CN103626239A - 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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- CN103626239A CN103626239A CN201310471549.4A CN201310471549A CN103626239A CN 103626239 A CN103626239 A CN 103626239A CN 201310471549 A CN201310471549 A CN 201310471549A CN 103626239 A CN103626239 A CN 103626239A
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- ferrous sulfate
- titanium white
- solution
- demanganization
- 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 44
- 239000011572 manganese Substances 0.000 title claims abstract description 22
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 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
- 239000004408 titanium dioxide Substances 0.000 title abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 235000010215 titanium dioxide Nutrition 0.000 claims description 43
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 26
- 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
- 239000006228 supernatant Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 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
- 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
- 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
- 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
- 230000005611 electricity 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
Landscapes
- Removal Of Specific Substances (AREA)
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, every production 1t titanium dioxide, approximately produces 3 ~ 4tFeSO
47H
2o, annual titanium white by product product ferrous sulfate approximately 3,000,000 t that produce in the whole nation, because it is containing plurality of impurities, can not directly utilize, a part is 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 preparing the starting material Ferrox of lithium ferrous phosphate as anode material of lithium ion battery.The height of Ferrox purity and the size of particle diameter are very large to synthetic LiFePO 4 performance impact, correspondingly higher to the purity requirement of ferrous sulfate.Titanium white by product product ferrous sulfate is carried out to purification processes, be expected to for the raw-material preparation of lithium ion battery industry.Conventional impurity-removing method is mainly ion exchange method, but ion exchange method is not obvious to the removal effect of Mn.
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 electricity industry, demand to lithium cell increases considerably, and 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 to purification processes, prepare cell-grade high purity superfine ferrous oxalate, the heavy demand of supply lithium cell industry, can solve the problem of environmental pollution that ferrous sulfate bulk deposition causes, can meet again lithium cell industry for the demand of Ferrox, 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 ferrous sulfate that purity is higher, 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: titanium white by product ferrous sulfate is dissolved, and carry out a series of in earlier stage processing and obtain ferrous sulfate clear liquid, by ferrous sulfate clear liquid evaporation concentration filtered while hot, again by filtrate crystallisation by cooling, and filter, filter residue is dried, finally obtain the ferrous sulfate solid that purity is higher.Concrete steps comprise as follows:
(1) titanium white by product ferrous sulfate is dissolved in and in water, is modulated into the solution that concentration is 26~41wt%, then according to solid-to-liquid ratio 1.5~2.7:100g/ml, in solution, add iron powder, the pH of regulator solution is 1.5~2.5 again, and under the condition of isolated air, is heated to the temperature insulation 3~5 hours of 70~80 ℃;
(2) in the solution after step (1) insulation, add flocculation agent, after solution layering, isolate supernatant liquid, supernatant liquid is constantly stirred to also ebuillition of heated and be evaporated to below 2/3 of former clear liquid volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally suction filtration being obtained is dried, obtain the ferrous sulfate after demanganization, the clearance of Mn is that 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 manganese content is 0.037~0.092wt%.
The water that dissolves 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 dilute sulphuric acid that the vitriol oil or concentration are 30~50volt%.
Described flocculation agent is that concentration is the polyacrylamide solution of 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 effective 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 be take titanium white by product ferrous sulfate as raw material, through recrystallization, can prepare the ferrous sulfate that purity is higher, and this technical process is short, simple to operate.
(2) the present invention can remove Mn and other each impurity by repeatedly carrying out the operation of 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%, the titanium white by product ferrous sulfate of effectively having purified.Purity is brought up to more than 99%.
(3) the present invention prepares the ferrous sulfate that purity is higher as take titanium white by product ferrous sulfate as raw material, the raw material that can be used for lithium ion battery material, has solved titanium white by product ferrous sulfate and has stacked as waste, abandons, 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 and in water, is modulated into the solution that concentration is 26wt%, then according to solid-to-liquid ratio 2.4:100g/ml, in solution, add iron powder, the pH of the dilute sulphuric acid regulator solution that is 50volt% by concentration is again 2.5, and with the temperature insulation of paraffin sealing post-heating to 70 ℃ 5 hours (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 that 0.00031%, Ni content is 0.0019%; Zn content is 0.0026%; Mg content is 0.87%);
(2) in the solution after step (1) insulation, add the flocculation agent (polyacrylamide solution that concentration is 0.5wt%, the add-on of flocculation agent and the volume ratio of solution are 0.1: 100), after solution layering, isolate supernatant liquid, supernatant liquid is constantly stirred to also ebuillition of heated and be evaporated to 2/3 of former clear liquid volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally suction filtration being obtained is dried, and obtains the ferrous sulfate after demanganization, and 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 and in water, is modulated into the solution that concentration is 41wt%, then according to solid-to-liquid ratio 1.5:100g/ml, in solution, add iron powder, with the pH of vitriol oil regulator solution, be 1.5 again, and the temperature that is heated to 80 ℃ under the condition of isolated air is incubated 3 hours (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 that 85%, Mn content is 0.080%);
(2) in the solution after step (1) insulation, add the flocculation agent (polyacrylamide solution that concentration is 0.4wt%, the add-on of flocculation agent and the volume ratio of solution are 0.05: 100), after solution layering, isolate supernatant liquid, supernatant liquid is constantly stirred to also ebuillition of heated and be evaporated to below 1/3 of former clear liquid volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally suction filtration being obtained is dried, and obtains the ferrous sulfate after demanganization, and 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 and in water, is modulated into the solution that concentration is 30wt%, then according to solid-to-liquid ratio 2.7:100g/ml, in solution, add iron powder, the pH of the dilute sulphuric acid regulator solution that is 40volt% by concentration is again 2, and the temperature that is heated to 78 ℃ under the condition of isolated air is incubated 4 hours (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 that 76%, Mn content is 0.092%);
(2) in the solution after step (1) insulation, add the flocculation agent (polyacrylamide solution that concentration is 0.3wt%, the add-on of flocculation agent and the volume ratio of solution are 0.1: 100), after solution layering, isolate supernatant liquid, supernatant liquid is constantly stirred to also ebuillition of heated and be evaporated to 1/3 of former clear liquid volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally suction filtration being obtained is dried, and obtains the ferrous sulfate after demanganization, and 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 and in water, is modulated into the solution that concentration is 38wt%, then according to solid-to-liquid ratio 2.3:100g/ml, in solution, add iron powder, the pH of the dilute sulphuric acid regulator solution that is 30volt% by concentration is again 2.2, and the temperature that is heated to 76 ℃ under the condition of isolated air is incubated 3.6 hours (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 that 76%, Mn content is 0.092%);
(2) in the solution after step (1) insulation, add the flocculation agent (polyacrylamide solution that concentration is 0.5wt%, the add-on of flocculation agent and the volume ratio of solution are 0.2: 100), after solution layering, isolate supernatant liquid, supernatant liquid is constantly stirred to also ebuillition of heated and be evaporated to 1/4 of former clear liquid volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally suction filtration being obtained is dried, and obtains the ferrous sulfate after demanganization, and 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 possessing those of ordinary skills, can also under the prerequisite that does not depart from aim of the present invention, makes various variations.
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 and in water, is modulated into the solution that concentration is 26~41wt%, then according to solid-to-liquid ratio 1.5~2.7:100g/ml, in solution, add iron powder, the pH of regulator solution is 1.5~2.5 again, and under the condition of isolated air, is heated to the temperature insulation 3~5 hours of 70~80 ℃;
(2) in the solution after step (1) insulation, add flocculation agent, after solution layering, isolate supernatant liquid, supernatant liquid is constantly stirred to also ebuillition of heated and be evaporated to below 2/3 of former clear liquid volume, again by suction filtration after filtrate crystallisation by cooling, the crystallisate finally suction filtration being obtained is dried, and 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 manganese 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 dilute sulphuric acid that the vitriol oil or concentration are 30~50volt%.
4. the method for titanium white by product ferrous sulfate demanganization according to claim 1, is characterized in that: described flocculation agent is that concentration is the polyacrylamide solution of 0.3~0.5wt%.
5. according to the method for the titanium white by product ferrous sulfate demanganization described in claim 1 or 4, it 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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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN113816354A (en) * | 2021-11-04 | 2021-12-21 | 四川省盈达锂电新材料有限公司 | Method for preparing iron phosphate by using wastes 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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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN113816354A (en) * | 2021-11-04 | 2021-12-21 | 四川省盈达锂电新材料有限公司 | Method for preparing iron phosphate by using wastes 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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