CN107720782A - A kind of technique and system for use in carrying for dividing salt preparing potassium sulfate from high-salt wastewater - Google Patents
A kind of technique and system for use in carrying for dividing salt preparing potassium sulfate from high-salt wastewater Download PDFInfo
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- CN107720782A CN107720782A CN201710985171.8A CN201710985171A CN107720782A CN 107720782 A CN107720782 A CN 107720782A CN 201710985171 A CN201710985171 A CN 201710985171A CN 107720782 A CN107720782 A CN 107720782A
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- 239000002351 wastewater Substances 0.000 title claims abstract description 46
- 229910052939 potassium sulfate Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 40
- 150000003839 salts Chemical class 0.000 title claims abstract description 40
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 title claims abstract description 39
- 235000011151 potassium sulphates Nutrition 0.000 title claims abstract description 32
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 93
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000001728 nano-filtration Methods 0.000 claims abstract description 54
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 47
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 45
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 43
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 33
- 239000012452 mother liquor Substances 0.000 claims abstract description 24
- 238000001471 micro-filtration Methods 0.000 claims abstract description 22
- 239000011780 sodium chloride Substances 0.000 claims abstract description 22
- 239000012528 membrane Substances 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 19
- 238000002425 crystallisation Methods 0.000 claims abstract description 18
- 230000008025 crystallization Effects 0.000 claims abstract description 18
- 239000005416 organic matter Substances 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 239000001103 potassium chloride Substances 0.000 claims abstract description 16
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000005649 metathesis reaction Methods 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 35
- 238000000926 separation method Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 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 14
- 239000000126 substance Substances 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 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 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 8
- 229910001385 heavy metal Inorganic materials 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 5
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910001424 calcium ion Inorganic materials 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000003610 charcoal Substances 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000006385 ozonation reaction Methods 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 241000370738 Chlorion Species 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 2
- 238000001694 spray drying Methods 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 2
- 238000001816 cooling Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011591 potassium Substances 0.000 abstract description 6
- 229910052700 potassium Inorganic materials 0.000 abstract description 6
- 238000001223 reverse osmosis Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 239000003245 coal Substances 0.000 description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 238000004064 recycling Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 239000010842 industrial wastewater Substances 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000007832 Na2SO4 Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241001086438 Euclichthys polynemus Species 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- -1 basicity Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing Methods 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
- C01D5/06—Preparation of sulfates by double decomposition
- C01D5/08—Preparation of sulfates by double decomposition with each other or with ammonium sulfate
-
- 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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of technique of zero discharge and its processing system from high slat-containing wastewater preparing potassium sulfate, the system includes tubular type Microfiltration Unit, weak acid resin except hard unit, nanofiltration film unit, nanofiltration concentrated water matter-water-organic matter purification unit, nanofiltration concentrated water high-pressure membrane upgrading unit, nanofiltration concentrated water preparing potassium sulfate system, nanofiltration production water high-pressure membrane concentration systems etc..The waste water that hard unit is removed by tubular type Microfiltration Unit, weak acid resin tentatively divides salt using nanofiltration, nanofiltration produces water and obtains NaCl of the purity not less than 98.5% through film concentration and evaporative crystallization, sodium sulphate is mainly contained through high pressure reverse osmosis concentration after the purifying of nanofiltration concentrated water, carrying out metathesis reaction as raw material and potassium chloride obtains more than 92% K2SO4, so as to which sodium sulphate is converted into potassium product, solve the problems, such as a point market for sodium sulphate caused by salt process, last a small amount of mother liquor solidifies by being spray-dried, while reaches wastewater zero discharge.
Description
Technical field
The present invention relates to a kind of high slat-containing wastewater to divide salt resource technology, in particular it relates to a kind of from high salt
The technique of zero discharge of waste water preparing potassium sulfate and the system equipment for realizing this technique.
Background technology
Shortage of water resources and environmental capacity of water deficiency, are the important bottlenecks for restricting certain areas Modern Coal-based Chemical industry development
Problem.Wherein, highly concentrated saline treatment and emission problem, it is one of significant challenge that industry development faces.Waste water zero emission solution
Certainly scheme is to crack Modern Coal-based Chemical industry development and the important channel of water resource and environment contradiction.However, traditional waste water
The crystallization carnallite that " zero " discharges by-product is worth without recycling, is easily met water leaching drip and is oozed out, secondary pollution risk be present, and useless
In water treatment procedure, micro heavy ion and residual organic matter in water constantly concentrate, and may eventually enter into crystallization salt slurry
In so that crystal salt may have the hazard property of hazardous waste, and therefore, the Environmental Safety disposal of crystallization carnallite faces choosing for sternness
One of the problem of war is Modern Coal-based Chemical industry development urgent need to resolve.
In order to crack this problem, carry out the exploitation of crystal salt application technology as the second resource, effectively, economical, efficiently recovery is high
Sodium chloride and sodium sulphate in strong brine, recycling recycling is carried out as product, to realize《Modern Coal-based Chemical is built
If project environment entry criteria (tentative)》Environmental protection demonstration require that turning into industry needs one of problem for solving.
But because the sodium sulphate economic value of crystal salt recycling is not high, market is perplex crystal salt recycling one
Problem.If sodium sulphate is converted to and is worth higher potassium sulfate fertilizer, the market problem of sodium sulphate is not only solved, and
Because the value of potassium sulfate is higher than potassium chloride, it is possible to coal chemical industry is combined with salt chemical engineering industry, is the zero of coal chemical industry
Discharge crystal salt finds technically reliable, economically viable outlet.
Chinese patent application 201610072833.8 discloses a kind of system that potassium sulfate is prepared using high salt industrial wastewater
And its technique, tentatively divide high-salt wastewater to salt by nanofiltration, after Re Fa or freezing production saltcake, recycle saltcake to prepare sulphur
Sour potassium.
Chinese patent application 201610072782.9 discloses a kind of high saliferous Industry Waste moisture salt Zero discharging system, by height
Salt waste water tentatively divides salt by nanofiltration, and Re Fa or freezing production sodium chloride and sulfuric acid is respectively adopted in the concentrated water and production water to nanofiltration
Sodium.
However, a point salt is carried out using the technical scheme of the above, otherwise it can only obtain economic value not high sodium sulphate and chlorine
Change sodium, market is problematic, and particularly sodium sulphate gets nowhere substantially；Obtained sodium sulphate or saltcake must be converted again
For potassium sulfate, if first preparing saltcake, potassium sulfate then is prepared using saltcake, it is high to freeze the saltcake energy consumption of production, if with
Sodium sulphate prepares potassium sulfate, it is necessary to be dissolved in water again, again evaporative crystallization, technological process length, high energy consumption.
Therefore, finding one kind can be by high-salt wastewater salinity recycling, and the not high sodium sulphate of economic value is passed through low
The method of energy consumption is converted into potassium sulfate, has both solved the problem of outlet of sodium sulphate, has also solved the problems, such as high energy consumption, is to need to solve in the industry
Technical problem certainly.
The content of the invention
Present invention aim to solve high saliferous industrial wastewater " zero-emission " and recycling sodium sulphate in the prior art
The problem of economic value is low, sodium sulphate is converted into potassium sulfate.
To realize the object of the invention, on the one hand, the invention provides a kind of zero-emission from high-salt wastewater preparing potassium sulfate
Technique, wherein, the technique comprises the following steps：
(1) high-salt wastewater is pumped into Microfiltration Unit by raw water, and by adding sodium carbonate and sodium hydroxide, removed big
Part calcium ions and magnesium ions, silicon, heavy metal and suspension and partial organic substances；
(2) high-salt wastewater after micro-filtration softens is sent into weak acid resin and removes hard unit, further reduce the hard of waste water
Degree, basicity；
(3) high-salt wastewater after weak acid resin softens is divided to salt by the preliminary of NF membrane, high-salt wastewater is divided into two
Stock, that is, water side and concentrated water side are produced, wherein, production water side salinity is mainly sodium chloride and minimal amount of sodium sulphate, concentrated water side salinity master
If sodium sulphate and partial oxidation sodium；
(4) production water obtained by above-mentioned nanofiltration membrane treatment is concentrated and evaporative crystallization obtains that purity is higher (to be such as not less than by film
98.5%) NaCl, a small amount of mother liquor discharge into capable spray drying outside, last carnallite are solidified；
(5) after the concentrated water obtained by above-mentioned nanofiltration membrane treatment being removed into most of organic matter by matter-water-organic matter purification system, warp
Cross film and be concentrated to more than TDS160000mg/L；
(6) by being mixed with additional solid potassium chloride metathesis reaction, evaporative removal occur for the concentrate of nanofiltration concentrated water
Part water, part K is obtained by dewaterer separation of solid and liquid2SO4Product；
(7) output K is separated out through step (6)2SO4Mother liquor carries out multiple reaction with additional solid sodium sulfate or saltcake, obtains potassium
Saltcake and partial mother liquid, mother liquor arrange disposal outside；
(8) glaserite and additional solid potassium chloride and part aqueous solution is added, metathesis reaction occurs again, generates
K2SO4, part K is obtained by dewaterer separation of solid and liquid2SO4Product, and mother liquor then return to step (7), caused by step (6)
Mother liquor mixes, and carries out multiple reaction with additional solid sodium sulfate or saltcake, is obtained after evaporative crystallization, by dewaterer separation of solid and liquid
Part K2SO4Product, so circulation；
(9) chlorination mother liquid of sodium and potassium sulfate mother liquid mixing are spray-dried, and last carnallite is solidified, realized
Zero-emission.
The method of the invention described above carries out a point salt by the continuous nanofiltration system being arranged in membrane separation concentration unit, and
Using the technique of the direct preparing potassium sulfate of high concentration sodium sulfate concentrated water, to realize sodium chloride, sodium sulphate in high saliferous industrial wastewater
Separation, while sodium sulphate is converted into the higher potassium sulfate of economic value, while the zero-emission for the waste water realized.
The present invention process the step of in (1), the circulation fluid of micro-filtration intermittent can enter dewaterer and be dehydrated, at sludge outward transport
Put.Handled by microfiltration systems, the hardness, heavy metal and silicon in haline water largely precipitate, while produce the suspension of water
Concentration is extremely low, typically can main road turbidity≤0.5NTU, total hardness≤50mg/L (calcium carbonate), SiO2≤10mg/L, ensure that
The stable operation of nanofiltration system.
Preferably, the pretreating process of step (1) uses tube type filter membrance TMF techniques, to go the easy fouling in water removal
Calcium, magnesium, the easy scale forming matter such as silicon, reduce the fouling and pollution problem of follow-up membranous system and evaporative crystallization technique, it is used
System include reaction tank, concentration basin, microfiltration membranes and other corollary equipments etc..Micro-filtration is using the film of micropore the precipitation in waste water
Thing is separated, and the dirt for washing away mitigation film circulated by big flow is blocked up, and circular flow may generally be the 60-80 of processing water
Times.
The present invention process the step of in (2), total hardness≤5mg/L (calcium carbonate) for softening by weak acid, after avoiding
Continuous system produces the fouling of calcium salt, while further improves the crystallization purity salt that follow-up system is produced.
Preferably, the calcium and magnesium hardness of waste water is removed completely using weak acid resin hard-removal system in step (2), weak acid resin
Operational mode be sodium form, it is it is possible to prevente effectively from the high salinity of waste water removes hard performance impact to resin.Wherein, weak acid resin is first
After 5% HCl regeneration, continue the NaOH transition with 5%, the water hardness that goes out of weak acid resin is controlled in below 5mg/L.
In the technique of the present invention, nanofiltration water inlet TDS is can be controlled in 20,000 or so, tentatively divides salt, nanofiltration by nanofiltration
It is more than 98% to sulfate radical rejection to chlorion without rejection.
Preferably, in the technique of the present invention, the concentrated water purifyingization system of nanofiltration also includes catalytic ozonation and activity
Charcoal adsorbs.
In the technique of the present invention, the nanofiltration concentrate after purifying and film concentrates, the strong brine salt content TDS of concentration
≥160000mg/L。
The forming steps of potassium sulfate are mixed using nanofiltration concentrate with KCl solids, and by evaporative removal part water, can be dropped
Temperature passes through centrifuge separation of solid and liquid generating portion K to 20-30 DEG C2SO4；Separation of solid and liquid Mother liquor is mixed with additional sulfuric acid sodium or saltcake
Close, and pass through evaporative crystallization, 20-30 DEG C can be cooled to, glaserite is generated by centrifuge separation of solid and liquid；Separation of solid and liquid generating unit
Point glaserite and additional KCl secondary response again, 20-30 DEG C can be cooled to, pass through centrifuge separation of solid and liquid generating portion K2SO4；Gu
Mother liquor after liquid separation generating portion glaserite, mixed salt outward transport disposal is gone out by evaporative crystallization.
It is worth noting that, in the technique of the invention described above, can be to the order of some processes step according to specific occasion
It is adjusted.
On the other hand, in order to realize the purpose of the present invention, present invention also offers a kind of high salt for above-mentioned technique to give up
Water treatment system, the system include：
Tubular type Microfiltration Unit, its be used to remove in high-salt wastewater most of calcium ions and magnesium ions, silicon, heavy metal and suspension and
Partial organic substances；
Weak acid resin removes hard unit, and it is used for the hardness, the basicity that further reduce high-salt wastewater；
Nanofiltration film unit, it is used for the preliminary of high-salt wastewater and divides salt, and high-salt wastewater is divided into two strands, that is, produces water side and concentrated water
Side, wherein, production water side salinity is mainly sodium chloride and minimal amount of sodium sulphate, and concentrated water side salinity is mainly sodium sulphate and part chlorine
Change sodium；
Nanofiltration concentrated water matter-water-organic matter purification unit, it is used for the waste water removal after NF membrane cell processing is most of organic
Thing；
Nanofiltration concentrated water high-pressure membrane upgrading unit；
Nanofiltration concentrated water preparing potassium sulfate system；
Water high-pressure membrane concentration systems are produced in nanofiltration；
Water multiple-effect crystal system is produced in nanofiltration；And
Carnallite crystal system.
Preferably, in the system of the present invention, tubular type Microfiltration Unit include reaction tank, concentration basin, microfiltration membranes and other match somebody with somebody
Complete equipment.
Preferably, in the system of the present invention, nanofiltration concentrated water matter-water-organic matter purification unit includes catalytic ozonation and activity
Charcoal adsorbs.
Divide salt technique compared to other zero-emissions in the prior art, technical scheme has the advantage that and had
Beneficial effect：
A, sodium sulphate is converted to and is worth higher potassium sulfate (chemical fertilizer), not only solve the market problem of sodium sulphate, and
And it is the zero of coal chemical industry so as to which coal chemical industry is combined with salt chemical engineering industry because the value of potassium sulfate is higher than potassium chloride
Discharge crystal salt finds technically reliable, economically viable outlet；
B, the concentrate of sodium sulphate is directly generated into potassium sulfate with chlorination nak response, solves and pass through from high slat-containing wastewater
Evaporation or freezing first prepare sodium sulphate or saltcake comes out, and then add water convert high energy consumption, the long flow path of potassium sulfate the problem of；
C, potassium sulfate is produced using two step reflux techniques, the rate of recovery of potassium can be made to reach more than 84%, solved to greatest extent
Determine the problem of preparing potassium lost during potassium sulfate process.
Below, the present invention is described in detail with reference to the drawings and specific embodiments, but this explanation is not
Limiting the scope of the invention.One of ordinary skill in the art should be understood that certain in the specific embodiment of the invention
A little processing steps and device therefor, the implementation for suitably adjusting or replacing without influenceing the present invention can be carried out completely.
Brief description of the drawings
Fig. 1 is the separating sodium sulfate from high-salt wastewater and sodium chloride and the process chart for preparing potassium sulfate of the present invention.
Embodiment
Referring to Fig. 1, process of the invention can be embodied as follows：
1) high-salt wastewater is pumped into Microfiltration Unit by raw water, by adding sodium carbonate and sodium hydroxide, removes most of
Calcium ions and magnesium ions, silicon, heavy metal and suspension and partial organic substances, the intermittent dewaterer that enters of the circulation fluid of micro-filtration is dehydrated, dirty
Mud outward transport disposal.Handled by microfiltration systems, the hardness, heavy metal and silicon in haline water largely precipitate, while produce water
Concentration of suspension it is extremely low, general turbidity≤0.5NTU, total hardness≤50mg/L (calcium carbonate), SiO2≤ 10mg/L, ensure
The stable operation of nanofiltration system.
2) haline water after micro-filtration softens is sent into weak acid resin except hard unit, further by the hardness of waste water, basicity, warp
Total hardness≤5mg/L (calcium carbonate) of weak acid softening is crossed, avoids follow-up system from producing the fouling of calcium salt, while further improve
The crystallization purity salt that follow-up system is produced.
3) haline water after weak acid resin softens divides salt by the preliminary of NF membrane, and haline water is divided into two strands, that is, produced
Water side is mainly sodium chloride and minimal amount of sodium sulphate, and concentrated water side is mainly sodium sulphate and partial oxidation sodium.
4) nanofiltration production water is concentrated by film and evaporative crystallization obtains the NaCl that purity is not less than 98.5%, is arranged outside a small amount of mother liquor
It is spray-dried, last carnallite is carried out into solidification puts.
5) after the concentrated water of nanofiltration removes most of organic matter by matter-water-organic matter purification system, it is concentrated to by film
More than TDS160000mg/L.
6) by being mixed with additional solid potassium chloride metathesis reaction, evaporative removal portion occur for the concentrate of nanofiltration concentrated water
Divide water, part K is obtained by dewaterer separation of solid and liquid2SO4Product.
7) by 6) separating out output K2SO4Mother liquor carries out multiple reaction with additional solid sodium sulfate or saltcake, obtains glaserite
And partial mother liquid, mother liquor arrange disposal outside.
8) glaserite and additional solid potassium chloride and part aqueous solution is added, metathesis reaction occurs again, generates K2SO4,
Part K is obtained by dewaterer separation of solid and liquid2SO4Product, and mother liquor then returns to the 7) step, with 6) caused by mother liquor mix, with
Additional solid sodium sulfate or saltcake carry out multiple reaction, are evaporated after crystallization and obtain part K by dewaterer separation of solid and liquid2SO4
Product, so circulation.
9) chlorination mother liquid of sodium and potassium sulfate mother liquid mixing are spray-dried, and last carnallite is solidified, realized
Zero-emission.
Embodiment
By taking the high saliferous Industry Waste moisture salt zero-emission project (treating capacity 195m3/h) of certain coal chemical industry enterprises as an example, use
Above-mentioned high saliferous Industry Waste moisture salt technique of zero discharge and system are handled.
Wherein, the mean concentration of high each pollutant of saliferous industrial wastewater is as follows：
Table 1
By pretreatment system include tubular type microfiltration systems, weak acid resin hard-removal system by the hardness of waste water, basicity, silicon,
Fluorine ion and suspension, the water quality of high-salt wastewater is as follows after pretreatment system：
Table 2
By the salt treatment of dividing of nanofiltration, production water side salinity is mainly sodium chloride, and concentrated water side salinity is mainly sodium chloride and sulphur
Sour sodium, water quality are as follows：
Table 3
| Project | Nanofiltration concentrated water | Water is produced in nanofiltration |
| Na2SO4(mg/L) | 63409.68 | 292.81 |
| NaCl(mg/L) | 11567.67 | 11567.67 |
| CODcr(mg/L) | 223.125 | 10.625 |
| SiO2(mg/L) | 15 | 15 |
| TDS(mg/L) | 75238.13 | 11918.07 |
| Flow (m3/h) | 29.25 | 165.75 |
It is mainly sodium chloride by the production water side salinity divided after salt of nanofiltration, is crystallized by multiple-effect evaporation, is steamed by controlling
Hair amount, avoid sodium chloride and sodium sulphate eutectoid, may finally obtain 3312.54Kg/h, the NaCl solids of more than 97% purity and
Partial mother liquid, mother liquor composition are as follows：
Table 4
Divide salt concentrated water side salinity to be mainly sodium sulphate by nanofiltration, pass through matter-water-organic matter purification unit, including ozone catalytic
Oxidation and charcoal absorption, the clearance of organic matter is 60%, i.e. COD is reduced to 93.25mg/l by 223.125mg/l.
Nanofiltration concentrated water after matter-water-organic matter purification unit is concentrated using disc-type counter-infiltration, and water quality is as follows：
Table 5
By the Na containing 15.43% NaCl and 84.57% of disc-type reverse osmosis concentration2SO4, consolidate with 1.8T/H
Body KCL is mixed, and metathesis reaction is carried out in conversion reactor 1, and is concentrated by evaporator evaporation, removes 4.5T/h's
Water, solution be cooled to 25 DEG C after by dewaterer separation of solid and liquid, obtain 1.2t/h K2SO4Solid, mother liquor composition are as follows：
Table 6
Mother liquor by above-mentioned separation of solid and liquid mixes with additional 2.3T/H sodium sulphate, is carried out in conversion reactor 2
Metathesis reaction, glaserite mixed liquor is obtained, 2.5t/H glaserites solid and reaction are obtained by centrifugal dehydrator separation of solid and liquid
Raffinate, the composition of raffinate include：NaCl1.2t/h, Na2SO40.9t/h, KCl0.3t/h, other carnallites and organic matter 0.1Kg/
H, remnants realize zero-emission by being spray-dried solidification.
The glaserite of above-mentioned precipitation is mixed with additional 2.3T/H KCl, and adds the dissolving of 3.2T/H water, glaserite and KCl
Metathesis reaction occurs in conversion reactor 3, generates K2SO43.4/H and 5.9/H mother liquor, mother liquor return, so circulation.
By two step metathesis reactions, reaction consumption 4.1T/h potassium chloride obtains 5.18T/H potassium sulfate, and potassium returns
Yield is 84%, while obtains 3.5T/h sodium chloride and 1.2T/H carnallite, and carnallite sends disposal outside.
Claims (9)
1. a kind of technique of zero discharge from high-salt wastewater preparing potassium sulfate, wherein, the technique comprises the following steps：
(1) high-salt wastewater is pumped into Microfiltration Unit by raw water, and by adding sodium carbonate and sodium hydroxide, removed most of
Calcium ions and magnesium ions, silicon, heavy metal and suspension and partial organic substances；
(2) high-salt wastewater after micro-filtration softens is sent into weak acid resin and removes hard unit, further reduce the hard of high-salt wastewater
Degree, basicity；
(3) high-salt wastewater after weak acid resin softens is divided to salt by the preliminary of NF membrane, high-salt wastewater is divided into two strands, i.e.,
Water side and concentrated water side are produced, wherein, production water side salinity is mainly sodium chloride and minimal amount of sodium sulphate, and concentrated water side salinity is mainly sulphur
Sour sodium and partial oxidation sodium；
(4) production water obtained by above-mentioned nanofiltration membrane treatment is concentrated by film and evaporative crystallization obtains purity higher NaCl, Shao Liangmu
Capable spray drying is discharged into outside liquid, last carnallite is solidified；
(5) after the concentrated water obtained by above-mentioned nanofiltration membrane treatment being removed into most of organic matter by matter-water-organic matter purification system, by film
It is concentrated to more than TDS160000mg/L；
(6) by being mixed with additional solid potassium chloride metathesis reaction, evaporative removal part occur for the concentrate of nanofiltration concentrated water
Water, part K is obtained by dewaterer separation of solid and liquid2SO4Product；
(7) output K is separated out through step (6)2SO4Mother liquor carries out multiple reaction with additional solid sodium sulfate or saltcake, obtains glaserite
And partial mother liquid, mother liquor arrange disposal outside；
(8) glaserite and additional solid potassium chloride and part aqueous solution is added, metathesis reaction occurs again, generates K2SO4, warp
Cross dewaterer separation of solid and liquid and obtain part K2SO4Product, and mother liquor then return to step (7), with step (6) caused by mother liquor mix,
And carry out multiple reaction with additional solid sodium sulfate or saltcake, obtain part K after evaporative crystallization, by dewaterer separation of solid and liquid2SO4
Product, so circulation；
(9) chlorination mother liquid of sodium and potassium sulfate mother liquid mixing are spray-dried, and last carnallite is solidified, realizes zero-emission
Put.
2. technique as claimed in claim 1, wherein, tube type filter membrance TMF techniques are used in step (1), used in the step
System includes reaction tank, concentration basin, microfiltration membranes and other corollary equipments.
3. technique as claimed in claim 1, wherein, it is using weak acid resin hard-removal system that the calcium and magnesium of waste water is hard in step (2)
Degree removes completely, and the operational mode of weak acid resin is sodium form.
4. technique as claimed in claim 1, wherein, nanofiltration intakes TDS 20,000 or so, tentatively divides salt, nanofiltration by nanofiltration
It is more than 98% to sulfate radical rejection to chlorion without rejection.
5. technique as claimed in claim 1, wherein, the concentrated water purifyingization system of nanofiltration includes catalytic ozonation and activated carbon
Absorption.
6. technique as claimed in claim 1, wherein, the forming steps of potassium sulfate are mixed using nanofiltration concentrate with KCl solids,
And by evaporative removal part water, cooling, pass through centrifuge separation of solid and liquid generating portion K2SO4；Separation of solid and liquid Mother liquor with it is additional
Sodium sulphate or saltcake mixing, and pass through evaporative crystallization, cool, glaserite is generated by centrifuge separation of solid and liquid；Separation of solid and liquid is given birth to
Into glaserite and additional the KCl secondary response again of part, pass through centrifuge separation of solid and liquid generating portion K2SO4, and separation of solid and liquid generates
Mother liquor partial, after glaserite, then mixed salt outward transport disposal is gone out by evaporative crystallization.
7. a kind of high-salt wastewater processing system for being used for the technique as described in one of claim 1-6, the system include：
Tubular type Microfiltration Unit, it is used to remove most of calcium ions and magnesium ions, silicon, heavy metal and suspension and part in high-salt wastewater
Organic matter；
Weak acid resin removes hard unit, and it is used for the hardness, the basicity that further reduce high-salt wastewater；
Nanofiltration film unit, it is used for the preliminary of high-salt wastewater and divides salt, and high-salt wastewater is divided into two strands, that is, produces water side and concentrated water side,
Wherein, it is mainly sodium chloride and minimal amount of sodium sulphate to produce water side salinity, and concentrated water side salinity is mainly sodium sulphate and partial oxidation
Sodium；
Nanofiltration concentrated water matter-water-organic matter purification unit, it is used to the waste water after NF membrane cell processing removing most of organic matter；
Nanofiltration concentrated water high-pressure membrane upgrading unit；
Nanofiltration concentrated water preparing potassium sulfate system；
Water high-pressure membrane concentration systems are produced in nanofiltration；
Water multiple-effect crystal system is produced in nanofiltration；And
Carnallite crystal system.
8. system as claimed in claim 7, wherein, tubular type Microfiltration Unit include reaction tank, concentration basin, microfiltration membranes and other match somebody with somebody
Complete equipment.
9. the system as claimed in claim 1, wherein, nanofiltration concentrated water matter-water-organic matter purification unit includes catalytic ozonation and activity
Charcoal adsorbs.
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