CN115321559B - Device and method for producing high-concentration sodium sulfate solution by nanofiltration membrane concentration technology - Google Patents
Device and method for producing high-concentration sodium sulfate solution by nanofiltration membrane concentration technology Download PDFInfo
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- CN115321559B CN115321559B CN202211034447.1A CN202211034447A CN115321559B CN 115321559 B CN115321559 B CN 115321559B CN 202211034447 A CN202211034447 A CN 202211034447A CN 115321559 B CN115321559 B CN 115321559B
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- 238000001728 nano-filtration Methods 0.000 title claims abstract description 186
- 239000012528 membrane Substances 0.000 title claims abstract description 152
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- 229910052938 sodium sulfate Inorganic materials 0.000 title claims abstract description 36
- 235000011152 sodium sulphate Nutrition 0.000 title claims abstract description 36
- 238000005516 engineering process Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 204
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 96
- 239000012267 brine Substances 0.000 claims abstract description 50
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 50
- 239000011780 sodium chloride Substances 0.000 claims abstract description 47
- 239000011734 sodium Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 11
- 150000002500 ions Chemical class 0.000 claims abstract description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 229910002651 NO3 Inorganic materials 0.000 claims description 41
- 150000003839 salts Chemical class 0.000 claims description 37
- 239000012141 concentrate Substances 0.000 claims description 16
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 14
- 238000010612 desalination reaction Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 238000004064 recycling Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 9
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 230000004907 flux Effects 0.000 claims description 7
- 235000010265 sodium sulphite Nutrition 0.000 claims description 7
- 238000006722 reduction reaction Methods 0.000 claims description 6
- 239000012466 permeate Substances 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000000502 dialysis Methods 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 230000000903 blocking effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 238000005185 salting out Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 12
- 239000010446 mirabilite Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical group [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 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 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 235000015073 liquid stocks Nutrition 0.000 description 1
- -1 manometer 7 Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to the technical field of separating sodium sulfate from dilute brine after ion membrane electrolysis in chlor-alkali industry, in particular to a device and a method for producing high-concentration sodium sulfate solution by adopting nanofiltration membrane concentration technology. The invention improves Na by arranging a first section nanofiltration membrane device, a second section nanofiltration membrane device and a third section nanofiltration membrane device and concentrating the materials section by section 2 SO 4 The concentration of the sodium sulfate and sodium chloride on the concentrated water side of the nanofiltration is reduced by arranging a pure water tank, a pure water high-pressure pump and a special high-pressure nanofiltration membrane element and utilizing the separation characteristic of the nanofiltration membrane for intercepting divalent ions, so that the concentration of the sodium sulfate on the concentrated water side of the nanofiltration is reduced, the fouling and blocking of the nanofiltration membrane element due to salting-out is reduced, the high-concentration of the sodium sulfate to 150-160g/L is realized, the multi-effect evaporation crystallization energy consumption of more than 50% is reduced, and the sodium sulfate yield is more than 88.4%. Meanwhile, the nanofiltration device is provided with recovery energy, so that the energy consumption can be reduced by 35%.
Description
Technical Field
The invention relates to the technical field of separating sodium sulfate from dilute brine after ion membrane electrolysis in chlor-alkali industry, in particular to a device and a method for producing high-concentration sodium sulfate solution by adopting nanofiltration membrane concentration technology.
Background
The chlor-alkali industry uses crude salt as raw material to produce industrial alkali and chlorine gas, but the crude salt of natural mine contains sodium sulfate and other impurities, na 2 SO 4 Continuously enriching Na in salt water in the production process of the ionic membrane caustic soda device 2 SO 4 Which can lead to the formation of precipitates on the electrode surfaces in the electrolyzer, which increases the energy consumption (higher voltage) and reduces the service life of very expensive electrodes and chloride ion exchange membranes in the membrane electrolysis process;
at present, a membrane method and freezing are commonly adopted in China to remove Na in dilute brine (NaCl=210+/-10 g/L) after ion membrane electrolysis 2 SO 4 Nanofiltration membrane device produced water (namely lean nitrate water, naCl=210+ -10 g/L, na) 2 SO 4 Less than 1 g/L) to dissolve sodium chloride or to be injected into mine for continuous production, nanofiltration membrane concentrated water (namely high-nitrate water, NaCl=205±10g/L，Na 2 SO 4 Content of 60g-88 g/L) after freezing the crystallizer Na 2 SO 4 With sodium sulfate decahydrate crystal (Na 2 SO 4 ·10H 2 O) is precipitated, and the mother liquor after denitration (nacl=205±g/L, na) 2 SO 4 Less than 5 g/L) and nanofiltration refined lean-nitrate water are blended for recycling, and the mirabilite decade crystal slurry is centrifugally separated to obtain mirabilite decade solid, but the mirabilite product contains crystal water, has narrow application range and poor nitric acid selling, has low industrial utilization value and serious resource waste.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a device and a method for producing a high-concentration sodium sulfate solution by adopting a nanofiltration membrane concentration technology, and solves the problems in the background art.
In order to achieve the above purpose, the present invention provides the following technical solutions: the method for producing the high-concentration sodium sulfate solution by adopting the nanofiltration membrane concentration technology comprises the following steps:
the first step: pretreating and cooling the dilute brine (the sodium chloride content is controlled to be 210+/-10 g/L, and the sodium sulfate is less than 20 g/L) after the ionic membrane electrolysis in the chlor-alkali industry, and reducing the temperature of the dilute brine from 60-70 ℃ to 40+/-3 ℃;
and a second step of: adding a reducing agent (sodium thiosulfate or sodium sulfite) according to the content of the dilute brine (1 ton of brine plus 0.1Kg of sodium thiosulfate or sodium sulfite), and removing sodium hypochlorite remained in the electrolytic process by utilizing a reduction reaction;
and a third step of: after the sodium hypochlorite is remained by the activated carbon filter, the sodium hypochlorite enters a first-stage nanofiltration device (nanofiltration membrane has selective permeability to divalent ions), the NaCl=210+/-10 g/L, na2SO4 is controlled to be less than 20g/L, the operating pressure of the first-stage nanofiltration membrane device, the second-stage nanofiltration membrane device and the third-stage nanofiltration membrane device is 20-28Bar, the first-stage nanofiltration recovery rate is 60-85%, the flux of nanofiltration membrane element is 18-25L/m2.H, and the NaCl=210+/-10 g/L of the separated lean-nitrate light brine is Na 2 SO 4 Less than 1g/L, directly entering a production process to dissolve crude salt or injecting the crude salt into an underground mine for recycling;
fourth step: high-nitrate strong brine NaCl=205+ -10 g/L, na of first-stage nanofiltration device 2 SO 4 The content of 60-88g/L enters a super concentration nanofiltration device, the super concentration nanofiltration device comprises a first section nanofiltration membrane device, a second section nanofiltration membrane device and a third section nanofiltration membrane device, the operation pressure is 55-60Bar, the flux of a high-pressure nanofiltration membrane element is 12-18L/m < 2 >. H, and during concentration, 1/3 of pure water is supplemented to dialyze sodium chloride to improve the quality ratio of sodium sulfate, so that the total salt concentration of sodium sulfate and sodium chloride on the concentrated water side of nanofiltration is reduced, and the high-power concentration sodium sulfate is up to 150-160g/L, and the NaCl content is less than 150g/L. After separation, the NaCl of the lean and light salt water is more than 150g/L, na 2 SO 4 Less than 5g/L, directly entering a production process to dissolve crude salt or injecting the crude salt into an underground mine for recycling;
fifth step: concentrated liquid high-nitrate water of the super-concentration nanofiltration device enters direct MVR for evaporative crystallization to produce high-purity Na 2 SO 4 Mirabilite product.
As a preferred technical scheme of the invention, the device for producing the high-concentration sodium sulfate solution by adopting the nanofiltration membrane concentration technology comprises a first-stage nanofiltration concentrated water tank, a high-pressure pump, a pure water tank and a pure water high-pressure pump, and is characterized in that: a pressure gauge is arranged behind a valve behind the high-pressure pump, a section of nanofiltration membrane device is arranged at the water outlet end of the high-pressure pump, the section of nanofiltration membrane device consists of a nanofiltration membrane shell, the pressure gauge and a special high-pressure nanofiltration membrane element, a section of water production flowmeter is arranged at the rear end of the section of nanofiltration membrane device, a low-nitrate water desalination brine tank is arranged at the rear end of the section of water production flowmeter, the water outlet end of the pure water high-pressure pump is divided into three pipelines, dialysis water flow regulating valves are respectively arranged at the water outlet end of the pure water high-pressure pump, the three pipelines of the water outlet end of the pure water high-pressure pump are respectively communicated with the section of nanofiltration membrane device, the second section of nanofiltration membrane device and the third section of nanofiltration membrane device, the device comprises a first nanofiltration membrane device, a second nanofiltration membrane device, a third nanofiltration membrane device, a pressure gauge, a low-nitrate water desalination salt water tank, a second water production flow meter, a third nanofiltration membrane device and a high-nitrate water MVR water tank, wherein the second nanofiltration membrane device is communicated with the third nanofiltration membrane device, the pressure gauge is arranged, the pressure gauge, a concentrated water flow regulating valve, an energy recoverer and the concentrated water flow meter are sequentially arranged between the high-nitrate water MVR water tank and the third nanofiltration membrane device.
As a preferable technical scheme of the invention, valves are arranged at two ends of the first-stage nanofiltration concentrated water tank, a water supply pump is arranged at the rear end of the valve far away from the water inlet of the first-stage nanofiltration concentrated water tank, a security filter is arranged at the water outlet end of the water supply pump, pressure gauges are arranged at two ends of the security filter, a high-pressure pump is arranged at the water outlet end of the security filter, a valve is arranged between the high-pressure pump and the security filter, and a valve is arranged at the water outlet end of the high-pressure pump.
As a preferable technical scheme of the invention, valves are arranged at two ends of the pure water tank, a pure water supply pump is arranged at the rear end of the valve far away from the water inlet end of the pure water tank, a security filter is arranged at the rear end of the pure water supply pump, pressure gauges are fixedly arranged at two ends of the security filter, a pure water high-pressure pump is arranged at the water outlet end of the security filter, and a valve is arranged at the water outlet end of the high-pressure pump.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, by arranging a first-stage nanofiltration membrane device, a second-stage nanofiltration membrane device and a third-stage nanofiltration membrane device, pure water and brine are respectively supplemented by using three feed inlets, so that concentrated water (NaCl=205+/-10 g/L, na) subjected to first-stage nanofiltration is obtained 2 SO 4 Content of 60-88 g/L) is further concentrated, na thereof 2 SO 4 The concentration can reach 150-160g/L, and the concentration of Na is high 2 SO 4 The solution may be subjected to MVR evaporation crystallization to separate salts.
2. According to the invention, by arranging the nanofiltration membrane shell and the special high-pressure nanofiltration membrane element, sodium chloride can enter the dilute brine side through the nanofiltration membrane by utilizing the selective separation performance of the nanofiltration membrane, sodium sulfate is retained on the concentrated brine side of the membrane by nanofiltration, meanwhile, the sodium sulfate content on the concentrated side is higher and the sodium chloride content is lower, the total salt content of sodium sulfate, sodium chloride and the like is lower than 300g/L and lower than the saturated solubility, the fouling and fouling can not appear, the nanofiltration membrane element is blocked, the operation pressure is low in the nanofiltration membrane concentration process, and the selective separation effect of divalent salt is good.
3. The invention, through setting up pure water tank, pure water high-pressure pump and energy recoverer, its purpose: firstly, reduce sodium sulfate and sodium chloride and separate out the scale deposit dirt stifled risk of reduction high pressure nanofiltration membrane, secondly, adopt the energy recuperation ware, make full use of concentrate pressure, can save 35% energy consumption, the device operation is reliable and stable.
Drawings
FIG. 1 is a schematic diagram of the device connection of the present invention;
FIG. 2 is a schematic diagram of the process flow of the present invention.
In the figure: 1. a first-stage nanofiltration concentrated water tank; 2. a water supply pump; 3. a cartridge filter; 4. a high pressure pump; 5. a valve; 6. a nanofiltration membrane shell; 7. a pressure gauge; 8. a first section of produced water flowmeter; 9. a pure water tank; 10. pure water supply pump; 11. a special high-pressure nanofiltration membrane element; 12. pure water high-pressure pump; 13. a dialysis water flow regulating valve; 14. a second-stage water production flowmeter; 15. a two-stage nanofiltration membrane device; 16. a section of nanofiltration membrane device; 17. a three-section nanofiltration membrane device; 18. a three-stage water production flowmeter; 19. low-nitrate water desalination brine tank; 20. a concentrate flow regulating valve; 21. an energy recovery device; 22. a concentrated water flowmeter; 23. high-nitrate water goes to MVR water tank.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
Referring to fig. 1-2, the present invention provides the following technical solutions: adopt the concentrated device of high concentrated sodium sulfate solution of nanofiltration membrane concentration technique production, including one-level nanofiltration concentrate water tank 1, high-pressure pump 4, pure water tank 9 and pure water high-pressure pump 12, its characterized in that: a pressure gauge 7 is arranged behind a valve 5 behind the high-pressure pump 4, a section of nanofiltration membrane device 16 is arranged at the water outlet end of the high-pressure pump 4, the section of nanofiltration membrane device 16 consists of a nanofiltration membrane shell 6, the pressure gauge 7 and a special high-pressure nanofiltration membrane element 11, a section of water production flowmeter 8 is arranged at the rear end of the section of nanofiltration membrane device 16, a low-nitrate water desalination salt water tank 19 is arranged at the rear end of the section of water production flowmeter 8, the water outlet end of the pure water high-pressure pump 12 is divided into three pipelines, dialysis water flow regulating valves 13 are respectively arranged on the three pipelines at the water outlet end of the pure water high-pressure pump 12, the three pipelines are respectively communicated with the section of nanofiltration membrane device 16, the second section of nanofiltration membrane device 15 and the third section of nanofiltration membrane device 17, the section of nanofiltration membrane device 16 is communicated with the second section of nanofiltration membrane device 15, the device is provided with a pressure gauge 7, a second section nanofiltration membrane device 15 is communicated with a third section nanofiltration membrane device 17 and is provided with the pressure gauge 7, the second section nanofiltration membrane device 15 is communicated with a low-nitrate water desalination salt water tank 19 and is provided with a second section water production flow meter 14, the third section nanofiltration membrane device 17 is communicated with the low-nitrate water desalination salt water tank 19 and is provided with a third section water production flow meter 18, the second section nanofiltration membrane device 15 and the third section nanofiltration membrane are both composed of a nanofiltration membrane shell 6 and a special high-pressure nanofiltration membrane element 11, the third section nanofiltration membrane device 17 is communicated with a high-nitrate water desalination MVR water tank 23, and the pressure gauge 7, a permeable concentrated water flow regulating valve 20, an energy recoverer 21 and a concentrated water flow meter 22 are sequentially arranged between the high-nitrate water desalination MVR water tank 23 and the third section nanofiltration membrane device 17.
In this embodiment, the high pressure pump 4 and the pure water high pressure pump 12 are both used to increase the pressure of the liquid in the conveying pipeline, ensure the smooth circulation of the liquid, the valve 5 is used to control the circulation of the liquid in the pipeline, the valve 5 is arranged at multiple positions, so that under different conditions, the staff can control the circulation of the liquid by closing or opening the valve 5 at different positions, the first section of nanofiltration membrane device 16, the second section of nanofiltration membrane device 15 and the third section of nanofiltration membrane device 17 are sequentially connected, the separation and concentration of the input liquid are realized, meanwhile, the nanofiltration membrane is selected for special high pressure nanofiltration, has a binary selection separation performance high, the pressure resistance grade is 1200psi (8.27 MPa), and is divided into three sections, the three sections of design can be adjusted according to the actual treatment capacity, the applicability of the device is improved, the nanofiltration membrane shell 6 and the high pressure nanofiltration membrane element 11 both use the working principle of nanofiltration membranes, under a certain pressure, when the liquid stock flows across the membrane surface,the dense capillary pores on the surface of the nanofiltration membrane can make water and Cl - The small molecular substances permeate to become permeate liquid, and the volume of SO in the stock solution is larger than the nanofiltration pore diameter of the membrane surface 4 2- The high-nitrate water is trapped at the thick liquid side of the membrane and becomes concentrated liquid, thereby realizing the purposes of purifying, separating and concentrating the stock solution, the low-nitrate water desalination brine tank 19 has the function of temporary storage, the high-nitrate water desalination brine tank 23 enables the entered liquid to be subjected to MVR thermal salt separation process, and Na is produced 2 SO 4 The product, manometer 7, concentrate water flow regulator 20 and concentrate water flow meter 22 all play the detection to whole device running state, make the staff can the actual conditions carry out corresponding adjustment, energy recoverer 21 adopts the mode of energy recuperation, make full use of concentrate water pressure again, can save 35% energy, make whole device operation reliable and stable, the inside that one section receives filter membrane device 16, two sections receive filter membrane device 15 and three sections receive filter membrane device 17 all can be according to the condition of difference, install additional in the quantity of inside nanofiltration membrane shell 6, manometer 7 and special high pressure receive filter membrane element 11, deal with different actual production conditions.
Specifically, the both ends of one-level nanofiltration dense water tank 1 all are provided with valve 5, and the rear end of valve 5 that keeps away from one-level nanofiltration dense water tank 1 water inlet is provided with working shaft 2, and the play water end of working shaft 2 is provided with cartridge filter 3, and the both ends of cartridge filter 3 all are provided with manometer 7, and the play water end of cartridge filter 3 is provided with high-pressure pump 4, is provided with valve 5 between high-pressure pump 4 and the cartridge filter 3, and the play water end of high-pressure pump 4 is provided with valve 5.
In this embodiment, the first-stage nanofiltration concentrate tank 1 temporarily stores the dilute brine first-stage nanofiltration concentrate after the ion membrane electrolysis, the water supply pump 2 supplies the first-stage nanofiltration concentrate in the first-stage nanofiltration concentrate tank 1 to the high-pressure pump 4, the high-pressure pump 4 enhances the pressure of the first-stage nanofiltration concentrate, and the pressure of the first-stage nanofiltration concentrate is sent to the next process for relevant treatment, and the security filter 3 adopts a 5 μm PP cotton filter core to protect the nanofiltration membrane element from mechanical damage caused by the entry of tiny solid particles.
Specifically, the both ends of pure water tank 9 all are provided with valve 5, and the rear end of valve 5 that keeps away from the water inlet of pure water tank 9 is provided with pure water supply pump 10, and the rear end of pure water supply pump 10 is provided with cartridge filter 3, and the both ends of cartridge filter 3 all fixed mounting have manometer 7, and the play water end of cartridge filter 3 is provided with pure water high-pressure pump 12, and the play water end of high-pressure pump 4 is provided with valve 5.
In this embodiment, the pure water tank 9 provides temporary pure water storage, and the pure water supply pump 10 supplies the pure water temporarily stored in the pure water tank 9 to the pure water high pressure pump 12, and then the pure water high pressure pump 12 is pressurized and supplied to the next process, to perform the related operations.
Specifically, the method for producing the high-concentration sodium sulfate solution by adopting the nanofiltration membrane concentration technology comprises the following steps:
the first step: pretreating and cooling the dilute brine (the sodium chloride content is controlled to be 210+/-10 g/L, and the sodium sulfate is less than 20 g/L) after the ionic membrane electrolysis in the chlor-alkali industry, and reducing the temperature of the dilute brine from 60-70 ℃ to 40+/-3 ℃;
and a second step of: adding a reducing agent (sodium thiosulfate or sodium sulfite) according to the content of the dilute brine (1 ton of brine plus 0.1Kg of sodium thiosulfate or sodium sulfite), and removing sodium hypochlorite remained in the electrolytic process by utilizing a reduction reaction;
and a third step of: after the sodium hypochlorite is remained by the activated carbon filter, the sodium hypochlorite enters a first-stage nanofiltration device (nanofiltration membrane has selective permeability to divalent ions), and the NaCl=210+/-10 g/L and Na of the light salt water component are controlled 2 SO 4 The operation pressure of the first-stage nanofiltration membrane device, the second-stage nanofiltration membrane device and the third-stage nanofiltration membrane device is 20-28Bar, the first-stage nanofiltration recovery rate is 60-85%, and the flux of the nanofiltration membrane element is 18-25L/m 2 H, separating the separated lean-nitrate light brine NaCl=210+/-10 g/L, na 2 SO 4 Less than 1g/L, directly entering a production process to dissolve crude salt or injecting the crude salt into an underground mine for recycling;
fourth step: high-nitrate strong brine NaCl=205+ -10 g/L, na of first-stage nanofiltration device 2 SO 4 The content of 60-88g/L enters a super concentration nanofiltration device, the super concentration nanofiltration device comprises a first section nanofiltration membrane device, a second section nanofiltration membrane device and a third section nanofiltration membrane device, the running pressure is 55-60Bar, and the flux of the high-pressure nanofiltration membrane element is 12-18L/m 2 H, supplementing 1/3 of pure water to dialyze sodium chloride during concentration to improve the quality of sodium sulfateThe ratio of the sodium sulfate to sodium chloride is reduced, so that the high-concentration sodium sulfate to 150-160g/L and the NaCl content is less than 150g/L are realized. After separation, the NaCl of the lean and light salt water is more than 150g/L, na 2 SO 4 Less than 5g/L, directly entering a production process to dissolve crude salt or injecting the crude salt into an underground mine for recycling;
fifth step: concentrated liquid high-nitrate water of the super-concentration nanofiltration device enters direct MVR for evaporative crystallization to produce high-purity Na 2 SO 4 Mirabilite product.
Case one:
the first step: taking 100 tons of dilute brine (with the content of 213.2g/L of sodium chloride and 8.60g/L of sodium sulfate) after ion membrane electrolysis, wherein the flow rate of the dilute brine is 20.0m 3 Reducing the temperature from 65 ℃ to 41 ℃ through condensed water;
and a second step of: adding 10.0kg sodium sulfite, and removing sodium hypochlorite remained in the electrolytic process by utilizing a reduction reaction;
and a third step of: after passing through an activated carbon filter, the mixture enters a first-stage nanofiltration device, and the light salt water component NaCl=213.2 g/L and Na is controlled 2 SO 4 At 8.60g/L, the operating pressure of the first-stage nanofiltration device is 24.8Bar, and the flux of nanofiltration membrane elements is 20.4L/m 2 H, 89.8m of separated lean-nitrate light brine 3 ,NaCl=214.1g/L，Na 2 SO 4 =0.63 g/L, directly entering into production and dissolution of crude salt or injection into underground mine for recycling;
fourth step: first-stage nanofiltration high-nitrate strong brine 10.2m 3 ,NaCl=205.4g/L，Na 2 SO 4 The mixture is controlled to be 78.86g/L and enters a super-concentration nanofiltration device, the operation pressure of the super-concentration nanofiltration device is 58.6Bar, and the water yield is 14.7L/m 2 H, continuously supplementing pure water for 3.0m total 3 The device produces 8.2m of light brine 3 Its component NaCl= 167.2g/L, na 2 SO 4 4.54g/L, directly entering into production of dissolved crude salt or injecting into an underground mine for recycling;
fifth step: super concentrated nanofiltration device high nitrate water 5.0m 3 Its component NaCl=144.9 g/L, na 2 SO 4 153.1g/L, high-nitrate strong brine MVR evaporation crystallization salt separation, obtaining 760Kg Na 2 SO 4 The yield of the product was 88.4%. Reduced by 5.2m 3 The evaporation capacity is saved by 50.98 percent, sodium chloride and nanofiltration membrane permeate light brine to return to the production process, and the utilization rate is 100 percent.
And a second case:
the first step: taking 100 tons of dilute brine (containing 209.7g/L of sodium chloride and 13.86g/L of sodium sulfate) after ion membrane electrolysis, wherein the flow rate of the dilute brine is 20.0m3/h, and cooling the dilute brine to 41.7 ℃ from 65 ℃ through condensed water;
and a second step of: adding 10.0kg sodium sulfite, and removing sodium hypochlorite remained in the electrolytic process by utilizing a reduction reaction;
and a third step of: after passing through an active carbon filter, the water enters a first-stage nanofiltration device, and the light salt water component NaCl= 209.7g/L and Na is controlled 2 SO 4 At 13.86g/L, the operating pressure of the first-stage nanofiltration device is 27.8Bar, and the flux of nanofiltration membrane elements is 18.2L/m 2 H, separating the separated lean-nitrate light brine 83.4m 3 ,NaCl=210.9g/L，Na 2 SO 4 =0.68 g/L, directly entering into production and dissolution of crude salt or injection into underground mine for recycling;
fourth step: first-stage nanofiltration high-nitrate strong brine 16.6m 3 ,NaCl=203.7g/L，Na 2 SO 4 79.08g/L, and the water enters a super-concentration nanofiltration device, the operation pressure of the super-concentration nanofiltration device is 59.2Bar, and the water yield is 14.2L/m 2 H, continuously supplementing pure water for 5.4m in total 3 The device produces 14.0m of light brine 3 Its component NaCl=162.3 g/L, na 2 SO 4 4.47g/L, directly entering into production of dissolved crude salt or injecting into underground mine for recycling;
fifth step: super concentrated nanofiltration device high nitrate water 8.0m 3 Its component NaCl=139.6 g/L, na 2 SO 4 =156.0g/L, high-nitrate strong brine MVR evaporation crystallization salt separation, 1236.4Kg Na 2 SO 4 The yield of the product was 89.2%. Reduced by 8.6m 3 The evaporation capacity is saved by 51.8 percent, sodium chloride and nanofiltration membrane permeate light brine to return to the production process, and the utilization rate is 100 percent.
The working principle and the using flow of the invention are as follows: after the equipment is started, the dilute brine after the ion membrane electrolysis passes through the first-stage nanofiltration concentrated water tank 1Temporary storage is carried out, pure water enters a pure water tank 9 for temporary storage, fresh brine is fed onto a high-pressure pump 4 through a water supply pump 2 for pressurized conveying, the pressure in a pipeline is ensured, the pressurized fresh brine is subjected to denitration through a first-stage nanofiltration membrane device 16, a second-stage nanofiltration membrane device 15 and a third-stage nanofiltration membrane device 17, the concentrated fresh brine is respectively fed into a low-nitrate water desalination water tank 19 and a high-nitrate water MVR water tank 23 for temporary storage, the pure water is fed into a pure water high-pressure pump 12 for pressurized through a pure water supply pump 10, the pressurized pure water is respectively fed into the first-stage nanofiltration membrane device 16, the second-stage nanofiltration membrane device 15 and the third-stage nanofiltration membrane device 17, the scaling and blocking risks of high-pressure nanofiltration membranes are reduced due to precipitation of sodium sulfate and sodium chloride, and the salt blockage of the high-pressure nanofiltration membranes are reduced, and the liquid entering the high-nitrate water MVR water tank 23 is subjected to MVR thermal salt separation process to produce sodium sulfate (Na 2 SO 4 ) And (5) a product.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The method for producing the high-concentration sodium sulfate solution by adopting the nanofiltration membrane concentration technology comprises the following steps:
the first step: taking 100 tons of dilute brine after ion membrane electrolysis; sodium chloride content 209.7g/L and sodium sulfate content 13.86g/L in the light brine; the flow rate of the dilute brine is 20.0m 3 And/h, cooling to 41.7 ℃ from 65 ℃ through condensed water;
and a second step of: adding 10.0kg of sodium sulfite, and removing sodium hypochlorite remained in the electrolytic process by utilizing a reduction reaction;
and a third step of: after passing through an active carbon filter, the water enters a first-stage nanofiltration device, and the light salt water component NaCl= 209.7g/L and Na is controlled 2 SO 4 At 13.86g/L, the operating pressure of the primary nanofiltration device is 27.8Bar, and the nanofiltration device is nanoThe flux of the filter membrane element is 18.2L/m 2 H, 83.4m of separated lean-nitrate light brine 3 ，NaCl=210.9g/L，Na 2 SO 4 =0.68 g/L, directly entering into production and dissolution of crude salt or injection into underground mine for recycling;
fourth step: first-stage nanofiltration high-nitrate strong brine 16.6m 3 ，NaCl=203.7g/L，Na 2 SO 4 79.08g/L, and enters a super-concentration nanofiltration device, wherein the operation pressure of the super-concentration nanofiltration device is 59.2Bar, and the water yield is 14.2L/m 2 H, continuously supplementing pure water for 5.4m in total 3 The device produces 14.0m of light brine 3 Its component NaCl=162.3 g/L, na 2 SO 4 4.47g/L, directly entering into production of dissolved crude salt or injecting into underground mine for recycling;
fifth step: super concentrated nanofiltration device high nitrate water 8.0m 3 Its component NaCl=139.6 g/L, na 2 SO 4 =156.0g/L, high-nitrate strong brine MVR evaporation crystallization salt separation, 1236.4Kg Na 2 SO 4 The yield of the product is 89.2%, and the yield is reduced by 8.6m 3 The evaporation capacity is saved by 51.8 percent, sodium chloride and nanofiltration membrane permeate light brine to return to the production process, and the utilization rate is 100 percent.
2. Adopt the concentrated device of high concentrated sodium sulfate solution of nanofiltration membrane concentration technique production, including one-level nanofiltration concentrate water tank (1), high-pressure pump (4), pure water tank (9) and pure water high-pressure pump (12), its characterized in that: the back of the valve (5) behind the high-pressure pump (4) is provided with a pressure gauge (7), the water outlet end of the high-pressure pump (4) is provided with a section of nanofiltration membrane device (16), the section of nanofiltration membrane device (16) consists of a nanofiltration membrane shell (6), the pressure gauge (7) and a special high-pressure nanofiltration membrane element (11), the back end of the section of nanofiltration membrane device (16) is provided with a section of water production flowmeter (8), the back end of the section of water production flowmeter (8) is provided with a low-nitrate water desalination water tank (19), the water outlet end of the pure water high-pressure pump (12) is divided into three pipelines, and the three pipelines of the water outlet end of the pure water high-pressure pump (12) are respectively provided with a dialysis water flow regulating valve (13), the three pipelines of the water outlet end of the pure water high-pressure pump (12) are respectively communicated with the section of nanofiltration membrane device (16), the second section of nanofiltration membrane device (15) and the third section of nanofiltration membrane device (17), the second section of nanofiltration membrane device (16) is communicated with the second section of nanofiltration membrane device (15) and the pressure gauge (7), the second section of nanofiltration membrane device (15) is provided with the pressure gauge (7), the second section of water production desalination device (19) is communicated with the third section of water tank (19), the second section of nanofiltration membrane device (17) is communicated with the third section of water tank (19), the two-section nanofiltration membrane device (15) and the three-section nanofiltration membrane are composed of a nanofiltration membrane shell (6) and a special high-pressure nanofiltration membrane element (11), the three-section nanofiltration membrane device (17) is communicated with a high-nitrate water MVR removal water tank (23), and a pressure gauge (7), a concentrate water flow regulating valve (20), an energy recoverer (21) and a concentrate water flow meter (22) are sequentially arranged between the high-nitrate water MVR removal water tank (23) and the three-section nanofiltration membrane device (17).
3. The apparatus for producing high-concentration sodium sulfate solution by nanofiltration membrane concentration technology according to claim 2, wherein: the utility model discloses a high-pressure water pump, including concentrated water tank, high-pressure pump (4) and safety filter (3), the both ends of one-level nanofiltration concentrate water tank (1) all are provided with valve (5) the rear end of valve (5) of keeping away from the concentrated water tank (1) water inlet is provided with working shaft (2), the play water end of working shaft (2) is provided with safety filter (3), the both ends of safety filter (3) all are provided with manometer (7), the play water end of safety filter (3) is provided with high-pressure pump (4), be provided with valve (5) between high-pressure pump (4) and the safety filter (3), the play water end of high-pressure pump (4) is provided with valve (5).
4. The apparatus for producing high-concentration sodium sulfate solution by nanofiltration membrane concentration technology according to claim 2, wherein: the utility model discloses a pure water pump, including pure water tank (9), valve (5) are all provided with at the both ends of pure water tank (9), the rear end of valve (5) of the water inlet end of keeping away from pure water tank (9) is provided with pure water supply pump (10), the rear end of pure water supply pump (10) is provided with cartridge filter (3), the both ends of cartridge filter (3) are all fixed mounting has manometer (7), the play water end of cartridge filter (3) is provided with pure water high-pressure pump (12), the play water end of high-pressure pump (4) is provided with valve (5).
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