CN103011298A - Method for production of high purity manganese sulfate by using metal manganese sheet as raw material - Google Patents
Method for production of high purity manganese sulfate by using metal manganese sheet as raw material Download PDFInfo
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- CN103011298A CN103011298A CN201210519872XA CN201210519872A CN103011298A CN 103011298 A CN103011298 A CN 103011298A CN 201210519872X A CN201210519872X A CN 201210519872XA CN 201210519872 A CN201210519872 A CN 201210519872A CN 103011298 A CN103011298 A CN 103011298A
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- manganese
- purity
- manganese metal
- metal
- deionized water
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- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 title claims abstract description 55
- 235000007079 manganese sulphate Nutrition 0.000 title claims abstract description 40
- 239000011702 manganese sulphate Substances 0.000 title claims abstract description 40
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229940099596 manganese sulfate Drugs 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000002994 raw material Substances 0.000 title abstract description 9
- 239000011572 manganese Substances 0.000 title abstract description 5
- 229910052748 manganese Inorganic materials 0.000 title abstract description 4
- 229910052751 metal Inorganic materials 0.000 title abstract 2
- 239000002184 metal Substances 0.000 title abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- ISPYRSDWRDQNSW-UHFFFAOYSA-L manganese(II) sulfate monohydrate Chemical compound O.[Mn+2].[O-]S([O-])(=O)=O ISPYRSDWRDQNSW-UHFFFAOYSA-L 0.000 claims description 12
- 230000018044 dehydration Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 10
- 238000005868 electrolysis reaction Methods 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000003978 infusion fluid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000012452 mother liquor Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 12
- 230000008025 crystallization Effects 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 229910052708 sodium Inorganic materials 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 1
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 abstract 1
- 238000002161 passivation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 4
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- RLBLFSQXAKQALA-UHFFFAOYSA-N [Na].[K].[Mg].[Ca] Chemical compound [Na].[K].[Mg].[Ca] RLBLFSQXAKQALA-UHFFFAOYSA-N 0.000 description 3
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- -1 feed Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229910052935 jarosite Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 1
- KNLQKHUBPCXPQD-UHFFFAOYSA-N manganese;sulfuric acid Chemical compound [Mn].OS(O)(=O)=O KNLQKHUBPCXPQD-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The invention relates to a production method for high purity manganese sulfate. The production method is characterized in that a metal manganese sheet is used as a raw material and is directly added in concentrated sulfuric acid for leaching to obtain a high purity manganese sulfate solution without passivation and drying, and then crystallization is carried out to obtain a high purity manganese sulfate product. According to the invention, no impurity removing agent is needed, process flow is simple, and the high purity manganese sulfate product in which MnSO4 content is more than 99.8% and respective content of impurities consisting of Ca, Mg, K and Na is lower than 10 ppm is produced.
Description
Technical field
The present invention relates to a kind of production method of high-purity manganese sulphate, specifically adopting the manganese metal sheet is raw material, produces manganese sulfate monohydrate content more than 99.9%, calcium magnesium potassium sodium impurity all less than the method for the high-purity sulphuric acid manganese product of 10ppm.
Background technology
Manganous sulfate is a kind of traditional manganese product salt, and purposes is very extensive.At present, domestic production of manganese sulfate as, mainly take pyrolusite as raw material, divide two kinds of reduction of carbon fire reduction and wet reducing (reductive agents such as sulfurous iron ore, ferrous sulfate or titanium white waste acid) acidleach extract technology technology, and then carry out simple oxidation-hydrolysis deironing, sulfuration removing heavy metals, filter, staticly settle, solution crystallization, centrifuge dehydration oven dry, obtain technical grade, feed grade or three kinds of other manganese sulfate products of level of elaboration level, be used for the fields such as chemical fertilizer, feed, paint, agricultural chemicals.In recent years, along with the development of New Energy Sources lithium manganate battery technology, more and more come into one's own take high purity manganese sulfate as the raw material production lithium manganate, Technology is also more and more ripe.And consider that for various reasons such as environment protection, cost consumptions particularly the developed countries such as America and Europe, Japan and Korea S almost do not have manganous sulfate production abroad; China has become in the world main manganous sulfate producing country and supply country, about 150,000 tons of annual output.Therefore, overseas lithium manganate battery manufacturer wishes to seek high-purity manganous sulfate material in China, is used for tapping a new source of energy lithium cell.
Product specification requires as follows: Mn:31.5%MIN, Fe:0.0005%MAX, K:0.01% MAX, Na:0.01% MAX, Co:0.003% MAX, Zn:0.001% MAX, Ca:0.01%MAX, Mg:0.01%MAX, Ni:0.003%MAX.
And no matter domestic production of manganese sulfate as technology is wet method or pyrogenic process, and the purification and impurity removal technology all only rests on oxidation-hydrolysis deironing, sulfuration removing heavy metals simple process stage, the low (MnSO of product master content
4H
2O is between 98% ~ 98.5%), foreign matter content high (calcium-magnesium content all more than 1200ppm, each about 600ppm of potassium sodium content), can't reach above high purity manganese sulfate technical requirement far away.Therefore, from original ore powder, expect to make the product that meets high-purity index request, mainly be will calcium magnesium and potassium sodium are technical to make a breakthrough and improve purifying.Aspect purification potassium sodium, Chinese patent 201010243859.7 high purity manganese sulfate monohydrates and preparation method thereof, 200910193398.4 the preparation method of an electronic grade high-purity manganese sulfate monohydrate, announced adding iron content medicament, by generating the potassium sodium impurity in jarosite, the yellow sodium ferrovanadium removal manganese sulfate solution; Taking off aspect the calcium-magnesium removing, Chinese patent 201010243859.7 high purity manganese sulfate monohydrates and preparation method thereof, 200910006889.3 method for preparing high-purity manganese sulphate, 200910006888.9 the preparation method of a high purity manganese sulfate adopts all kinds of fluorochemicals generation of adding Calcium Fluoride (Fluorspan), magnesium fluoride precipitation to remove calcium-magnesium removing.These methods need strict control temperature of reaction and pH value, consume a large amount of highly purified removal of impurities medicaments, are unfavorable for reducing production costs.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of high-purity manganese sulphate, the manganese metal that the present invention adopts firm electrolysis to go out groove is raw material, use sulfuric acid dissolution, obtain manganese sulfate solution, through crystallization, after centrifuge dehydration and the oven dry, obtain content greater than 99.8% manganese sulfate product, present method does not need to add the chemical reagent removal of impurities, and technique is simple, the manganese sulfate product purity that makes is high, can satisfy the demand of special occasions.
Technical scheme of the present invention is:
The production method of high-purity manganese sulphate, it is characterized in that: the manganese metal that goes out groove with the deionized water rinsing electrolysis, drop into retort, add deionized water, stir the lower vitriol oil that slowly adds and soak manganese metal, the weight concentration of the sulfuric acid that adds is 90-98%, the mol ratio of manganese metal and sulfuric acid is 1～1.1:1, makes that the content of manganous sulfate reaches 350g/L～500g/L in the infusion solution, and the terminal point pH value of solution reaches 4.0～6.0, filter, the filtrate heating evaporation makes manganese sulfate solution concentration reach 600～800g/L, leaves standstill, be cooled to room temperature, separate out the Manganous sulfate monohydrate crystal, dry with the whizzer centrifuge dehydration, drying obtains high-purity manganese sulphate again, the purity of manganous sulfate is greater than 99.8%, and the content of the impurity such as calcium magnesium potassium sodium is all less than 10ppm.
The mother liquor that above-mentioned crystallisation process obtains turns back to the acid soak operation of manganese metal, soaks manganese metal with deionized water, the vitriol oil.
Advantage of the present invention:
1. the present invention's manganese metal of adopting electrolysis to obtain is raw material, and raw material impurity is few, does not need to add any chemical substance removal of impurities, and technique is simple, and flow process is short, and products obtained therefrom purity is very high, reaches more than 99.8%.
2. method removal of impurities process temperature of the present invention and pH value do not have special stipulation, and these parameters do not need strict control, and be therefore simple to operate, allows easily producers grasp.
Embodiment
Embodiment 1
Go out the manganese metal of groove with the deionized water rinsing electrolysis, drop into retort, add deionized water, stir the lower vitriol oil that slowly adds and soak manganese metal, the weight concentration of the sulfuric acid that adds is 90%, the mol ratio of manganese metal and sulfuric acid is 1:1, makes that the content of manganous sulfate reaches 350g/L in the infusion solution, and the terminal point pH value of solution reaches 4.0, filter, the filtrate heating evaporation makes manganese sulfate solution concentration reach 600g/L, leaves standstill, be cooled to room temperature, separate out the Manganous sulfate monohydrate crystal, dry with the whizzer centrifuge dehydration, drying obtains high-purity manganese sulphate again.
Embodiment 2
Go out the manganese metal of groove with the deionized water rinsing electrolysis, drop into retort, add the mother liquor that deionized water and embodiment 1 obtain, stir the lower vitriol oil that slowly adds and soak manganese metal, the weight concentration of the sulfuric acid that adds is 95%, the mol ratio of manganese metal and sulfuric acid is 1.05:1, makes that the content of manganous sulfate reaches 380g/L in the infusion solution, and the terminal point pH value of solution reaches 4.0, filter, the filtrate heating evaporation makes manganese sulfate solution concentration reach 600g/L, leaves standstill, be cooled to room temperature, separate out the Manganous sulfate monohydrate crystal, dry with the whizzer centrifuge dehydration, drying obtains high-purity manganese sulphate again.
Embodiment 3
Go out the manganese metal of groove with the deionized water rinsing electrolysis, drop into retort, add the mother liquor that deionized water and embodiment 2 obtain, stir the lower vitriol oil that slowly adds and soak manganese metal, the weight concentration of the sulfuric acid that adds is 95%, the mol ratio of manganese metal and sulfuric acid is 1.02:1, makes that the content of manganous sulfate reaches 400g/L in the infusion solution, and the terminal point pH value of solution reaches 5.0, filter, the filtrate heating evaporation makes manganese sulfate solution concentration reach 650g/L, leaves standstill, be cooled to room temperature, separate out the Manganous sulfate monohydrate crystal, dry with the whizzer centrifuge dehydration, drying obtains high-purity manganese sulphate again.
Embodiment 4
Go out the manganese metal of groove with the deionized water rinsing electrolysis, drop into retort, add the mother liquor that deionized water and embodiment 1 obtain, stir the lower vitriol oil that slowly adds and soak manganese metal, the weight concentration of the sulfuric acid that adds is 98%, the mol ratio of manganese metal and sulfuric acid is 1.06:1, makes that the content of manganous sulfate reaches 450g/L in the infusion solution, and the terminal point pH value of solution reaches 6.0, filter, the filtrate heating evaporation makes manganese sulfate solution concentration reach 700g/L, leaves standstill, be cooled to room temperature, separate out the Manganous sulfate monohydrate crystal, dry with the whizzer centrifuge dehydration, drying obtains high-purity manganese sulphate again.
Embodiment 5
Go out the manganese metal of groove with the deionized water rinsing electrolysis, drop into retort, add the mother liquor that deionized water and embodiment 1 obtain, stir the lower vitriol oil that slowly adds and soak manganese metal, the weight concentration of the sulfuric acid that adds is 98%, the mol ratio of manganese metal and sulfuric acid is 1.08:1, makes that the content of manganous sulfate reaches 500g/L in the infusion solution, and the terminal point pH value of solution reaches 4.5, filter, the filtrate heating evaporation makes manganese sulfate solution concentration reach 750g/L, leaves standstill, be cooled to room temperature, separate out the Manganous sulfate monohydrate crystal, dry with the whizzer centrifuge dehydration, drying obtains high-purity manganese sulphate again.
Embodiment 6
Go out the manganese metal of groove with the deionized water rinsing electrolysis, drop into retort, add the mother liquor that deionized water and embodiment 1 obtain, stir the lower vitriol oil that slowly adds and soak manganese metal, the weight concentration of the sulfuric acid that adds is 98%, the mol ratio of manganese metal and sulfuric acid is 1.1:1, makes that the content of manganous sulfate reaches 500g/L in the infusion solution, and the terminal point pH value of solution reaches 5.5, filter, the filtrate heating evaporation makes manganese sulfate solution concentration reach 800g/L, leaves standstill, be cooled to room temperature, separate out the Manganous sulfate monohydrate crystal, dry with the whizzer centrifuge dehydration, drying obtains high-purity manganese sulphate again.
Table 1 obtains manganese content and the foreign matter content result of manganese sulfate product for embodiment
It can be seen from the table the present invention produce the manganous sulfate that the method for high-purity manganese sulphate produces purity all greater than 99.8%, the content of the impurity such as calcium magnesium potassium sodium is all less than 10ppm.
Claims (2)
1. the production method of a high-purity manganese sulphate, it is characterized in that: the manganese metal that goes out groove with the deionized water rinsing electrolysis, drop into retort, add deionized water, stir the lower vitriol oil that slowly adds and soak manganese metal, the weight concentration of the sulfuric acid of adding is 90-98%, and the mol ratio of manganese metal and sulfuric acid is 1～1.1:1, make that the content of manganous sulfate reaches 350g/L～500g/L in the infusion solution, the terminal point pH value of solution reaches 4.0～6.0, filters the filtrate heating evaporation, make manganese sulfate solution concentration reach 600～800g/L, leave standstill, be cooled to room temperature, separate out the Manganous sulfate monohydrate crystal, dry with the whizzer centrifuge dehydration, drying obtains high-purity manganese sulphate again.
2. the production method of high-purity manganese sulphate according to claim 1, it is characterized in that: the mother liquor that crystallisation process obtains turns back to the acid soak operation of manganese metal, soaks manganese metal with deionized water, the vitriol oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210519872XA CN103011298A (en) | 2012-12-07 | 2012-12-07 | Method for production of high purity manganese sulfate by using metal manganese sheet as raw material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210519872XA CN103011298A (en) | 2012-12-07 | 2012-12-07 | Method for production of high purity manganese sulfate by using metal manganese sheet as raw material |
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| CN103011298A true CN103011298A (en) | 2013-04-03 |
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| CN201210519872XA Pending CN103011298A (en) | 2012-12-07 | 2012-12-07 | Method for production of high purity manganese sulfate by using metal manganese sheet as raw material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107640789A (en) * | 2017-10-25 | 2018-01-30 | 成都先进金属材料产业技术研究院有限公司 | A kind of manganese sulfate preparation method for lithium battery |
| CN108622941A (en) * | 2018-05-09 | 2018-10-09 | 湘潭埃索凯生化科技有限公司 | A kind of environmental friendly method and apparatus preparing high purity manganese sulfate using industrial manganese |
| CN114835167A (en) * | 2022-04-13 | 2022-08-02 | 贵州大龙汇成新材料有限公司 | Process for producing manganese sulfate by using poor manganese ore |
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- 2012-12-07 CN CN201210519872XA patent/CN103011298A/en active Pending
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| CN101767827A (en) * | 2008-12-31 | 2010-07-07 | 杜祖德 | Method for recycling manganese sulfate by using electrolytic metal manganese waste slag |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107640789A (en) * | 2017-10-25 | 2018-01-30 | 成都先进金属材料产业技术研究院有限公司 | A kind of manganese sulfate preparation method for lithium battery |
| CN108622941A (en) * | 2018-05-09 | 2018-10-09 | 湘潭埃索凯生化科技有限公司 | A kind of environmental friendly method and apparatus preparing high purity manganese sulfate using industrial manganese |
| CN114835167A (en) * | 2022-04-13 | 2022-08-02 | 贵州大龙汇成新材料有限公司 | Process for producing manganese sulfate by using poor manganese ore |
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Application publication date: 20130403 |