation unit of secondary connection；
The upgrading unit includes the first reverse osmosis enrichment facility being sequentially connected and just oozes enrichment facility, the first reverse osmosis concentration
Device is connected with the nanofiltration separation device, and the enrichment facility that just oozing is connected with the sodium chloride crystallizer.
2. the device of sub-prime salt manufacturing according to claim 1, it is characterised in that also including mother liquor separating and reclaiming device, institute
State the second mother liquor outlet for being provided with and being connected with the mother liquor separating and reclaiming device on sulfate crystal device.
3. the device of sub-prime salt manufacturing according to claim 2, it is characterised in that the mother liquor separating and reclaiming device include with
The ion membrane separation device of the second mother liquor outlet connection, the ion membrane separation device connects with the sodium chloride crystallizer
Connect.
4. the device of sub-prime salt manufacturing according to claim 3, it is characterised in that the mother liquor separating and reclaiming device also includes
It is arranged at the heat exchanger between second mother liquor outlet and ion membrane separation device.
5. the device of sub-prime salt manufacturing according to claim 1, it is characterised in that is provided with the sodium chloride crystallizer
One mother liquor outlet, first mother liquor outlet is connected with the sulfate crystal device.
6. the device of sub-prime salt manufacturing according to claim 1, it is characterised in that
The upgrading unit also includes just oozing the second reverse osmosis enrichment facility that enrichment facility is connected with described, for recycling
State the second separating liquid in the second reverse osmosis enrichment facility.
7. a kind of method of sub-prime salt manufacturing, it is characterised in that comprise the following steps：
S1, waste water carry out pretreating process, and the easy scale-forming ion and organic matter in waste water are removed substantially；
S2, pretreated waste water obtain the first separating liquid and the first concentrate by nanofiltration separation device；
S31, the first separating liquid are condensed into the second separating liquid and the second concentrate by upgrading unit separation；
S32, the first concentrate are evaporated into sulfate crystal device after oxidation unit and obtain divalence crystal salt；
S4, the second concentrate are evaporated into sodium chloride crystallizer obtains monovalence crystal salt.
8. the method for sub-prime salt manufacturing according to claim 7, it is characterised in that the second separating liquid returns dense in step S31
Contracting unit is recycled.
9. the method for sub-prime salt manufacturing according to claim 7, it is characterised in that the first concentrate is in sulfuric acid in step S32
The second mother liquor produced in the processing procedure of sodium crystallizer is followed by mother liquor separating and reclaiming device into sodium chloride crystallizer
Ring is utilized.
10. the method for sub-prime salt manufacturing according to claim 7, it is characterised in that the second concentrate is in chlorination in step S4
The first mother liquor produced in the processing procedure of sodium crystallizer enters sulfate crystal device and recycled.
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| CN110451706A (en) * | 2019-05-13 | 2019-11-15 | 上海晶宇环境工程股份有限公司 | The separating technology and special equipment of high-enriched organics and salt during strong brine zero-emission |
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