CN115771905A - Production method of food-grade potassium chloride - Google Patents
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- CN115771905A CN115771905A CN202111038432.8A CN202111038432A CN115771905A CN 115771905 A CN115771905 A CN 115771905A CN 202111038432 A CN202111038432 A CN 202111038432A CN 115771905 A CN115771905 A CN 115771905A
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- potassium chloride
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 354
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 154
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 154
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 65
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000012047 saturated solution Substances 0.000 claims abstract description 30
- 238000002425 crystallisation Methods 0.000 claims abstract description 27
- 230000008025 crystallization Effects 0.000 claims abstract description 27
- 239000007800 oxidant agent Substances 0.000 claims abstract description 26
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 25
- 230000001590 oxidative effect Effects 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003463 adsorbent Substances 0.000 claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 18
- 230000008020 evaporation Effects 0.000 claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 235000013305 food Nutrition 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 12
- MXZRMHIULZDAKC-UHFFFAOYSA-L ammonium magnesium phosphate Chemical compound [NH4+].[Mg+2].[O-]P([O-])([O-])=O MXZRMHIULZDAKC-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910052567 struvite Inorganic materials 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims description 19
- -1 ammonium ions Chemical class 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 11
- 230000001276 controlling effect Effects 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- 239000011575 calcium Substances 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 9
- 229910001415 sodium ion Inorganic materials 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 229910001424 calcium ion Inorganic materials 0.000 claims description 8
- 229910001385 heavy metal Inorganic materials 0.000 claims description 8
- 230000001105 regulatory effect Effects 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
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 239000010451 perlite Substances 0.000 claims description 5
- 235000019362 perlite Nutrition 0.000 claims description 5
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 4
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 4
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 4
- 235000019797 dipotassium phosphate Nutrition 0.000 claims description 4
- 229910052816 inorganic phosphate Inorganic materials 0.000 claims description 4
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 4
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 235000019800 disodium phosphate Nutrition 0.000 claims description 3
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000010455 vermiculite Substances 0.000 claims description 3
- 235000019354 vermiculite Nutrition 0.000 claims description 3
- 229910052902 vermiculite Inorganic materials 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- SHFGJEQAOUMGJM-UHFFFAOYSA-N dialuminum dipotassium disodium dioxosilane iron(3+) oxocalcium oxomagnesium oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Na+].[Na+].[Al+3].[Al+3].[K+].[K+].[Fe+3].[Fe+3].O=[Mg].O=[Ca].O=[Si]=O SHFGJEQAOUMGJM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- 239000003002 pH adjusting agent Substances 0.000 claims 1
- 239000003337 fertilizer Substances 0.000 abstract description 10
- 239000011777 magnesium Substances 0.000 abstract description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 abstract description 4
- 235000013373 food additive Nutrition 0.000 abstract description 3
- 239000002778 food additive Substances 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 230000009615 deamination Effects 0.000 abstract 1
- 238000006481 deamination reaction Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 208000005156 Dehydration Diseases 0.000 description 15
- 230000018044 dehydration Effects 0.000 description 15
- 238000006297 dehydration reaction Methods 0.000 description 15
- 239000000047 product Substances 0.000 description 14
- 150000001412 amines Chemical class 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 238000000926 separation method Methods 0.000 description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- 238000010981 drying operation Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 238000005188 flotation Methods 0.000 description 5
- 239000013505 freshwater Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011343 solid material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- ZRIILUSQBDFVNY-UHFFFAOYSA-N 4-dodecylmorpholine Chemical compound CCCCCCCCCCCCN1CCOCC1 ZRIILUSQBDFVNY-UHFFFAOYSA-N 0.000 description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910017958 MgNH Inorganic materials 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Natural products C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
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- Fertilizers (AREA)
Abstract
The invention relates to a production method of food-grade potassium chloride, and relates to the field of food additives. Dissolving potassium chloride in water to obtain a saturated solution I, adding a pH regulator to regulate the pH to 8-12, then adding a strong oxidant and a settling agent, and converting inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate to obtain a saturated solution II of potassium chloride; adding an adsorbent into the solution, and filtering out precipitates to obtain a potassium chloride saturated solution III; then adding hydrochloric acid into the mixture to adjust the pH value to 4 to 7, and carrying out multiple-effect flash evaporation, cooling and crystallization to obtain crystal mush; concentrating, dehydrating, and drying to obtain high-quality food grade potassium chloride with ammonium content of 1-20 ppm. According to the invention, a two-stage deamination process is adopted for a potassium chloride saturated solution, and a strong oxidant and a settling agent are added into the potassium chloride saturated solution to achieve the purposes of magnesium removal and ammonium removal, so that high-purity food-grade potassium chloride is finally obtained. The byproduct magnesium ammonium phosphate can be used as a slow release fertilizer, and tail-free discharge is realized.
Description
Technical Field
The invention relates to the field of food additives, in particular to a production method of food-grade potassium chloride.
Background
The food-grade potassium chloride is a very popular product, has wide application in the food industry, can be used as a salt substitute, a nutritional supplement, a gelling aid, yeast foodstuff, a flavoring agent, a pH value control agent and the like, is one of high-end products which can be derived from the potassium fertilizer industry, and has great market development potential in the future food-grade potassium chloride industry.
At present, most of raw materials for producing food-grade potassium chloride at home and abroad are industrial-grade potassium chloride, and the production process basically adopts an evaporative crystallization process including dissolution, impurity removal, crystallization, filtration and drying. The process can produce products meeting the quality requirement, but has higher requirement on the quality of raw materials. Although China is a country with serious shortage of potassium resources, the production of food-grade potassium chloride can be completely self-sufficient only by using the current domestic capacity of potassium chloride in the Carer sweat lake. However, according to research, most of domestic food-grade potassium chloride manufacturers are far away and use imported potassium as a production raw material, but the reason is that most of potassium chloride produced in China is produced by a conventional flotation method, and potassium chloride products contain a large amount of impurities which cannot be removed by a simple physical method, and mainly comprise ammonium chloride, magnesium chloride, octadecylamine flotation reagent, dodecyl morpholine flotation reagent, calcium sulfate acid insoluble substances and other impurities. The contents of inorganic ammonium and organic amine are seriously exceeded, and organic amine has irritation to skin and mucosa and certain irritation to central nerve, which greatly limits the application of potassium chloride in the industries of medicine and food additives. Therefore, if the salt lake potassium fertilizer is used as a raw material to produce food-grade potassium chloride, the removal process research of inorganic ammonium and organic amine must be firstly carried out.
Several methods for removing ammonium from potassium chloride are disclosed in chinese patents. The organic nitrogen in the industrial potassium chloride, such as octadecylamine, dodecyl morpholine, 2# oil and the like, is removed by adopting methods of chemical separation, macroporous resin adsorption, nanofiltration membrane separation and the like respectively. The method can theoretically effectively remove ammonia nitrogen in industrial potassium chloride, but the removal process is complex and high in cost, and is not beneficial to industrialization. The inventor finds in experiments that directly by adopting the hot melting method, the solubility of the octadecylamine or the alkyl morpholine is increased along with the increase of the temperature, and organic matters are remained in a liquid phase and adsorbed on the surface of a potassium chloride crystal in the cooling crystallization process to be mixed into a product and are not easy to remove.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a production method of food-grade potassium chloride, which has the advantages of simple process and low production cost and can effectively remove calcium, magnesium, ammonium and organic amine organic matters in raw material potassium chloride.
The technical problem to be solved by the present invention is achieved by the following technical means. The invention relates to a production method of food-grade potassium chloride, which comprises the following specific steps:
(1) Dissolving a raw material potassium chloride in water to prepare a saturated potassium chloride solution, controlling the dissolving temperature to be 20-110 ℃ to obtain a saturated potassium chloride solution I, adding a pH regulator into the saturated potassium chloride solution I, regulating the pH to 8-12, adding a strong oxidant and a precipitation aid, wherein the precipitation aid is phosphoric acid or inorganic phosphate, and converting inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate to obtain a saturated potassium chloride solution II;
(2) Adding an adsorbent into the potassium chloride saturated solution II, then filtering, and removing precipitates to obtain a potassium chloride saturated solution III;
(3) Adding hydrochloric acid into the saturated potassium chloride solution III to adjust the pH value to 4-7, and then carrying out multi-effect flash evaporation, cooling and crystallization to obtain crystal slurry;
(4) Concentrating, dehydrating and drying the crystal mush to obtain the high-quality food-grade potassium chloride with the ammonium content of 1-20 ppm.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that:
(1) Adding an adsorbent into the potassium chloride saturated solution II, continuously stirring, then performing primary dehydration operation, piling filter residues obtained after the filter residues are analyzed by the adsorbent into a storage yard, and selling the filter residues as a fertilizer, wherein the filtrate is the obtained potassium chloride saturated solution III;
(2) Feeding potassium chloride crystal slurry obtained by multi-effect flash evaporation, concentration and crystallization into secondary dehydration operation for solid-liquid separation, washing a dehydrated product by fresh water, feeding the dehydrated product into tertiary dehydration operation, and performing the tertiary dehydration operation to obtain a potassium chloride solid wet material; and feeding the obtained potassium chloride wet material into drying operation, and drying to obtain high-quality food-grade potassium chloride with the water content of the product below 1%.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: the raw material potassium chloride can be industrial grade and agricultural grade potassium chloride. The further preferable raw material is agricultural or industrial potassium chloride produced by Qinghai in China, the content of the potassium chloride is 93-98%, the content of sodium ions is 0.1-2.0%, the content of magnesium ions is 0.1-0.5%, and the content of ammonium is 400-2500 mg/kg.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: in the step (1), the dissolving temperature is controlled to be 40-90 ℃, and further preferably 60-80 ℃.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: the molar ratio of the magnesium ion to the ammonium ion in the potassium chloride solution in the step (1) is 0.7 to 3, and more preferably 1 to 2.5.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: adding a pH regulator into the saturated potassium chloride solution I to adjust the pH to 8.5-10 in the step (1); and (3) adding hydrochloric acid into the saturated potassium chloride solution III to adjust the pH value to 6 to 7.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: the alkali for adjusting the pH value in the step (1) is one or the combination of more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or lime.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: the precipitation aid added in the step (1) is one or more of phosphoric acid, sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate or other inorganic phosphates, and the molar ratio of phosphate ions to ammonium ions is preferably 0.7 to 3.0, and more preferably 0.8 to 2.0. The addition mode of adding the settling agent and then adding the strong oxidant is adopted.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: the strong oxidant in the step (1) is one or a combination of more of ozone, hydrogen peroxide, hypochlorous acid, peracetic acid, nitrous acid, nitrite and chlorine; the strong oxidant is added under acidic conditions or under basic conditions.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: adding the adsorbent in the step (2) after adding the settling agent, or adding the adsorbent after adjusting the pH to acidity; the adsorbent is one or a combination of more of activated carbon, perlite, diatomite or vermiculite. The addition amount of the adsorbent is preferably 0.05-3% of the mass of potassium chloride.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: in the step (1), an adding mode of adding the settling agent firstly and then adding the strong oxidant is adopted.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: and (4) performing multi-effect flash evaporation, cooling and crystallization in the step (3) by adopting a 2-to-4-effect DTB type vacuum crystallizer.
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: the oxidizing agent in the potassium chloride solution I in the step (1) and the adsorbent in the step (2) may be added after hydrochloric acid is added in the step (3).
The production method of the food-grade potassium chloride further adopts the preferable technical scheme that: and (5) one or more of a thickener, a cyclone, a belt filter and a centrifuge are selected for dehydration operation in the step (4). The drying operation selects a fluidized bed or a rotary dryer as the drying equipment.
The high-quality food-grade potassium chloride obtained by the method has the advantages that the content of potassium chloride is more than or equal to 99.8 percent, the content of sodium ions is less than or equal to 0.5 percent, the total content of calcium and magnesium ions is less than or equal to 100mg/kg, the content of ammonium is less than or equal to 20mg/kg, the content of heavy metal is less than or equal to 1mg/kg, and the content of organic matters is less than or equal to 1mg/kg.
The inventor finds that: agricultural or industrial potassium chloride products contain a large amount of impurities which cannot be removed by a simple physical method, and mainly comprise ammonium chloride, magnesium chloride, octadecylamine flotation reagent, dodecylmorpholine flotation reagent, calcium sulfate acid insoluble substances and other impurities. The inventor finds out through research that:
(1) At pH =8 to 12, phosphate can react with MgCl 2 、NH 4 + React to generate MgNH 4 PO 4 ·H 2 The precipitation of O can realize the effect of simultaneously removing magnesium and ammonium of a medicament.
(2) The strong oxidant can react with amine molecules on the organic amine to generate pollution-free nitrogen which can be directly discharged.
(3) The acid insoluble substances are removed by dewatering equipment under the condition of hot melting by adopting a hot-melting cold crystallization process, and then the high-quality food-grade potassium chloride is obtained by a vacuum crystallization process.
(4) When the temperature exceeds 80 ℃, the octadecylamine can generate ammonia separating reaction to release NH 3 The reaction is accelerated with increasing temperature, and in particular, the more basic, the faster the ammonia evolution reaction.
The process for obtaining food-grade potassium chloride commonly used in the prior art comprises the following steps: firstly, the potassium chloride raw material of the invention is hot-dissolved to prepare saturated solution, and then Mg carried in the solution is removed by adding alkali 2+ Inorganic ammonium is removed by an air stripping method, then organic amine is absorbed by activated carbon and ion exchange resin, and finally qualified food-grade potassium chloride is obtained by a cold crystallization process. In addition, the blowing-off method needs an ammonia gas recovery device, the process flow is complex, the investment cost is high, and if the recovery is not considered, the environment is polluted.
Compared with the traditional process, the method has the beneficial effects that:
(1) The invention adopts a two-stage deammoniation process for the saturated potassium chloride solution, and adds a strong oxidant and a settling agent into the hot saturated potassium chloride solution to achieve the purposes of magnesium removal and ammonium removal, thereby finally obtaining the high-purity food-grade potassium chloride.
(2) Mg can be removed in one step by adding phosphoric acid or phosphate precipitation aid under alkaline condition 2+ And NH 4+ And MgNH formed 4 PO 4 ·H 2 O is a good slow-release multi-element compound fertilizer, can change the cost into valuable, and reduces the environmental pollution.
(3) By adding a strong oxidant into the saturated potassium chloride solution, the amine molecules of organic amine can be discharged in a nitrogen form, and secondary pollution is avoided.
The invention has simple process flow, lower operating cost, coarse granularity and high quality of the obtained potassium chloride, and the byproduct magnesium ammonium phosphate can be used as the slow-release multi-element compound fertilizer, thereby really realizing tailless discharge and not generating environmental pollution, thus being a green production process.
Detailed Description
The following more detailed description of the present invention is provided to enable those skilled in the art to further understand the present invention, and is not to be construed as limiting the claims of the present invention.
Example 1, a method for producing food grade potassium chloride, the method comprising the specific steps of:
(1) Dissolving industrial potassium chloride with the potassium chloride grade of 94% and the ammonium content of 1300mg/kg serving as a raw material in water to prepare a saturated potassium chloride solution, and controlling the dissolving temperature at 45 ℃ to obtain a saturated potassium chloride solution I.
(2) Firstly, adding a pH regulator potassium hydroxide into a potassium chloride saturated solution I, after the pH is regulated to 9, adding a strong oxidant sodium hypochlorite and a settling agent potassium hydrogen phosphate, converting inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate, wherein the molar ratio of the phosphate ions to the ammonium ions is 1:1, obtaining a potassium chloride saturated solution II, wherein the molar ratio of sodium hypochlorite to total amine is 2;
(3) Adding perlite serving as an adsorbent into the saturated potassium chloride solution II, wherein the addition amount of perlite is 0.5 percent of the mass of potassium chloride. Continuously stirring, then feeding into a primary dehydration operation, wherein a centrifuge is selected as dehydration equipment, filter residues obtained after the filter residues are resolved by an adsorbent are piled in a storage yard and can be sold as fertilizer, and filtrate is the obtained potassium chloride saturated solution III;
(4) Adding hydrochloric acid into the saturated potassium chloride solution III, adjusting the pH value to 8, performing flash evaporation, cooling, concentration and crystallization through triple-effect flash evaporation crystallization, wherein a DTB type vacuum crystallizer is selected as crystallization equipment;
(5) Feeding potassium chloride crystal slurry obtained by multi-effect flash evaporation, concentration and crystallization into a centrifugal machine for solid-liquid separation, washing solid materials by fresh water, and feeding the washed solid materials into the centrifugal machine to obtain potassium chloride solid wet materials;
(6) Feeding the obtained wet potassium chloride material into drying operation, drying to obtain high-quality food-grade potassium chloride, wherein the potassium chloride content is 99.8%, the sodium ion content is less than or equal to 0.5%, the total content of calcium and magnesium ions is less than or equal to 100mg/kg, the ammonium content is 15mg/kg, the heavy metal content is less than or equal to mg/kg, the organic matter content is less than or equal to 1mg/kg, the water content of the product is 1.0%, and a rotary drum dryer is selected as drying equipment.
Embodiment 2, a method for producing food grade potassium chloride, the method comprising the steps of:
(1) Dissolving industrial potassium chloride with a potassium chloride grade of 96% and an ammonium content of 2000mg/kg serving as a raw material in water to prepare a saturated potassium chloride solution, controlling the dissolving temperature at 60 ℃ to obtain a saturated potassium chloride solution I, wherein magnesium chloride is added because the concentration of magnesium ions in the solution is low, and the molar ratio of the magnesium ions to the ammonium ions in the solution is controlled to be 1.2.
(2) Firstly, adding a pH regulator potassium hydroxide into a potassium chloride saturated solution I, adjusting the pH to 9.5,
adding a settling agent sodium hydrogen phosphate to convert inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate, wherein the molar ratio of phosphate ions to ammonium ions is 1.5:1, controlling to obtain a potassium chloride saturated solution II;
(3) Adding hydrochloric acid into the saturated potassium chloride solution II, adjusting the pH value to 5.0, and then adding hydrogen peroxide into the saturated potassium chloride solution II, wherein the molar ratio of the hydrogen peroxide to the total amine is 2;
(4) Then adding adsorbent active carbon into the medium potassium chloride saturated solution II, wherein the adding amount is 1 percent of the mass of the potassium chloride. Continuously stirring, then feeding into a primary dehydration operation, wherein a centrifuge is selected as dehydration equipment, filter residues obtained after the filter residues are resolved by an adsorbent are piled in a storage yard and can be sold as fertilizer, and filtrate is the obtained potassium chloride saturated solution III;
(5) Carrying out flash evaporation, cooling, concentration and crystallization on the potassium chloride saturated solution through double-effect flash evaporation crystallization operation, wherein a DTB type vacuum crystallizer is selected as crystallization equipment;
(6) Feeding potassium chloride crystal slurry obtained by multi-effect flash evaporation, concentration and crystallization into a centrifugal machine for solid-liquid separation, and feeding the solid material into the centrifugal machine after fresh water washing to obtain a potassium chloride solid wet material;
(7) And (3) feeding the obtained wet potassium chloride material into drying operation, drying to obtain high-quality food-grade potassium chloride, wherein the potassium chloride content is 99.8%, the sodium ion content is less than or equal to 0.5%, the total content of calcium and magnesium ions is less than or equal to 100mg/kg, the ammonium content is 9mg/kg, the heavy metal content is less than or equal to 1mg/kg, the organic matter content is less than or equal to 1mg/kg, the water content of the product is 1%, and a fluidized bed is selected as drying equipment.
Embodiment 3, a method for producing food grade potassium chloride, the method comprising the steps of:
(1) Dissolving industrial potassium chloride with the potassium chloride grade of 95% and the ammonium content of 1950mg/kg as a raw material in water to prepare a saturated potassium chloride solution, and controlling the dissolving temperature at 85 ℃ to obtain a saturated potassium chloride solution I.
(2) Firstly, adding a pH regulator sodium hydroxide into a potassium chloride saturated solution I, adding a precipitation aid sodium dihydrogen phosphate after the pH is regulated to 9.5, converting inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate, wherein the molar ratio of phosphate ions to ammonium ions is 1.2:1, controlling to obtain a potassium chloride saturated solution II, feeding the potassium chloride saturated solution II into a horizontal sedimentation centrifuge or a filter press, and piling filter residues to a tailing yard for taking out as a fertilizer;
(3) Adding hydrochloric acid into the saturated potassium chloride solution II, adjusting the pH value to 5.0, and then adding sodium nitrite into the saturated potassium chloride solution II, wherein the molar ratio of nitrite to total amine is 1.2;
(4) Then adding adsorbent active carbon into the medium potassium chloride saturated solution II, wherein the adding amount is 1.0 percent of the mass of the potassium chloride. Continuously stirring, then feeding into a primary dehydration operation, wherein a centrifuge is selected as dehydration equipment, filter residues are obtained after being analyzed by an adsorbent and are stacked into a storage yard, and filtrate is obtained and is the obtained potassium chloride saturated solution III;
(5) Carrying out flash evaporation, cooling, concentration and crystallization on the potassium chloride saturated solution through triple effect flash evaporation crystallization operation, wherein a DTB type vacuum crystallizer is selected as crystallization equipment;
(6) Feeding potassium chloride crystal slurry obtained by multi-effect flash evaporation, concentration and crystallization into a centrifugal machine for solid-liquid separation, and feeding the solid material into the centrifugal machine after fresh water washing to obtain a potassium chloride solid wet material;
(7) Feeding the obtained wet potassium chloride material into drying operation, drying to obtain high-quality food-grade potassium chloride, wherein the potassium chloride content is 99.8%, the sodium ion content is less than or equal to 0.5%, the total content of calcium and magnesium ions is less than or equal to 100mg/kg, the ammonium content is 18mg/kg, the heavy metal content is less than or equal to 1mg/kg, the organic matter content is less than or equal to 1mg/kg, the water content of the product is 1%, and a fluidized bed is selected as drying equipment.
Example 4, a method of producing food grade potassium chloride, comprising the steps of:
(1) The content of the raw material potassium chloride is 95 percent, and the content of ammonium is 1500mg/kg; dissolving a raw material potassium chloride in water to prepare a saturated potassium chloride solution, controlling the dissolving temperature at 40 ℃ to obtain a saturated potassium chloride solution I, adding a pH regulator into the saturated potassium chloride solution I, after the pH is regulated to 8.5, adding a strong oxidant and a precipitation aid, wherein the precipitation aid is phosphoric acid, and converting inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate to obtain a saturated potassium chloride solution II; the molar ratio of magnesium ions to ammonium ions in the potassium chloride solution was 1.2. The alkali for adjusting the pH is lime; the addition mode of adding the settling agent and then adding the strong oxidant is adopted; the strong oxidant is hypochlorous acid;
(2) Adding an adsorbent into the potassium chloride saturated solution II, then filtering, and removing precipitates to obtain a potassium chloride saturated solution III; the adsorbent is vermiculite;
(3) Adding hydrochloric acid into the saturated potassium chloride solution III to adjust the pH value to 6, and then carrying out 4-effect flash evaporation, cooling and crystallization to obtain crystal slurry;
(4) And concentrating, dehydrating and drying the crystal mush to obtain the food-grade potassium chloride with high ammonium content. The prepared food-grade potassium chloride comprises the following components: the content of potassium chloride is more than or equal to 99.8 percent, the content of sodium ions is less than or equal to 0.5 percent, the total content of calcium and magnesium ions is less than or equal to 100mg/kg, the content of ammonium =12mg/kg, the content of heavy metal is less than or equal to 1mg/kg, and the content of organic matters is less than or equal to 1mg/kg.
Example 5, a method for producing food grade potassium chloride comprising the steps of:
(1) The content of the raw material potassium chloride is 96 percent, and the content of ammonium is 2250mg/kg; dissolving a raw material potassium chloride in water to prepare a saturated potassium chloride solution, controlling the dissolving temperature at 90 ℃ to obtain a saturated potassium chloride solution I, adding a pH regulator into the saturated potassium chloride solution I, after the pH is regulated to 10, adding a strong oxidant and a settling agent potassium hydrogen phosphate, and converting inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate to obtain a saturated potassium chloride solution II; the molar ratio of magnesium ions to ammonium ions in the potassium chloride solution was 2.5. The base for adjusting the pH is sodium carbonate. The molar ratio of phosphate ions to ammonium ions is 2.0; the addition mode of adding the settling agent and then adding the strong oxidant is adopted. The strong oxidant is chlorine;
(2) Adding perlite serving as an adsorbent into the saturated potassium chloride solution II, filtering, and removing precipitates to obtain a saturated potassium chloride solution III;
(3) Adding hydrochloric acid into the saturated potassium chloride solution III to adjust the pH value to 7, and then carrying out 3-effect flash evaporation, cooling and crystallization to obtain crystal slurry;
(4) Concentrating, dehydrating and drying the crystal mush to obtain the high-quality food-grade potassium chloride with the ammonium content of 1-20 ppm. The prepared food-grade potassium chloride comprises the following components: the content of potassium chloride is more than or equal to 99.8 percent, the content of sodium ions is less than or equal to 0.5 percent, the total content of calcium and magnesium ions is less than or equal to 100mg/kg, the content of ammonium =16mg/kg, the content of heavy metal is less than or equal to 1mg/kg, and the content of organic matters is less than or equal to 1mg/kg.
Example 6, a method for producing food grade potassium chloride comprising the steps of:
(1) The content of the raw material potassium chloride is 97.5 percent, and the content of ammonium is 1200mg/kg; dissolving potassium chloride serving as a raw material in water to prepare a saturated potassium chloride solution, controlling the dissolving temperature at 80 ℃ to obtain a saturated potassium chloride solution I, adding a pH regulator into the saturated potassium chloride solution I, adding a strong oxidant and a settling agent sodium dihydrogen phosphate after the pH is regulated to 9.5, and converting inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate to obtain a saturated potassium chloride solution II; the molar ratio of magnesium ions to ammonium ions in the potassium chloride solution was 2. The base to adjust the pH is sodium hydroxide. The molar ratio of phosphate ions to ammonium ions is 1.0; the addition mode of adding the settling agent and then adding the strong oxidant is adopted. The strong oxidant is nitrous acid; the strong oxidant is added under acidic conditions or under basic conditions.
(2) Adding adsorbent diatomite into the potassium chloride saturated solution II, continuously stirring, then performing primary dehydration operation, stacking filter residues obtained after the filter residues are analyzed by the adsorbent into a storage yard, and taking the filter residues as a fertilizer for sale, wherein the filtrate is the obtained potassium chloride saturated solution III;
(3) Adding hydrochloric acid into the saturated potassium chloride solution III to adjust the pH value to 6.5, and then carrying out 3-effect flash evaporation, cooling and crystallization to obtain potassium chloride crystal slurry;
(4) Feeding the potassium chloride crystal slurry into secondary dehydration operation for solid-liquid separation, washing a dehydrated product by fresh water, and feeding the dehydrated product into tertiary dehydration operation, wherein the tertiary dehydration operation is carried out to obtain a potassium chloride solid wet material; and feeding the obtained potassium chloride wet material into drying operation, and drying to obtain high-quality food-grade potassium chloride with the water content of the product below 1%.
The prepared food-grade potassium chloride comprises the following components: the content of potassium chloride is more than or equal to 99.8 percent, the content of sodium ions is less than or equal to 0.5 percent, the total content of calcium and magnesium ions is less than or equal to 100mg/kg, the content of ammonium =14mg/kg, the content of heavy metal is less than or equal to 1mg/kg, and the content of organic matters is less than or equal to 1mg/kg.
It is to be understood that the present embodiments are capable of numerous changes, modifications, substitutions and alterations without departing from the principles of the invention, the scope of which is defined by the appended claims and their equivalents.
Claims (10)
1. A production method of food-grade potassium chloride is characterized by comprising the following steps:
(1) Dissolving a raw material potassium chloride in water to prepare a saturated potassium chloride solution, controlling the dissolving temperature to be 20-110 ℃ to obtain a saturated potassium chloride solution I, adding a pH regulator into the saturated potassium chloride solution I, regulating the pH to 8-12, adding a strong oxidant and a precipitation aid, wherein the precipitation aid is phosphoric acid or inorganic phosphate, and converting inorganic ammonium and magnesium ions in the solution into magnesium ammonium phosphate to obtain a saturated potassium chloride solution II;
(2) Adding an adsorbent into the potassium chloride saturated solution II, then filtering, and removing precipitates to obtain a potassium chloride saturated solution III;
(3) Adding hydrochloric acid into the saturated potassium chloride solution III to adjust the pH value to 4-7, and then carrying out multi-effect flash evaporation, cooling and crystallization to obtain crystal slurry;
(4) Concentrating, dehydrating and drying the crystal mush to obtain the high-quality food-grade potassium chloride with the ammonium content of 1-20 ppm.
2. The method for producing food grade potassium chloride according to claim 1, wherein the dissolving temperature in the step (1) is controlled to be 40 ℃ to 90 ℃, further preferably 60 ℃ to 80 ℃.
3. The method for producing food grade potassium chloride according to claim 1, wherein the molar ratio of magnesium ions to ammonium ions in the potassium chloride solution in the step (1) is 0.7 to 3, preferably 1 to 2.5.
4. The method for producing food-grade potassium chloride according to claim 1, wherein in the step (1), a pH adjusting agent is added to the saturated potassium chloride solution I to adjust the pH to 8.5 to 10; and (3) adding hydrochloric acid into the saturated potassium chloride solution III to adjust the pH value to 6 to 7.
5. The process for producing food grade potassium chloride according to claim 1, wherein the base for adjusting the pH in step (1) is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, or lime.
6. The method for producing food grade potassium chloride according to claim 1, wherein the precipitation aid added in step (1) is one or more of phosphoric acid, sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate or other inorganic phosphates, and the molar ratio of phosphate ions to ammonium ions is preferably 0.7 to 3.0, more preferably 0.8 to 2.0; preferably, the method of adding the settling agent first and then adding the strong oxidant is adopted.
7. The method for producing food-grade potassium chloride according to claim 1, wherein the strong oxidant in the step (1) is one or more of ozone, hydrogen peroxide, hypochlorous acid, peracetic acid, nitrous acid, nitrite and chlorine; the strong oxidant is added under acidic conditions or under basic conditions.
8. The method of claim 1, wherein the adsorbent is one or more selected from activated carbon, perlite, diatomaceous earth, and vermiculite.
9. The production method of food grade potassium chloride according to claim 1, wherein the multi-effect flash evaporation cooling crystallization in the step (3) adopts a 2-4-effect DTB type vacuum crystallizer.
10. The method for producing food grade potassium chloride according to claim 1, wherein the food grade potassium chloride in step (4) comprises the following components: the content of potassium chloride is more than or equal to 99.8 percent, the content of sodium ions is less than or equal to 0.5 percent, the total content of calcium and magnesium ions is less than or equal to 100mg/kg, the content of ammonium is less than or equal to 20mg/kg, the content of heavy metal is less than or equal to 1mg/kg, and the content of organic matters is less than or equal to 1mg/kg.
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