CN101767837A - Method for removing titanium in ferrous sulfate as titanium dioxide byproduct - Google Patents
Method for removing titanium in ferrous sulfate as titanium dioxide byproduct Download PDFInfo
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- CN101767837A CN101767837A CN201010046570A CN201010046570A CN101767837A CN 101767837 A CN101767837 A CN 101767837A CN 201010046570 A CN201010046570 A CN 201010046570A CN 201010046570 A CN201010046570 A CN 201010046570A CN 101767837 A CN101767837 A CN 101767837A
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- China
- Prior art keywords
- titanium
- ferrous sulfate
- titanium dioxide
- byproduct
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910000359 iron(II) sulfate Inorganic materials 0.000 title claims abstract description 32
- 235000003891 ferrous sulphate Nutrition 0.000 title claims abstract description 29
- 239000011790 ferrous sulphate Substances 0.000 title claims abstract description 29
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 25
- 239000010936 titanium Substances 0.000 title claims abstract description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 22
- 239000006227 byproduct Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 16
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 title claims abstract 10
- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- 239000012065 filter cake Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000002893 slag Substances 0.000 claims abstract description 4
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 4
- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 4
- 239000002244 precipitate Substances 0.000 abstract 2
- 239000008394 flocculating agent Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 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 description 24
- 238000004519 manufacturing process Methods 0.000 description 10
- 230000007062 hydrolysis Effects 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001034 iron oxide pigment Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a method for removing titanium in titanium dioxide by-product ferrous sulfate, which comprises the steps of mixing and stirring the titanium dioxide by-product ferrous sulfate and water according to the weight part ratio of 1: 1-2, heating and dissolving, then carrying out hydrolysis reaction for 1-2 hours at 78-80 ℃ to generate titanium hydroxide precipitate, adding a flocculating agent for stirring to enable suspended small particles to generate large-particle precipitate, and then carrying out filter pressing to obtain filter cake titanium white powder slag as a raw material for producing titanium dioxide; and cooling, crystallizing and filtering the filtrate to obtain the ferrous sulfate and clear liquid after titanium removal. The method effectively removes the titanium in the ferrous sulfate serving as the byproduct of the titanium dioxide, and the titanium content in the ferrous sulfate after titanium removal is less than 100 ppm.
Description
Technical field
The present invention relates to the titanium dioxide manufacture field, specifically is the removing method of titanium in a kind of byproduct ferrous sulfate of titanium dioxide.
Background technology
Surplus the domestic titanium dioxide output about 100 in 2007 ten thousand tons, have 60 many enterprises, at present China's titanium white powder industry is in production capacity expansionary phase, the national according to statistics titanium dioxide project that is in different stepss such as project verification, declaration, design, construction also has 25, newly-increased aggregated capacity is about 1,280,000 tons/year, as can both realize on schedule, will reach above the U.S. to China's titanium white powder throughput in 2010 and produce 2500000 tons per year, become the big producing country of the first in the world.
But what do not match with throughput is the titanium white production technology that China falls behind, the chloride process titanium dioxide powder accounts for 60% of ultimate production in the world at present, and China only has and climbs bright and beautiful titanium and already produce 1.5 ten thousand tons chlorination process production equipment per year, all the other all are the Production By Sulfuric Acid Process technology, the ferrous sulfate of 1 ton of about by-product 3-4 of titanium dioxide of every production ton, the whole nation year produces 3,000,000 tons ferrous sulfate approximately, as not fully utilized, not only pollutes the environment but also causes the waste of iron resources.
The research that just this is fully utilized as far back as China's researcher in 2002, the by-product ferrous sulfate during that successively will produce titanium dioxide is used for water purification agent, produces bodied ferric sulfate, produces iron oxide pigment, but because " impurity " the particularly existence of titanium in the ferrous sulfate influences its use.
Summary of the invention
The invention provides the removing method of titanium in a kind of byproduct ferrous sulfate of titanium dioxide; have raw material applied widely, purify thoroughly, energy consumption is low, free from environmental pollution, production control reliable and be convenient to mass-producing quantity-produced characteristics, the ferrous sulfate of being produced can satisfy the production requirement of high-quality iron oxide pigment.
Technical scheme of the present invention is:
The removing method of titanium in a kind of byproduct ferrous sulfate of titanium dioxide, it is characterized in that: be with byproduct ferrous sulfate of titanium dioxide and water by 1: the weight part ratio of 1-2 mixes stirring, heating for dissolving, generated the titanium hydroxide precipitation then at 78-80 ℃ of following hydrolysis reaction 1-2 hour, adding flocculation agent stirs, make the suspension small-particle generate the macrobead precipitation, get filter cake titanium white granulated slag through press filtration then, as the raw material of producing titanium dioxide; Ferrous sulfate and the clarified liq of filtrate after crystallisation by cooling, suction filtration obtain removing titanium.
The removing method of titanium in the described byproduct ferrous sulfate of titanium dioxide is characterized in that: described flocculation agent is selected Tai-Ace S 150, poly-iron chloride or polysilicate sulfuric acid aluminium for use; Described clarified liq recycle is dissolved in the raw material sulphuric acid ferrous.
Hydrolysis equation of the present invention: TiOSO
4+ 3H
2O=Ti (OH)
4↓+H
2SO
4
The present invention can effectively remove the titanium in the raw material byproduct ferrous sulfate of titanium dioxide, removes titanium content in the ferrous sulfate behind the titanium less than 100ppm, and method is feasible, effective, and production cost is low, be convenient to large-scale production.
Component list except that the ferrous sulfate behind the titanium:
| Sequence number | Title | Component content % | Target value |
| ??1 | ??FeSO 47H 2O | ??90.0 | |
| ??2 | ??Fe 2(SO 4) 3 | ??1.0 | |
| ??3 | ??TiO(SO 4) | ??0.6 | Less than 100ppm |
| ??4 | Free-water | ??6.0 | |
| ??5 | Other | ??2.4 |
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Specific implementation method
1, raw material sulphuric acid ferrous dissolving:
In 10 cubic metres reactive tank byproduct ferrous sulfate of titanium dioxide and water or the copperas solution that recycles are mixed stirring between by 1: 1.5, heating makes ferrous sulfate dissolve the saturated copperas solution of system fully;
2, hydrolysis:
The copperas solution that dissolving is good is with steam heating and be warming up to 70-80 ℃, keeps this temperature 1-2 hour, allows its abundant hydrolysis; 3, filtering separation:
After the abundant hydrolysis of copperas solution, add precipitation agent and stir, make the suspension small-particle generate the macrobead precipitation, see have obvious macrobead to generate after, solution is filtered through pressure filter with pump delivery, and filter cake is the titanium white granulated slag, can be used as after the discharging packing and produces the titanium dioxide raw material; Clarifying filtrate is delivered to crystallizer tank;
4, crystallisation by cooling:
Saturated copperas solution is through cooling in crystallizer tank, the ferrous sulfate crystallization is separated out, and slip takes off ferrous sulfate behind the titanium and filtrate after the automatic centrifugal separating machine separates, the filtrate cycle utilization is used for the dissolving of raw material sulphuric acid ferrous, and solid sulphuric acid is ferrous to be finished product after packing.
Claims (2)
1. the removing method of titanium in the byproduct ferrous sulfate of titanium dioxide, it is characterized in that: be with byproduct ferrous sulfate of titanium dioxide and water by 1: the weight part ratio of 1-2 mixes stirring, heating for dissolving, generated the titanium hydroxide precipitation then at 78-80 ℃ of following hydrolysis reaction 1-2 hour, adding flocculation agent stirs, make the suspension small-particle generate the macrobead precipitation, get filter cake titanium white granulated slag through press filtration then, as the raw material of producing titanium dioxide; Ferrous sulfate and the clarified liq of filtrate after crystallisation by cooling, suction filtration obtain removing titanium.
2. the removing method of titanium in the byproduct ferrous sulfate of titanium dioxide according to claim 1 is characterized in that: described flocculation agent is selected Tai-Ace S 150, poly-iron chloride or polysilicate sulfuric acid aluminium for use; Described clarified liq recycle is dissolved in the raw material sulphuric acid ferrous.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010046570A CN101767837A (en) | 2010-01-20 | 2010-01-20 | Method for removing titanium in ferrous sulfate as titanium dioxide byproduct |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010046570A CN101767837A (en) | 2010-01-20 | 2010-01-20 | Method for removing titanium in ferrous sulfate as titanium dioxide byproduct |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101767837A true CN101767837A (en) | 2010-07-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010046570A Pending CN101767837A (en) | 2010-01-20 | 2010-01-20 | Method for removing titanium in ferrous sulfate as titanium dioxide byproduct |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101767837A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746082A (en) * | 2017-11-15 | 2018-03-02 | 攀钢集团攀枝花钢铁研究院有限公司 | The quick minimizing technology of titanium in byproduct ferrous sulfate of titanium dioxide |
| CN111055602A (en) * | 2019-12-31 | 2020-04-24 | 安徽省粤隆印刷科技有限公司 | Environment-friendly printing process with low migration volume |
| CN116239145A (en) * | 2023-03-24 | 2023-06-09 | 甘肃佰利联化学有限公司 | Method for co-production and recovery of titanium by iron phosphate-titanium |
-
2010
- 2010-01-20 CN CN201010046570A patent/CN101767837A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746082A (en) * | 2017-11-15 | 2018-03-02 | 攀钢集团攀枝花钢铁研究院有限公司 | The quick minimizing technology of titanium in byproduct ferrous sulfate of titanium dioxide |
| CN111055602A (en) * | 2019-12-31 | 2020-04-24 | 安徽省粤隆印刷科技有限公司 | Environment-friendly printing process with low migration volume |
| CN111055602B (en) * | 2019-12-31 | 2021-09-10 | 安徽省粤隆印刷科技有限公司 | Environment-friendly printing process with low migration volume |
| CN116239145A (en) * | 2023-03-24 | 2023-06-09 | 甘肃佰利联化学有限公司 | Method for co-production and recovery of titanium by iron phosphate-titanium |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100707 |