CN103626239B - Method for removing manganese out of titanium dioxide byproduct ferrous sulfate - Google Patents
Method for removing manganese out of titanium dioxide byproduct ferrous sulfate Download PDFInfo
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- ferrous sulfate
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- product ferrous
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- 235000003891 ferrous sulphate Nutrition 0.000 title claims abstract description 62
- 239000011790 ferrous sulphate Substances 0.000 title claims abstract description 62
- 229910000359 iron(II) sulfate Inorganic materials 0.000 title claims abstract description 62
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000006227 byproduct Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 45
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 title claims description 55
- 239000011572 manganese Substances 0.000 title abstract description 20
- 229910052748 manganese Inorganic materials 0.000 title abstract description 7
- 239000004408 titanium dioxide Substances 0.000 title abstract description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 235000010215 titanium dioxide Nutrition 0.000 claims description 43
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 27
- 239000006228 supernatant Substances 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 238000005189 flocculation Methods 0.000 claims description 14
- 230000016615 flocculation Effects 0.000 claims description 14
- 238000000967 suction filtration Methods 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000000706 filtrate Substances 0.000 abstract description 7
- 238000005342 ion exchange Methods 0.000 abstract description 5
- 238000001953 recrystallisation Methods 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 abstract 8
- 238000001914 filtration Methods 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000002203 pretreatment Methods 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- -1 catalyzer Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 229940062993 ferrous oxalate Drugs 0.000 description 1
- 229940116007 ferrous phosphate Drugs 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001034 iron oxide pigment Substances 0.000 description 1
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 description 1
- 229910000155 iron(II) phosphate Inorganic materials 0.000 description 1
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 description 1
- 239000010871 livestock manure Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Abstract
The invention relates to a method for removing manganese out of a titanium dioxide byproduct ferrous sulfate, belonging to the technical field of impurity removal of ferrous sulfate. The method comprises the following steps: dissolving the titanium dioxide byproduct ferrous sulfate and carrying out a series of pre-treatments to obtain a ferrous sulfate clear liquid; evaporating and concentrating the ferrous sulfate clear liquid and filtering when the ferrous sulfate clear liquid is hot; then, cooling and crystallizing the filtrate and filtering; and drying filter residues to finally obtain a ferrous sulfate heptahydrate solid with relatively high purity. According to the method provided by the invention, Mn and other impurities can be removed through repeated recrystallization. Compared with an ion exchange method for impurity removal by which the removal rate of Mn is just 12.5%, the method provided by the invention has the advantages of high impurity removal rate and simple technical flow. The removal rate of Mn is over 69.56%, so that the titanium dioxide byproduct ferrous sulfate is effectively purified.
Description
Technical field
The present invention relates to a kind of method of titanium white by product ferrous sulfate demanganization, belong to ferrous sulfate impurity removing technology field.
Background technology
Ferrous sulfate is of many uses, is typically used as water purification agent, additive, catalyzer, sorbent material, compound manure etc.Titanium White Production By Sulfuric Acid Process, the by product of pickling iron and steel process is ferrous sulfate.According to statistics, often produce 1t titanium dioxide, about produce 3 ~ 4tFeSO
47H
2o, the whole nation is annual produces titanium white by product product ferrous sulfate about 3,000,000 t, because it is containing plurality of impurities, can not directly utilize, a part is used as water purification agent, fertilizer and fodder additives, and a part is for the production of iron oxide pigment, the overwhelming majority is abandoned as waste, or stack everywhere, not only waste sulphur and iron resources, and serious environment pollution.
In lithium ion battery industry, the ferrous sulfate that purity is higher can be used for the starting material Ferrox preparing lithium ferrous phosphate as anode material of lithium ion battery.The height of Ferrox purity and the size of particle diameter are to the LiFePO 4 performance impact of synthesis very greatly, correspondingly higher to the purity requirement of ferrous sulfate.Titanium white by product product ferrous sulfate is carried out purification processes, is expected to for the raw-material preparation of lithium ion battery industry.Conventional impurity-removing method mainly ion exchange method, but the removal effect of ion exchange method to Mn is not obvious.
In recent years, the development of the portable energy storage devices such as 3G mobile, energy storage device, electromobile, electric bicycle impels the develop rapidly of lithium electrical travelling industry, increase considerably the demand of lithium cell, the market capacity of its starting material Ferrox also will sharply expand, and market outlook are very wide.If a large amount of titanium white by product product ferrous sulfate can be carried out purification processes to prepare cell-grade high purity superfine ferrous oxalate, the heavy demand of supply lithium cell industry, the problem of environmental pollution that ferrous sulfate bulk deposition causes can be solved, the demand of lithium cell industry for Ferrox can be met again, promote the development of power cell industry.
Summary of the invention
For solving the deficiencies in the prior art, the present invention proposes a kind of method of titanium white by product ferrous sulfate demanganization, adopt recrystallization method demanganization to prepare the higher ferrous sulfate of purity, provide that a kind of manganese clearance is high, flow process is short, cost is low, the novel method of environment amenable titanium white by product ferrous sulfate demanganization.
Technical scheme of the present invention is: dissolved by titanium white by product ferrous sulfate, and carry out a series of early stage process obtain ferrous sulfate clear liquid, by ferrous sulfate clear liquid evaporation concentration and filtered while hot, again by filtrate crystallisation by cooling, and filter, filter residue is dried, finally obtains the ferrous sulfate solid that purity is higher.Concrete steps comprise as follows:
(1) titanium white by product ferrous sulfate is dissolved in water is modulated into the solution that concentration is 26 ~ 41wt%, then in solution, iron powder is added according to solid-to-liquid ratio 1.5 ~ 2.7:100g/ml, the pH of regulator solution is 1.5 ~ 2.5 again, and under the condition of isolated air, be heated to the temperature 3 ~ 5 hours of 70 ~ 80 DEG C;
(2) in the solution after step (1) insulation, flocculation agent is added, supernatant liquid is isolated after solution layering, supernatant liquid is constantly stirred also ebuillition of heated and be evaporated to less than 2/3 of former supernatant volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally obtained by suction filtration is dried, namely obtain the ferrous sulfate after demanganization, the clearance of Mn is 52.5% ~ 69.56%(Mn content is 0.016wt% ~ 0.028wt%).
Described titanium white by product ferrous sulfate is the byproduct (the ferrous sulfate solid that foreign matter content is higher) in Titanium White Production By Sulfuric Acid Process pickling iron and steel process, and purity is 70% ~ 85%, and Fe content is 0.037 ~ 0.092wt%.
The water dissolving titanium white by product ferrous sulfate in described step (1) is deionized water or distilled water.
Described iron powder is analytical pure reduced iron powder.
In described step (1), the pH value of regulator solution adopts sulfuric acid, and sulfuric acid is the vitriol oil or concentration is the dilute sulphuric acid of 30 ~ 50volt%.
The polyacrylamide solution of described flocculation agent to be concentration be 0.3 ~ 0.5wt%.
The add-on of described flocculation agent and the ratio of solution are 0.05 ~ 0.2: 100.
The invention provides a kind of effectively demanganization, flow process is short, cost is low, environment amenable titanium white by product ferrous sulfate demanganization new approaches, beneficial effect is:
(1) the present invention is with titanium white by product ferrous sulfate for raw material, and can prepare the higher ferrous sulfate of purity through recrystallization, this technical process is short, simple to operate.
(2) the present invention removes Mn and other each impurity by the operation repeatedly carrying out recrystallization process, compare ion exchange method removal of impurities, have that impurities removing efficiency is high, the simple advantage of technical process, wherein, the clearance of Mn of the present invention is more than 69.56%, and the clearance of ion exchange method Mn is only 12.5%, titanium white by product ferrous sulfate of effectively having purified.Purity brings up to more than 99%.
(3) the present invention as with titanium white by product ferrous sulfate for the higher ferrous sulfate of purity prepared by raw material, can be used for the raw material of lithium ion battery material, solve titanium white by product ferrous sulfate and stack as waste, abandon, waste sulphur and iron resources, the problem of serious environment pollution.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment one: the method for the titanium white by product ferrous sulfate demanganization of present embodiment is:
(1) titanium white by product ferrous sulfate is dissolved in water is modulated into the solution that concentration is 26wt%, then in solution, iron powder is added according to solid-to-liquid ratio 2.4:100g/ml, be the pH of the dilute sulphuric acid regulator solution of 50volt% again by concentration be 2.5, and with the temperature 5 hours of paraffin sealing post-heating to 70 DEG C (wherein, titanium white by product ferrous sulfate is the byproduct in Titanium White Production By Sulfuric Acid Process pickling iron and steel process, purity is 70%, Mn content is 0.037%, Cu content is 0.00031%, Ni content is 0.0019%; Zn content is 0.0026%; Mg content is 0.87%);
(2) (concentration is the polyacrylamide solution of 0.5wt% in the solution after step (1) insulation, to add flocculation agent, the add-on of flocculation agent and the volume ratio of solution are 0.1: 100), supernatant liquid is isolated after solution layering, supernatant liquid is constantly stirred also ebuillition of heated and be evaporated to 2/3 of former supernatant volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally obtained by suction filtration is dried, and namely obtain the ferrous sulfate after demanganization, the clearance of Mn is 52.5%.
Embodiment two: the method for the titanium white by product ferrous sulfate demanganization of present embodiment is:
(1) titanium white by product ferrous sulfate is dissolved in water is modulated into the solution that concentration is 41wt%, then in solution, iron powder is added according to solid-to-liquid ratio 1.5:100g/ml, be 1.5 with the pH of vitriol oil regulator solution again, and the temperature 3 hours being heated to 80 DEG C under the condition of isolated air (wherein, titanium white by product ferrous sulfate is the byproduct in Titanium White Production By Sulfuric Acid Process pickling iron and steel process, purity is 85%, Mn content is 0.080%);
(2) (concentration is the polyacrylamide solution of 0.4wt% in the solution after step (1) insulation, to add flocculation agent, the add-on of flocculation agent and the volume ratio of solution are 0.05: 100), supernatant liquid is isolated after solution layering, supernatant liquid is constantly stirred also ebuillition of heated and be evaporated to less than 1/3 of former supernatant volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally obtained by suction filtration is dried, and namely obtain the ferrous sulfate after demanganization, the clearance of Mn is 59.70%.
Embodiment three: the method for the titanium white by product ferrous sulfate demanganization of present embodiment is:
(1) titanium white by product ferrous sulfate is dissolved in water is modulated into the solution that concentration is 30wt%, then in solution, iron powder is added according to solid-to-liquid ratio 2.7:100g/ml, be the pH of the dilute sulphuric acid regulator solution of 40volt% again by concentration be 2, and the temperature 4 hours being heated to 78 DEG C under the condition of isolated air (wherein, titanium white by product ferrous sulfate is the byproduct in Titanium White Production By Sulfuric Acid Process pickling iron and steel process, purity is 76%, Mn content is 0.092%);
(2) (concentration is the polyacrylamide solution of 0.3wt% in the solution after step (1) insulation, to add flocculation agent, the add-on of flocculation agent and the volume ratio of solution are 0.1: 100), supernatant liquid is isolated after solution layering, supernatant liquid is constantly stirred also ebuillition of heated and be evaporated to 1/3 of former supernatant volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally obtained by suction filtration is dried, and namely obtain the ferrous sulfate after demanganization, the clearance of Mn is 69.56%.
Embodiment four: the method for the titanium white by product ferrous sulfate demanganization of present embodiment is:
(1) titanium white by product ferrous sulfate is dissolved in water is modulated into the solution that concentration is 38wt%, then in solution, iron powder is added according to solid-to-liquid ratio 2.3:100g/ml, be the pH of the dilute sulphuric acid regulator solution of 30volt% again by concentration be 2.2, and the temperature 3.6 hours being heated to 76 DEG C under the condition of isolated air (wherein, titanium white by product ferrous sulfate is the byproduct in Titanium White Production By Sulfuric Acid Process pickling iron and steel process, purity is 76%, Mn content is 0.092%);
(2) (concentration is the polyacrylamide solution of 0.5wt% in the solution after step (1) insulation, to add flocculation agent, the add-on of flocculation agent and the volume ratio of solution are 0.2: 100), supernatant liquid is isolated after solution layering, supernatant liquid is constantly stirred also ebuillition of heated and be evaporated to 1/4 of former supernatant volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally obtained by suction filtration is dried, and namely obtain the ferrous sulfate after demanganization, the clearance of Mn is 66.29%.
Above the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (5)
1. a method for titanium white by product ferrous sulfate demanganization, is characterized in that concrete steps comprise:
(1) titanium white by product ferrous sulfate is dissolved in water is modulated into the solution that concentration is 26 ~ 41wt%, then in solution, iron powder is added according to solid-to-liquid ratio 1.5 ~ 2.7:100g/mL, the pH of regulator solution is 1.5 ~ 2.5 again, and under the condition of isolated air, be heated to the temperature 3 ~ 5 hours of 70 ~ 80 DEG C;
(2) in the solution after step (1) insulation, flocculation agent is added, supernatant liquid is isolated after solution layering, supernatant liquid is constantly stirred also ebuillition of heated and be evaporated to less than 2/3 of former supernatant volume, again by suction filtration after supernatant liquid crystallisation by cooling, the crystallisate finally obtained by suction filtration is dried, and namely obtains the ferrous sulfate after demanganization.
2. the method for titanium white by product ferrous sulfate demanganization according to claim 1, it is characterized in that: described titanium white by product ferrous sulfate is the byproduct in Titanium White Production By Sulfuric Acid Process pickling iron and steel process, purity is 70% ~ 85%, and Fe content is 0.037 ~ 0.092wt%.
3. the method for titanium white by product ferrous sulfate demanganization according to claim 1, is characterized in that: in described step (1), the pH value of regulator solution adopts sulfuric acid, and sulfuric acid is the vitriol oil or concentration is the dilute sulphuric acid of 30 ~ 50volt%.
4. the method for titanium white by product ferrous sulfate demanganization according to claim 1, is characterized in that: the polyacrylamide solution of described flocculation agent to be concentration be 0.3 ~ 0.5wt%.
5. the method for the titanium white by product ferrous sulfate demanganization according to claim 1 or 4, is characterized in that: the add-on of described flocculation agent and the ratio of solution are 0.05 ~ 0.2: 100.
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| CN201310471549.4A CN103626239B (en) | 2013-10-11 | 2013-10-11 | Method for removing manganese out of titanium dioxide byproduct ferrous sulfate |
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| CN107720833A (en) * | 2017-11-15 | 2018-02-23 | 攀钢集团攀枝花钢铁研究院有限公司 | The process for effectively purifying of byproduct ferrous sulfate of titanium dioxide |
| CN113816354B (en) * | 2021-11-04 | 2023-05-26 | 四川省盈达锂电新材料有限公司 | Method for preparing ferric phosphate by utilizing waste in titanium dioxide production process |
| CN115650310A (en) * | 2022-10-31 | 2023-01-31 | 湘潭大学 | Preparation of alpha-Fe from titanium dioxide waste residue 2 O 3 Method for preparing nano material and its application |
| CN116395752A (en) * | 2023-05-09 | 2023-07-07 | 金川集团股份有限公司 | Preparation and storage method of high-purity ferrous sulfate solution |
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| JPS59199534A (en) * | 1983-04-25 | 1984-11-12 | Teikoku Kako Kk | Method for purifying ferrous sulfate solution |
| CN1104999A (en) * | 1994-06-01 | 1995-07-12 | 山西省阳泉市磁粉工程筹建处 | Purified technology for ferrous sulfate of titanium white powder by-product |
| CN100396734C (en) * | 2002-12-04 | 2008-06-25 | 中国化工建设总公司常州涂料化工研究院 | Method for producing the yellow pigment of ferric oxide from ferrous sulphate of byproduct abolished by titanium white |
| CN1807262A (en) * | 2006-02-13 | 2006-07-26 | 上海一品颜料有限公司 | Method for preparing ferriferrous oxide black pigment |
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