CN106629644A - Method for producing industrial first-stage and battery-stage monoammonium phosphate by using fertilizer-stage monoammonium phosphate - Google Patents
Method for producing industrial first-stage and battery-stage monoammonium phosphate by using fertilizer-stage monoammonium phosphate Download PDFInfo
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- CN106629644A CN106629644A CN201710026629.7A CN201710026629A CN106629644A CN 106629644 A CN106629644 A CN 106629644A CN 201710026629 A CN201710026629 A CN 201710026629A CN 106629644 A CN106629644 A CN 106629644A
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- 238000004519 manufacturing process Methods 0.000 title abstract description 21
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 title abstract description 17
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 title abstract description 17
- 235000019837 monoammonium phosphate Nutrition 0.000 title abstract description 17
- 239000006012 monoammonium phosphate Substances 0.000 title abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 32
- 239000003337 fertilizer Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000003814 drug Substances 0.000 claims abstract description 10
- 229910001868 water Inorganic materials 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract 3
- 239000000706 filtrate Substances 0.000 claims description 78
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 34
- 229910052744 lithium Inorganic materials 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 239000003153 chemical reaction reagent Substances 0.000 claims description 18
- 230000001376 precipitating effect Effects 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 9
- 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 8
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 5
- 239000001099 ammonium carbonate Substances 0.000 claims description 5
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 3
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 claims description 2
- 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
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- 239000002826 coolant Substances 0.000 claims 1
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims 1
- 238000000643 oven drying Methods 0.000 claims 1
- 235000011181 potassium carbonates Nutrition 0.000 claims 1
- 235000017550 sodium carbonate Nutrition 0.000 claims 1
- 238000005292 vacuum distillation Methods 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract 6
- 230000001105 regulatory effect Effects 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 26
- 239000000047 product Substances 0.000 description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 229910052785 arsenic Inorganic materials 0.000 description 12
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 12
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 10
- 239000011777 magnesium Substances 0.000 description 10
- 229910052749 magnesium Inorganic materials 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 6
- 239000011575 calcium Substances 0.000 description 6
- 229910052791 calcium Inorganic materials 0.000 description 6
- 229910052804 chromium Inorganic materials 0.000 description 6
- 239000011651 chromium Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910052748 manganese Inorganic materials 0.000 description 6
- 239000011572 manganese Substances 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 239000011591 potassium Substances 0.000 description 6
- 229910052700 potassium Inorganic materials 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002686 phosphate fertilizer Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 229910000398 iron phosphate Inorganic materials 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000005955 Ferric phosphate Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- RFGNMWINQUUNKG-UHFFFAOYSA-N iron phosphoric acid Chemical compound [Fe].OP(O)(O)=O RFGNMWINQUUNKG-UHFFFAOYSA-N 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
-
- 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
Abstract
The invention discloses a method for producing industrial first-stage and battery-stage monoammonium phosphate by using fertilizer-stage monoammonium phosphate. The fertilizer-stage monoammonium phosphate is heated and dissolved by pure water and is then filtered; then, decolorizing agents and precipitants are added into filter liquid; after the pH value is regulated to a certain value, filtration is performed; filter liquid a is obtained; the filter liquid a is heated and concentrated and is then cooled for crystallization; after drying, the industrial first-stage monoammonium phosphate is obtained; if the precipitants are continuously added into the filter liquid a, filtering is performed after the pH value regulation; then, impurity removal medicaments are added into the filter liquid; still standing is performed; after impurities are separated out, filtering is performed; cooling crystallization is performed after the filter liquid is heated and concentrated; drying is performed; then, the battery-stage monoammonium phosphate is obtained. The powdery fertilizer-stage monoammonium phosphate with high impurity content and low price is used for producing the industrial first-stage and battery-stage monoammonium phosphate; in addition, three wastes in the production are totally recovered for fertilizer production; the process is reliable; the equipment is simple; the production safety is high; the energy is saved; the consumption is reduced; the production cost is greatly reduced.
Description
Technical field
The present invention relates to a kind of method of powdered fertilizer MAP purification, more particularly, to a kind of sulfur-bearing, iron, magnesium, aluminium,
The method of the more industrial one-level of powdered fertilizer MAP production of the impurity such as manganese, titanium and LITHIUM BATTERY MAP.
Background technology
MAP as a kind of high compound of nitrogen and phosphorus content, in being widely used in agricultural production, but fertilizer phosphoric acid one
Ammonium belongs to low-end product, and added value is low, and drug on the market with world's phosphate fertilizer production, market competition aggravation, chemical fertilizer phosphoric acid one
The profit margin of ammonium further reduces, therefore expands the new application of the particularly inexpensive chemical fertilizer MAP of chemical fertilizer ammonium dihydrogen phosphate
Field is extremely urgent.Compared to the fertilizer MAP of low side：Industrial grade monoammonium phosphate is widely used in extinguishing chemical, enamel addition
It is prepared by the production of the chemical products such as agent, papermaking；LITHIUM BATTERY MAP is mainly used in the preparation of lithium battery material ferric phosphate.At present
Industrial grade monoammonium phosphate mainly generated with the reaction of thermal phosphoric acid and ammonia or with high-purity phosphoric acid with it is impure mix compared with polyphosphoric acid and
Ammonia reaction is generated, and also partly using phosphoric acid by wet process or its raffinate, by reaction, again adjusted pH removal of impurities is crystallized with ammonia
Arrive, relative cost is higher.This patent is directly using more powdered fertilizer phosphoric acid of impurity such as a kind of sulfur-bearing, iron, magnesium, aluminium, manganese, titaniums
One ammonium or its not concentrate the slip before granulation be raw material, by dissolution filter or directly filter, filtrate decolouring removal of impurities, a step section
PH, recrystallization production industrial grade monoammonium phosphate, applied widely, low cost.At present about LITHIUM BATTERY MAP production method,
Chinese patent CN103754851A reports a kind of preparation method of the ammonium of LITHIUM BATTERY crystal phosphoric acid one, mainly uses a kind of agricultural
Crystalline MAP Jing dissolvings, filtration, again condensing crystallizing obtains battery grade crystal ammonium dihydrogen phosphate to filtrate after resin treatment
Product.The raw material that the method is used is agricultural lenticular MAP, and cost of material is higher；And the method utilizes resin treatment, tree
Fat consumption is big, regeneration trouble, and long flow path, and speed of production is slow, and high cost is not suitable for industrialized production.Chinese patent
CN105819414A reports a kind of production technology of LITHIUM BATTERY MAP, mainly uses the impure less of certain weight proportion
Phosphoric acid solution and ammonia neutralize, adjust certain pH, then LITHIUM BATTERY MAP is obtained by crystallisation by cooling, but used by the technique
Phosphoric acid purity is high, therefore production cost is high, and general LITHIUM BATTERY MAP to mainly use high-purity thermal phosphoric acid anti-with ammonia
Should generate, although production process equipment is simple, but apparatus and process technical requirements are high, and production is dangerous big, and pollution is big, high energy consumption；
This patent is using a kind of more agricultural greyish white of the impurity such as price is relatively low, quality is relatively low sulfur-bearing, iron, magnesium, aluminium, manganese, titanium
The MAP of color powder is purified, and prepares LITHIUM BATTERY monoammonium phosphate product, is come with respect to other technology of preparing raw materials
Source is wide, low cost, can be widely applied to the compound probability of battery-grade iron phosphate, and the product Jing ferric phosphates producer for preparing is on probation
Comply fully with its use requirement.Industrial one-level and LITHIUM BATTERY monoammonium phosphate product that this patent is prepared, can be widely used in
The fields such as extinguishing chemical, enamel, papermaking and lithium iron phosphate positive material manufacture, can produce preferable economic results in society, be phosphatization
The development of work brings new opportunity.
The content of the invention
The present invention using low side, low cost and the fertilizer MAP of the relatively low a kind of agricultural gray powdery of quality or
Industrial one-level and LITHIUM BATTERY MAP that the fertilizer does not concentrate the slip production high added value before granulation are produced, low side is alleviated
The easy situation of chemical fertilizer monoammonium phosphate product, is provided for new outlet, and there is provided a kind of process, preparation industry
The method of one-level and LITHIUM BATTERY MAP.To achieve these goals, this patent using by dissolution filter, decolourize to adjust by filtrate
Section pH precipitations are filtered, add a kind of special precipitating reagent removal of impurities is filtered, are combined by various methods such as crystallizations, by a kind of quality compared with
The MAP of the more agricultural gray powderies of impurity such as low and lower-cost sulfur-bearing, iron, magnesium, aluminium, manganese, titanium or production
The slip before granulation is not concentrated during phosphate fertilizer to carry out purifying the technical grade for obtaining high added value and LITHIUM BATTERY MAP.Currently nobody
LITHIUM BATTERY MAP is prepared by the method with the phosphate fertilizer or its slip of the poor quality, in LITHIUM BATTERY MAP field also
Unmanned repeatedly regulation pH and final step carry out removal of impurities with special precipitating reagent.A kind of chemical fertilizer level MAP of this patent is produced
The method of industrial one-level and LITHIUM BATTERY MAP, the preparation process is specific as follows:
A. by powdered fertilizer MAP pure water heating for dissolving, uniform rear filtration is thoroughly mixed, filtrate is stand-by；
B. decolorising agent is added in the filtrate for obtaining to a steps, decolouring 1-25h is stood, precipitating reagent is added, pH value is adjusted, fully
Uniform, standing 0.5-5h is mixed and stirred for, is filtered, filtrate is stand-by；
C. the filtrate obtained in b step is continuously added into precipitating reagent, adjusts pH value, be sufficiently mixed and stir, stand 0.5-
5h, filters, and filtrate is stand-by；
D. the filtrate obtained in step c is continuously added into removal of impurities medicament, is sufficiently mixed and stirs, stand 0.5-5h, filtered,
Filtrate is stand-by；
E. by filtrate in b be heated to 60-95 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain industry
One-level MAP；
F. by filtrate in d be heated to 60-95 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain phosphoric acid
Iron MAP.
The product obtained using the inventive method e step meets industrial one-level MAP quality standard：Main content >=
98.5%, nitrogen content >=11.8%, insoluble matter≤0.1%, moisture≤0.5%, fluorine ion ＜ 0.02%, sulfate radical ＜ 0.9%, arsenic≤
0.005%；
The product obtained using the inventive method f step meets battery-grade iron phosphate MAP（LITHIUM BATTERY MAP）Matter
Amount standard：Main content >=99%, nitrogen content >=11.8%, sodium≤0.02%, potassium≤0.02%, calcium≤0.001%, chromium≤0.001%, manganese
≤ 0.005%, copper≤0.0005%, lead≤0.0005%, nickel≤0.0005%, zinc≤0.0005%, magnesium≤0.0005%, fluorine ion ＜
0.0005%, arsenic≤0.001%.
Specific embodiment
Embodiment 1
A. 600g powdered fertilizers MAP 800g pure water is dissolved, is heated to 40 DEG C of stirring 30min, mistake after uniform mixing
Filter, filtrate is stand-by；
B. be passed through the decolorising agent ozone of filtrate quality 5% in the filtrate for obtaining to a steps, stand decolouring 5h, add precipitating reagent ammoniacal liquor and
Sodium carbonate, adjusts pH=4, is sufficiently mixed and stirs, and stands 5h, filters, and filtrate is stand-by；
C. the filtrate obtained in b step is continuously added into precipitating reagent ammoniacal liquor and potassium carbonate, adjusts pH=6, be sufficiently mixed and stir
It is even, 5h is stood, to filter, filtrate is stand-by；
D., the filtrate obtained in step c is continuously added the removal of impurities medicament potassium sulfide and NaOH of filtrate quality 5%, it is fully mixed
Merging stirs, and stands 0.5h, filters, and filtrate is stand-by；
E. by filtrate in b be heated to 60 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain industrial one-level phosphorus
A sour ammonium；
F. by filtrate in d be heated to 60 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain LITHIUM BATTERY phosphoric acid
One ammonium.
The present embodiment e walks the product quality indicator for obtaining：Main content：98.51%, nitrogen content：11.95%, insoluble matter：
0.05%, moisture：0.02%, fluorine ion：0.01%, sulfate radical：0.72%, arsenic：0.004%；Industrial one-level MAP is reached
Standard is required；
The present embodiment f walks the product quality indicator for obtaining：Main content：99.10%, nitrogen content：12.10%, sodium：0.014%, potassium：
0.009%, calcium：0.0005%, chromium：0.0003%, manganese：0.0045%, copper：0.0004%, lead：0.0003%, nickel：0.0001%, zinc：
0.0001%, magnesium：0.0005%, fluorine ion：0.0001%, arsenic：0.0005%.The standard for having reached LITHIUM BATTERY MAP is required.
Embodiment 2
A. 600g powdered fertilizers MAP 800g pure water is dissolved, 70 DEG C of stirring stirring 20min is heated to, after uniform mixing
Filter, filtrate is stand-by；
B. add the decolorising agent calcium hypochlorite of filtrate quality 10% in the filtrate for obtaining to a steps, stand decolouring 12h, add precipitating reagent
Ammoniacal liquor and ammonium carbonate, adjust pH=5, are sufficiently mixed and stir, and stand 3h, filter, and filtrate is stand-by；
C. the filtrate obtained in b step is continuously added into precipitating reagent ammoniacal liquor and sodium carbonate, adjusts pH=7.5, be sufficiently mixed and stir
Uniformly, 3.5h is stood, is filtered, filtrate is stand-by；
D., the filtrate obtained in step c is continuously added the removal of impurities medicament vulcanized sodium and potassium hydroxide of filtrate quality 2%, it is fully mixed
Merging stirs, and stands 3.5h, filters, and filtrate is stand-by；
E. by filtrate in b be heated to 80 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain industrial one-level phosphorus
A sour ammonium；
F. by filtrate in d be heated to 80 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain LITHIUM BATTERY phosphoric acid
One ammonium.
The present embodiment e walks the product quality indicator for obtaining：Main content：98.51%, nitrogen content：11.98%, insoluble matter：
0.03%, moisture：0.01%, fluorine ion：0.012%, sulfate radical：0.57%, arsenic：0.0026%；Industrial one-level MAP is reached
Standard require；
The present embodiment f walks the product quality indicator for obtaining：Main content：99.08%, nitrogen content：12.66%, sodium：0.016%, potassium：
0.008%, calcium：0.0005%, chromium：0.0004%, manganese：0.0035%, copper：0.0004%, lead：0.0005%, nickel：0.0001%, zinc：
0.0001%, magnesium：0.0004%, fluorine ion：0.0002%, arsenic：0.0004%.The standard for having reached LITHIUM BATTERY MAP is required.
Embodiment 3
A. 600g powdered fertilizers MAP 800g pure water is dissolved, is heated to 95 DEG C of stirring 5min, filtered after uniform mixing,
Filtrate is stand-by；
B. add the decolorising agent hydrogen peroxide of filtrate quality 20% in the filtrate for obtaining to a steps, stand decolouring 25h, add precipitating reagent
Ammoniacal liquor and potassium hydroxide, adjust pH=6, are sufficiently mixed and stir, and stand 5h, filter, and filtrate is stand-by；
C. the filtrate obtained in b step is continuously added into precipitating reagent ammoniacal liquor and NaOH, adjusts pH=9, be sufficiently mixed and stir
Uniformly, 0.5h is stood, is filtered, filtrate is stand-by；
D., the filtrate obtained in step c is continuously added the removal of impurities medicament potassium sulfide and ammonium carbonate of filtrate quality 0.1%, it is fully mixed
Merging stirs, and stands 5h, filters, and filtrate is stand-by；
E. by filtrate in b be heated to 95 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain industrial one-level phosphorus
A sour ammonium；
F. by filtrate in d be heated to 95 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain LITHIUM BATTERY phosphoric acid
One ammonium.
The present embodiment e walks the product quality indicator for obtaining：Main content：98.51%, nitrogen content：11.95%, insoluble matter：
0.04%, moisture：0.01%, fluorine ion：0.01%, sulfate radical：0.66%, arsenic：0.004%.Industrial one-level MAP is reached
Standard is required；
The present embodiment f walks the product quality indicator for obtaining：Main content：99.15%, nitrogen content：12.08%, sodium：0.013%, potassium：
0.008%, calcium：0.0004%, chromium：0.0003%, manganese：0.0038%, copper：0.0004%, lead：0.0004%, nickel：0.0001%, zinc：
0.0001%, magnesium：0.0005%, fluorine ion：0.0001%, arsenic：0.0005%.The standard for having reached LITHIUM BATTERY MAP is required.
Embodiment 4
A. 600g powdered fertilizers MAP 800g pure water is dissolved, 75 DEG C of stirring stirring 20min is heated to, after uniform mixing
Filter, filtrate is stand-by；
B. add the decolorising agent chlorine of filtrate quality 0.1% in the filtrate for obtaining to a steps, stand decolouring 1h, add precipitating reagent ammoniacal liquor
And NaOH, pH=5.5 is adjusted, it is sufficiently mixed and stirs, 3.5h is stood, to filter, filtrate is stand-by；
C. the filtrate obtained in b step is continuously added into precipitating reagent ammoniacal liquor and potassium hydroxide, adjusts pH=7.5, be sufficiently mixed and stir
Mix uniform, stand 3.5h, filter, filtrate is stand-by；
D., the filtrate obtained in step c is continuously added the removal of impurities medicament ammonium sulfide and sodium carbonate of filtrate quality 0.1%, it is fully mixed
Merging stirs, and stands 3.5h, filters, and filtrate is stand-by；
E. by filtrate in b be heated to 80 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain industrial one-level phosphorus
A sour ammonium；
F. by filtrate in d be heated to 80 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain LITHIUM BATTERY phosphoric acid
One ammonium.
The present embodiment e walks the product quality indicator for obtaining：Main content：98.58%, nitrogen content：11.93%, insoluble matter：
0.03%, moisture：0.01%, fluorine ion：0.01%, sulfate radical：0.68%, arsenic：0.003%.Industrial one-level MAP is reached
Standard is required；
The present embodiment f walks the product quality indicator for obtaining：Main content：99.12%, nitrogen content：12.16%, sodium：0.010%, potassium：
0.0065%, calcium：0.0001%, chromium：0.0003%, manganese：0.0039%, copper：0.0004%, lead：0.0004%, nickel：0.0001%, zinc：
0.0001%, magnesium：0.0005%, fluorine ion：0.0001%, arsenic：0.0004%.The standard for having reached LITHIUM BATTERY MAP is required.
Embodiment 5
A. 600g powdered fertilizers MAP 800g pure water is dissolved, 90 DEG C of stirring stirring 10min is heated to, after uniform mixing
Filter, filtrate is stand-by；
B. add the decolorising agent sodium hypochlorite of filtrate quality 0.2% in the filtrate for obtaining to a steps, stand decolouring 1h, add precipitating reagent
Ammonia and ammonium carbonate, adjust pH=6, are sufficiently mixed and stir, and stand 5h, filter, and filtrate is stand-by；
C. the filtrate obtained in b step is continuously added into precipitating reagent ammoniacal liquor and potassium carbonate, adjusts pH=8, be sufficiently mixed and stir
It is even, 5h is stood, to filter, filtrate is stand-by；
D., the filtrate obtained in step c is continuously added the removal of impurities medicament ammonium sulfide and potassium carbonate of filtrate quality 0.5%, it is fully mixed
Merging stirs, and stands 5h, filters, and filtrate is stand-by；
E. by filtrate in b be heated to 90 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain industrial one-level phosphorus
A sour ammonium；
F. by filtrate in d be heated to 90 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain LITHIUM BATTERY phosphoric acid
One ammonium.
The present embodiment e walks the product quality indicator for obtaining：Main content：98.59%, nitrogen content：11.90%, insoluble matter：
0.01%, moisture：0.008%, fluorine ion：0.008%, sulfate radical：0.56%, arsenic：0.0035%.Industrial one-level phosphoric acid one is reached
The standard of ammonium is required；
The present embodiment f walks the product quality indicator for obtaining：Main content：99.08%, nitrogen content：12.10%, sodium：0.019%, potassium：
0.0068%, calcium：0.0002%, chromium：0.0003%, manganese：0.0035%, copper：0.0002%, lead：0.0004%, nickel：0.0001%, zinc：
0.0001%, magnesium：0.0003%, fluorine ion：0.0001%, arsenic：0.0002%.The standard for having reached LITHIUM BATTERY MAP is required.
Claims (6)
1. a kind of method that use chemical fertilizer level MAP produces industrial one-level and LITHIUM BATTERY MAP, it is characterised in that：Specifically
Step is as follows:
A. by powdered fertilizer MAP pure water heating for dissolving, uniform rear filtration is thoroughly mixed, filtrate is stand-by；
B. decolorising agent is added in the filtrate for obtaining to a steps, decolouring 1-25h is stood, precipitating reagent is added, pH value is adjusted, fully
Uniform, standing 0.5-5h is mixed and stirred for, is filtered, filtrate is stand-by；
C. the filtrate obtained in b step is continuously added into precipitating reagent, adjusts pH value, be sufficiently mixed and stir, stand 0.5-
5h, filters, and filtrate is stand-by；
D. the filtrate obtained in step c is continuously added into removal of impurities medicament, is sufficiently mixed and stirs, stand 0.5-5h, filtered,
Filtrate is stand-by；
E. by filtrate in b be heated to 60-95 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain industry
One-level MAP；
F. by filtrate in d be heated to 60-95 DEG C be concentrated into micro-crystallization occur till, crystallisation by cooling, be dried after obtain battery
Level MAP.
2. a kind of use chemical fertilizer level MAP according to claim 1 produces the side of industrial one-level and LITHIUM BATTERY MAP
Method, it is characterised in that heating-up temperature is 40-95 DEG C in step a, and mixing time is 5-30min.
3. a kind of use chemical fertilizer level MAP according to claim 1 produces the side of industrial one-level and LITHIUM BATTERY MAP
Method, it is characterised in that decolorising agent is in step b：In hydrogen peroxide, sodium hypochlorite, calcium hypochlorite, chlorine, ozone it is a kind of or
Several mixtures, addition is the 0.1%-20% of filtrate weight；Added precipitating reagent is:Potassium carbonate, sodium carbonate, ammonium carbonate, ammonia
The mixture of one or more in water, ammonia, NaOH, potassium hydroxide, the pH value for being adjusted is 4-7.
4. a kind of use chemical fertilizer level MAP according to claim 1 produces industrial one-level and LITHIUM BATTERY MAP
Method, it is characterised in that precipitating reagent is in step c:Potassium carbonate, sodium carbonate, ammonium carbonate, ammoniacal liquor, ammonia, NaOH,
The mixture of one or more in potassium hydroxide, the pH value for being adjusted is 6-9.
5. a kind of use chemical fertilizer level MAP according to claim 1 produces industrial one-level and LITHIUM BATTERY MAP
Method, it is characterised in that removal of impurities medicament is in step d:Ammonium sulfide, vulcanized sodium, potassium sulfide, sodium carbonate, potassium carbonate, carbonic acid
The mixture of one or more in ammonium, potassium hydroxide, NaOH, addition is the 0.1%-5% of filtrate quality.
6. a kind of use chemical fertilizer level MAP according to claim 1 produces the side of industrial one-level and LITHIUM BATTERY MAP
Method, it is characterised in that concentrate in step e, f and concentrated for vacuum distillation, temperature is 60-95 DEG C, is crystallized as stirring cooling knot
Crystalline substance, cooling medium is desalted water or deionized water, and drying means used is vacuum drying oven drying.
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| CN107746044A (en) * | 2017-12-06 | 2018-03-02 | 上海新增鼎工业科技有限公司 | A kind of method for producing industrial grade monoammonium phosphate with agricultural MAP |
| CN115285956A (en) * | 2022-06-21 | 2022-11-04 | 贵阳开磷化肥有限公司 | Method for directly producing battery grade monoammonium phosphate from wet-process phosphoric acid |
| CN116553499A (en) * | 2023-04-25 | 2023-08-08 | 浙江友山新材料有限公司 | Monoammonium phosphate purification method |
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Effective date of registration: 20210610 Address after: 435406 Xiangyun group headquarters supply and marketing building, Tianzhen Town, Wuxue City, Huanggang City, Hubei Province Patentee after: Hubei Yunxiang Juneng New Energy Technology Co.,Ltd. Address before: No. 202, Yannong Chuangye building, Changsha hi tech Industrial Development Zone, Hunan 410205 Patentee before: HUNAN ZHENGYUAN INSTITUTE FOR ENERGY STORAGE MATERIALS AND DEVICES |
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Denomination of invention: A method for producing industrial grade and battery grade ammonium phosphate using fertilizer grade ammonium phosphate Granted publication date: 20181109 Pledgee: China Postal Savings Bank Co.,Ltd. Wuxue Branch Pledgor: Hubei Yunxiang Juneng New Energy Technology Co.,Ltd. Registration number: Y2024980004653 |