CN1321893C - Method for preparing potassium sulfate from bittern containing potassium and magnesium sulfate - Google Patents
Method for preparing potassium sulfate from bittern containing potassium and magnesium sulfate Download PDFInfo
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- CN1321893C CN1321893C CNB02143641XA CN02143641A CN1321893C CN 1321893 C CN1321893 C CN 1321893C CN B02143641X A CNB02143641X A CN B02143641XA CN 02143641 A CN02143641 A CN 02143641A CN 1321893 C CN1321893 C CN 1321893C
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- Prior art keywords
- potassium
- salt
- bittern
- halogen
- mixed salt
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000011591 potassium Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 24
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 title claims abstract description 15
- 229910052943 magnesium sulfate Inorganic materials 0.000 title claims abstract description 6
- 235000019341 magnesium sulphate Nutrition 0.000 title claims abstract description 6
- 241001131796 Botaurus stellaris Species 0.000 title claims description 34
- 229910052939 potassium sulfate Inorganic materials 0.000 title abstract 5
- 235000011151 potassium sulphates Nutrition 0.000 title abstract 5
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 title abstract 4
- 150000003839 salts Chemical class 0.000 claims abstract description 35
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 33
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 29
- BMQVDVJKPMGHDO-UHFFFAOYSA-K magnesium;potassium;chloride;sulfate;trihydrate Chemical compound O.O.O.[Mg+2].[Cl-].[K+].[O-]S([O-])(=O)=O BMQVDVJKPMGHDO-UHFFFAOYSA-K 0.000 claims abstract description 15
- 230000018044 dehydration Effects 0.000 claims abstract description 9
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 239000001103 potassium chloride Substances 0.000 claims abstract description 8
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 8
- -1 then Chemical compound 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract 3
- 229910052736 halogen Inorganic materials 0.000 claims description 29
- 150000002367 halogens Chemical class 0.000 claims description 29
- 208000006558 Dental Calculus Diseases 0.000 claims description 19
- GMLLYEDWRJDBIT-UHFFFAOYSA-J magnesium;dipotassium;disulfate Chemical compound [Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GMLLYEDWRJDBIT-UHFFFAOYSA-J 0.000 claims description 12
- WZISDKTXHMETKG-UHFFFAOYSA-H dimagnesium;dipotassium;trisulfate Chemical compound [Mg+2].[Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O WZISDKTXHMETKG-UHFFFAOYSA-H 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 7
- 239000012452 mother liquor Substances 0.000 claims description 7
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 6
- 238000005188 flotation Methods 0.000 claims description 6
- 230000003760 hair shine Effects 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- HAQAPRXIBNGFQH-UHFFFAOYSA-N [V].[K].[Mg] Chemical compound [V].[K].[Mg] HAQAPRXIBNGFQH-UHFFFAOYSA-N 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000013078 crystal Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000012267 brine Substances 0.000 abstract 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 abstract 6
- 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 abstract 2
- WRUGWIBCXHJTDG-UHFFFAOYSA-L magnesium sulfate heptahydrate Chemical class O.O.O.O.O.O.O.[Mg+2].[O-]S([O-])(=O)=O WRUGWIBCXHJTDG-UHFFFAOYSA-L 0.000 abstract 1
- 239000011780 sodium chloride Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229940072033 potash Drugs 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- FZFYOUJTOSBFPQ-UHFFFAOYSA-M dipotassium;hydroxide Chemical compound [OH-].[K+].[K+] FZFYOUJTOSBFPQ-UHFFFAOYSA-M 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a method for preparing potassium sulfate by using potassium-containing magnesium sulfate subtype brine. The process comprises the steps of firstly, sun-drying raw brine to extract most of sodium chloride, then, brine blending, sequentially introducing the brine into a epsomite salt field, a kainite potassium mixed salt field and a carnallite potassium mixed salt field, sun-drying the kainite potassium mixed salt and the carnallite potassium mixed salt respectively, then respectively introducing the raw brine into a picromerite selection plant and a potassium chloride selection plant, and carrying out conversion, decomposition, selective washing and dehydration to respectively obtain picromerite and potassium chloride. Adding brackish water into picromerite and potassium chloride to prepare brine, and then preparing potassium sulfate by drying in the sun, evaporating and dehydrating in a salt field or converting picromerite and potassium chloride in a device to obtain a potassium sulfate product.
Description
One, technical field
The present invention relates to a kind of utilization and contain the method that potassium magnesium sulfate bittern is produced vitriolate of tartar.
Two, background technology
Vitriolate of tartar is the indispensable few potash fertilizer of agriculture production.China is a large agricultural country, and the expense of potash fertilizer is big.In present prior art, the production technique of vitriolate of tartar mainly is to utilize commodity Repone K and the various compound (as sulfuric acid, ammonium sulfate, sal epsom, sodium sulfate, calcium sulfate etc.) that contains sulfate radical to carry out conversion method production.This kind method is to the specification of quality height of raw material Repone K, the raw materials cost height, produce required various device in addition, expenses such as transportation make investment strengthen product cost and increase, and easy contaminate environment, and at the landlocked arid biogeographic zone of northern China and northwest, be distributed with a large amount of salt lakes, there is the abundant potassium vitriolate type bittern resource that contains in some salt lake, and these salt lakes are not exploited mostly as yet.
Three, summary of the invention
The purpose of this invention is to provide that a kind of cost is low, less investment, free of contamination utilization contain the method that potassium magnesium sulfate bittern is produced vitriolate of tartar.
In order to achieve the above object, the technical solution adopted in the present invention is characterized in need not adding any raw material, make full use of sylvite contained in the magnesium sulfate bittern and vitriol and produce vitriolate of tartar at the scene, concrete technology is as follows: operation 1, elder generation import the NaCI salt pan with former halogen, separate out most of NaCI through solar evaporation; Operation 2, will extract bittern behind the NaCI and the old halogen after the operation 3 is converted halogen; Operation 3, the bittern of converting after the halogen import epsom salt salt pan, kainite potassium mixed salt salt pan and carnallitite potassium mixed salt salt pan successively, obtain epsom salt, kainite potassium mixed salt and carnallitite potassium mixed salt respectively behind solar evaporations, bittern behind the system carnallitite potassium mixed salt is old halogen, halogen is converted in the sodium salt pond that is used for shining next time after the system NaCI salt, and chloromagnesite is produced in unnecessary discharge; Operation 4: the kainite potassium mixed salt of the system of shining enters one section mother liquor and the slightly salty of workshop after with the thick KCI of washing kainite is formed slurry and transforms through ore grinding earlier, produces schoenite through the flotation dehydration again; Operation 5: carnallitite potassium mixed salt enters the Repone K enrichment plant, and the C point bittern decomposition carnallitite potassium mixed salt with beginning to separate out kainite passes through flotation, dehydration again, and obtains Repone K with two commentaries on classics mother liquors washings, the dehydration of vitriolate of tartar operation; Operation 6: with schoenite and Repone K is that raw material and slightly salty are joined halogen, after the bittern sedimentation for preparing, shine through the beach, salt pan, dehydration produces vitriolate of tartar, or is that raw material is a medium with the slightly salty with schoenite and Repone K, obtains potassium product after conversion in device, separation, the drying.
Said that (C point) bittern that in crystallisation process takes place, begins to separate out sylvite that preferably adopts in order to the bittern that decomposes carnallitite potassium mixed salt in the above-mentioned operation 5.
The said halogen of joining is preferably by K in the above-mentioned operation 6
+, Mg
2+//C1
-, SO
4 2-The proportion scale of 25 ℃ of calphad of quaternary salt-water system carries out.
The salinity of said slightly salty 3-10g/L preferably in the above-mentioned operation.
All take from from technique scheme raw material of the present invention as can be seen and to contain potassium magnesium sulfate bittern, do not need outsourcing Repone K, and adopt the saltpan method equipment used simple, save energy, thereby facility investment is few, production cost has only about half of prior art, uses or convert halogen repeatedly, no waste discharge thereby non-environmental-pollution because mother liquor that the per pass operation produces and bittern all return the front operation.Its chemical ingredients of high-quality vitriolate of tartar and the relative national standards HG/T3279-1990 that produce contrast as following table:
The order item | Measure unit | Index | Examination and test of products result | Individual event is judged | ||
Premium grads | Acceptable end product | Salable product | ||||
Potassium oxide (K 2O) content | % | ≥50.0 | ≥45.0 | ≥33.0 | 50.7 | Meet the premium grads index |
Chlorine (CI -) content | % | ≤1.5 | ≤2.5 | - | 0.8 | Meet the premium grads index |
Water content | % | ≤1.0 | ≤3.0 | ≤3.0 | 0.1 | Meet the premium grads index |
Free acid (H 2SO 4) content | % | ≤0.5 | ≤3.0 | - | Do not detect | Meet the premium grads index |
Basicity (NaOH) content | % | - | - | ≤1.0 | 0.1 | Meet index |
Four, description of drawings and embodiment
Fig. 1 utilizes to contain the process route chart that potassium magnesium sulfate bittern is produced the vitriolate of tartar saltpan method.As shown in Figure 1, earlier former halogen is imported the sodium-chlor salt pan, after solar evaporation is separated out most of sodium-chlor, bittern is imported secondary sodium salt pond convert halogen (not converting halogen when producing for the first time) with the old halogen that shines behind the system carnallitite potassium mixed salt, the bittern of converting after the halogen imports the epsom salt salt pan, kainite potassium mixed salt salt pan and carnallitite potassium mixed salt salt pan successively.After shining, the beach, salt pan obtains epsom salt respectively, kainite potassium mixed salt and carnallitite potassium mixed salt, and the bittern that shines behind the system carnallitite potassium mixed salt is old halogen, is used for and secondary sodium salt field bittern that former halogen shines behind the system sodium-chlor is converted halogen, and unnecessary old halogen row storage is stand-by.The kainite potassium mixed salt input schoenite that solarization is made selects factory to add conversion fluid (adding two behind the washing Repone K with slightly salty changes mother liquors and be made into), behind the ball milling pulping, squeeze into one section reactive tank and transform, the slurry after the conversion obtains schoenite through flotation, dehydration, and the liquid that removes is E
1Mother liquor.The carnallitite potassium mixed salt input Repone K obtain is shone on the beach select factory, the E that itself and schoenite are deviate from
1The point mother liquor is squeezed into decomposer, after decomposing with C point bittern, carries out dense, flotation, dehydration promptly obtains Repone K.The mother liquor that removes returns the salt pan recycle of kainite potassium mixed salt, and schoenite and the Repone K that makes with above-mentioned technology is produced vitriolate of tartar at last.Earlier slightly salty (salinity 3.02g/L) is squeezed into and joined the halogen groove, under agitation condition, press K
+, Mg
2+∥ Cl
-, SO
4 2--H
2The proportion scale of 25 ℃ of calphad of O quaternary salt-water system, add Repone K successively and schoenite is joined halogen, join halogen after sedimentation pumps into the salt pan solar evaporation with clear halogen, when being evaporated to bittern proportion near 1.20, when liquid phase was formed point and is positioned near the terminal point, dewatering promptly obtained potassium product.
Fig. 2 utilizes to contain the installation method process route chart that potassium magnesium sulfate bittern is produced vitriolate of tartar, among the figure as can be seen, compare with saltpan method, installation method is all identical with saltpan method to operation 5 from operation 1, the operation 6 of installation method is behind the schoenite and Repone K uniform mixing produced, add the slightly salty that salinity is 3.02g/L again, enter two sections convertors, dewater after in convertor, transforming and be drying to obtain vitriolate of tartar.
Claims (3)
1, a kind of utilization contains the method that potassium magnesium sulfate bittern is produced vitriolate of tartar, and it comprises operation 1: former halogen is imported the sodium-chlor salt pan, separate out most of sodium-chlor behind solar evaporation; Operation 2: will extract bittern behind the sodium-chlor and the old halogen after the operation 3 and convert halogen, it is characterized in that: it also comprises operation 3: the bittern of converting after the halogen imports the epsom salt salt pan successively, sylvite magnesium vanadium potassium mixed salt salt pan and carnallitite potassium mixed salt salt pan, behind solar evaporation, obtain epsom salt respectively, kainite potassium mixed salt and carnallitite potassium mixed salt, remaining bittern is old halogen, and the bittern after being used for next time and shining the system sodium chloride salt is converted halogen; Operation 4: the kainite potassium mixed salt of the system of shining enters mother liquor and the slightly salty of workshop after with the thick Repone K of washing kainite potassium mixed salt is obtained schoenite through the conversion again of ore grinding formation slurry, flotation, dehydration earlier; Operation 5: the carnallitite potassium mixed salt of the system of will shining decomposes dense, the flotation in back with the bittern in salt pan kainite stage, obtains Repone K with dehydration after the two commentaries on classics mother liquor washings of vitriolate of tartar operation again; Operation 6: with schoenite and Repone K is that raw material and slightly salty are joined halogen, the bittern for preparing shines through the beach, salt pan to be produced vitriolate of tartar or is that raw material is made conversion medium with slightly salty with schoenite and Repone K, produces vitriolate of tartar through conversion, separation, drying in device.
2, said utilization contains potassium magnesium sulfate bittern and produces the vitriolate of tartar method according to claim 1, it is characterized in that: said in the operation 5 is that the C point bittern that begins to separate out sylvite in evaporation and crystal process in order to the bittern that decomposes carnallitite potassium mixed salt.
3, produce the method for vitriolate of tartar according to claim 1 is said to contain potassium magnesium sulfate bittern, the salinity that it is characterized in that said slightly salty is 3-10g/L.
Priority Applications (1)
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CNB02143641XA CN1321893C (en) | 2002-09-25 | 2002-09-25 | Method for preparing potassium sulfate from bittern containing potassium and magnesium sulfate |
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CNB02143641XA CN1321893C (en) | 2002-09-25 | 2002-09-25 | Method for preparing potassium sulfate from bittern containing potassium and magnesium sulfate |
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CN1439602A CN1439602A (en) | 2003-09-03 |
CN1321893C true CN1321893C (en) | 2007-06-20 |
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CN100488874C (en) * | 2004-05-12 | 2009-05-20 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing potassium sulfate by using potassium mixed salt |
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CN100503440C (en) * | 2007-03-30 | 2009-06-24 | 中国科学院青海盐湖研究所 | Process of preparing potassium sulfate with potassium containing bittern of magnesium sulfate subtype |
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CN102249268B (en) * | 2011-05-04 | 2013-06-05 | 中国科学院青海盐湖研究所 | Method for enriching trace elements in saturated magnesium chloride brine by natural evaporation |
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CN107954750B (en) * | 2017-11-10 | 2021-03-09 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing top-grade potash magnesium sulphate fertilizer by using carnallite and potassium mixed salt ore |
CN111170338A (en) * | 2020-03-10 | 2020-05-19 | 青海中信国安锂业发展有限公司 | Process for preparing fully water-soluble potassium sulfate from magnesium sulfate subtype salt lake brine |
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- 2002-09-25 CN CNB02143641XA patent/CN1321893C/en not_active Expired - Lifetime
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