CN102660674A - Method for using titanium white waste acid to treat phosphorus in sulfurous iron ore - Google Patents
Method for using titanium white waste acid to treat phosphorus in sulfurous iron ore Download PDFInfo
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- CN102660674A CN102660674A CN2012101277309A CN201210127730A CN102660674A CN 102660674 A CN102660674 A CN 102660674A CN 2012101277309 A CN2012101277309 A CN 2012101277309A CN 201210127730 A CN201210127730 A CN 201210127730A CN 102660674 A CN102660674 A CN 102660674A
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- CN
- China
- Prior art keywords
- waste acid
- titanium white
- phosphorus
- pyrite cinder
- acid solution
- 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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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000002699 waste material Substances 0.000 title claims abstract description 49
- 239000002253 acid Substances 0.000 title claims abstract description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 235000010215 titanium dioxide Nutrition 0.000 title claims abstract description 37
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 36
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000011574 phosphorus Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 24
- 239000003818 cinder Substances 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 7
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims description 52
- 229910052683 pyrite Inorganic materials 0.000 claims description 52
- 239000011028 pyrite Substances 0.000 claims description 52
- 239000002893 slag Substances 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 3
- 239000001038 titanium pigment Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 230000002860 competitive effect Effects 0.000 abstract 1
- 239000004408 titanium dioxide Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 238000004064 recycling Methods 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The method discloses a method for using titanium white waste acid to treat phosphorus in sulfurous iron ore. Waste acid solution and sulfurous iron ore cinders, produced during the production process of titanium dioxide, are subject to stir treatment for 0.5 to 1.0 hours under the room temperature, and are subject to solid-liquid separation, after filter cinders are washed, low-phosphorous sulfurous iron ore cinders with phosphorus of which the content is lower than 0.03% is obtained, and the dephosphorization rate reaches above 92%. The method has the characteristics of simple treatment process, short treatment time, easiness in operation, high dephosphorization rate, reasonable resource utilization, simple equipment, low production cost and excellent dephosphorization performance, thereby having strong market competitive power and popularization and application value.
Description
Technical field
The present invention relates to a kind of method of utilizing titanium white waste acid to handle phosphorus in the sulfurous iron ore, belong to the research field of solid in the chemical industry, liquid debris utilization.
Background technology
China's ferro-sulphur ore is abundant, almost spreads all over national each province, and more than 40 hundred million tons of reserves are at the forefront in the world.Pyrite cinder is called sulfate slag again, is the waste residue that discharge when being raw material calcining production sulfuric acid in the chemical plant with the sulfurous iron ore.
Produce 0.8～1.0 ton by 1 ton of sulfuric acid of every production in the industry and burn slag; Iron level is generally 40～60% in the pyrite cinder; Also contain valuable elements such as a spot of Cu, Ag, Au simultaneously; Be a kind of secondary resource of preciousness, at present, pyrite cinder is mainly used in produces iron ore concentrate, iron pigment, molysite, water purification agent etc.Along with the high speed development of China's steel industry, the degree of dependence of imported iron ore stone is strengthened gradually, so pyrite cinder is used for steel industry, can partly alleviate the iron ore disparities between supply and demand.But since in the ironmaking production industry to fair Fe>=60%, P≤0.13% of requiring of the smart powder of raw material iron.
During Titanium White Production By Sulfuric Acid Process (titanium oxide), white titanium pigment per ton will produce 8～10 tons of sulfur waste acid (17%～22%H
2SO
4) solution, traditional treatment process is to adopt the lime neutralization or it is concentrated the back retrieval system to use, processing cost is high.
Utilization research major part for pyrite cinder focuses on how to improve the pyrite cinder iron-holder with in the research of producing qualified iron ore concentrate at present; And obtained good effect; But because the sulphur ore burns the harmful element phosphorus that contains in the slag; Adopt conventional mechanical beneficiation method and physical method dephosphorization to become impossible, seriously influence its application as iron-smelting raw material.According to the correlative study report, can remove part phosphorus when adopting magnetic separation, flotation, acidleach, mikrobe leaching etc. that pyrite cinder is carried out desulfurization, dearsenification, but the dephosphorization precision is not high.Adopt the research report of which kind of method dephosphorization when yet there are no about pyrite cinder as iron-smelting raw material.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing phosphorus in the titanium white waste acid solution-treated pyrite cinder; This method is utilized harmful element phosphorus in the waste sulfuric acid solution effective elimination pyrite cinder that produces in the industrial titanium white production, to satisfy pyrite cinder as the specification of quality of iron-smelting raw material to phosphorus; This is a kind of operational path that utilizes trade waste pyrite cinder and spent acid to be used to produce the metallurgical raw material with higher-value, reaches utilization of waste material, realizes recycling economy, energy-saving and emission-reduction purpose.
The present invention realizes the object of the invention through following technical scheme: be 7～12% titanium white waste acid solution with mass percent concentration; The ratio that in solid-to-liquid ratio is 1:1.0～1.5 adds in the pyrite cinder under the agitation condition of room temperature, 250～350rpm; Stirring reaction 0.5～1.0h; After solid-liquid separation, filter residue is washed with water to PH=5～6, promptly gets phosphorus content after the drying less than 0.03% low-phosphorous pyrite cinder.
Titanium white waste acid liquid is the waste sulfuric acid solution that produces in the production process of titanium pigment among the present invention, and its sulfuric acid concentration is 15%～25%.
Pyrite cinder upward is the solid slag that raw material is produced when fluidized bed roasting is produced sulfuric acid with the sulfurous iron ore for industry among the present invention, and its iron level is more than 55%, and phosphorus content is greater than 0.4%, and wherein granularity is that 100 purposes burning slag accounts for 75～90% of total burning slag amount.
After filtered liq after the solid-liquid separation uses titanium white waste acid solution adjusting concentration to mass percent concentration to be 7～12%; Circulation is used to handle pyrite cinder as reaction solution; Experiment proved response liquid recycles 19 times, still can make in the pyrite cinder after the processing phosphorus content less than 0.03%.
Washing process can adopt syllogic countercurrent washing mode to wash filter residue, and dense washing lotion part is used as the preparation reaction solution, and remainder neutralizes with lime, and the clarification back recycles and qualified discharge as the washing clear liquid.
Phosphorus content not only can satisfy iron-smelting raw material to its content requirement in the pyrite cinder after the present invention handles; The sulfur waste acid of adopting Titanium White Production By Sulfuric Acid Process to produce is simultaneously handled; Reduced useless vitriolic processing costs, concerning sulphur iron burns slag and sulfur waste acid, can turn waste into wealth, economized on resources; Reduce environmental pollution, realize the comprehensive utilization of resource.The technological process that the inventive method adopts is simple, and mild condition is easy to operate, and the treatment time is short; The phosphorus decreasing ratio is high, and dephosphorization rate reaches more than 92%, and use equipment is simple; Processing cost is low, is easy to realize suitability for industrialized production, has very strong market competition ability and application value.
Embodiment
Through embodiment the present invention is done further explain below, but protection domain of the present invention is not limited to said content, like no specified otherwise, percentage concentration is a mass percent concentration among the embodiment.
Embodiment 1: this utilizes the method for phosphorus in the titanium white waste acid solution-treated pyrite cinder, and particular content is following:
The titanium white waste acid Solution H of using in the present embodiment
2SO
4Content is 19.35%, and outward appearance is blackish green; The pyrite cinder outward appearance is a brown, and raw material slag iron level is 56.18%, and phosphorus content is 0.43%, and granularity is that 100 purposes burning slag accounts for 75% of total burning slag amount.
Titanium white waste acid solution 150 grams with concentration adjustment to 7.0%; Under the agitation condition of room temperature, 250rpm, add in the 100 gram pyrite cinders; Stirring reaction 1.0h, after solid-liquid separation, filter residue is washed with water between PH=5～6; Through 100 ℃ of dry 30min, take out cooling and promptly get low-phosphorous pyrite cinder then; This sample contains Fe 59.72% through analyzing, P0.029%, and outward appearance is a red-brown.
Embodiment 2: this utilizes the method for phosphorus in the titanium white waste acid solution-treated pyrite cinder, and particular content is following:
The pyrite cinder outward appearance of using in the present embodiment is brown, and raw material slag iron level is 57.2%, and phosphorus content is 0.46%, and granularity is that 100 purposes burning slag accounts for 80% of total burning slag amount.
Mother liquor after filtering among the embodiment 1 is added titanium white waste acid and is regulated acid concentration to 8.7%; Getting 150 gram waste acid liquors adds under the agitation condition of room temperature, 250rpm in the 100 gram pyrite cinders; Stirring reaction 1.0h after-filtration; Filter residue is washed with water between PH=5～6, then through 100 ℃ of dry 30min, takes out cooling and promptly gets low-phosphorous pyrite cinder; This sample contains Fe 58.94% through analyzing, and P 0.021%, and outward appearance is a red-brown.
Embodiment 3: this utilizes the method for phosphorus in the titanium white waste acid solution-treated pyrite cinder, and particular content is following:
The titanium white waste acid solution that uses in the present embodiment is the filtrated stock that recycles after 5 times; The pyrite cinder outward appearance is a brown, and raw material slag iron level is 58.17%, and phosphorus content is 0.51%, and granularity is that 100 purposes burning slag accounts for 90% of total burning slag amount.
Filtrated stock after recycling for 5 times is regulated concentration to 10.6% through adding titanium white waste acid; Getting 150 gram waste acid liquors adds under the agitation condition of room temperature, 300rpm in the 100 gram pyrite cinders; Stirring reaction 0.5h after-filtration; Filter residue adopts the syllogic countercurrent washing to PH=5～6, then through 100 ℃ of dry 30min, takes out cooling and promptly gets low-phosphorous pyrite cinder; This sample contains Fe 59.18% through analyzing, and P 0.026%, and outward appearance is a red-brown.
Embodiment 4: this utilizes the method for phosphorus in the titanium white waste acid solution-treated pyrite cinder, and particular content is following:
The titanium white waste acid solution that uses in the present embodiment is the filtrated stock that recycles after 10 times; The pyrite cinder outward appearance is a brown, and raw material slag iron level is 56.18%, and phosphorus content is 0.43%, and granularity is that 100 purposes burning slag accounts for 85% of total burning slag amount.
Filtrated stock after recycling for 10 times is regulated acid concentration to 12% through adding titanium white waste acid; Getting 150 gram waste acid liquors adds under the agitation condition of room temperature, 300rpm in the 100 gram pyrite cinders; Stirring reaction 0.5h after-filtration; Filter residue is washed with water between PH=5～6, then through 100 ℃ of dry 30min, takes out cooling and promptly gets low-phosphorous pyrite cinder; This sample contains Fe 57.38% through analyzing, and P 0.019%, and outward appearance is a red-brown.
Embodiment 5: this utilizes the method for phosphorus in the titanium white waste acid solution-treated pyrite cinder, and particular content is following:
The titanium white waste acid solution that uses in the present embodiment is the filtrated stock that recycles after 15 times; The pyrite cinder outward appearance is a brown, and raw material slag iron level is 56.18%, and phosphorus content is 0.43%, and granularity is that 100 purposes burning slag accounts for 75% of total burning slag amount.
Filtrated stock after recycling for 15 times is added titanium white waste acid and is regulated acid concentration to 9.1%; Getting 120 gram waste acid liquors adds under the agitation condition of room temperature, 350rpm in pyrite cinder 100 grams; Stirring reaction 0.5h after-filtration; Filter residue is washed with water between PH=5～6, then through 100 ℃ of dry 30min, takes out cooling and promptly gets low-phosphorous pyrite cinder; This sample contains Fe 58.16% through analyzing, and P 0.021%, and outward appearance is a red-brown.
Embodiment 6: this utilizes the method for phosphorus in the titanium white waste acid solution-treated pyrite cinder, and particular content is following:
The titanium white waste acid solution that uses in the present embodiment is the filtrated stock that recycles after 19 times; The pyrite cinder outward appearance is a brown, and raw material slag iron level is 56.18%, and phosphorus content is 0.43%, and granularity is that 100 purposes burning slag accounts for 75% of total burning slag amount.
Filtrated stock after recycling for 19 times is added titanium white waste acid and is regulated acid concentration to 8.2%; Getting 100 gram waste acid liquors adds under the agitation condition of room temperature, 350rpm in pyrite cinder 100 grams; Stirring reaction 0.7h after-filtration; Filter residue is washed with water between PH=5～6, then through 100 ℃ of dry 30min, takes out cooling and promptly gets low-phosphorous pyrite cinder; This sample contains Fe 59.37% through analyzing, and P 0.026%, and outward appearance is a red-brown.
Through embodiment 1-6, the result shows that mother liquor after the solid-liquid separation after adding spent acid and regulating concentration to 7～12%, still can be used as reaction solution and recycles, and in the pyrite cinder after handling phosphorus content all less than 0.03%.
Claims (5)
1. method of utilizing phosphorus in the titanium white waste acid solution-treated pyrite cinder; It is characterized in that: be 7～12% titanium white waste acid solution with mass percent concentration; The ratio that in solid-to-liquid ratio is 1:1.0～1.5 adds in the pyrite cinder under the agitation condition of room temperature, 250～350rpm, and stirring reaction 0.5～1.0h is after solid-liquid separation; Filter residue is washed with water to PH=5～6, promptly gets phosphorus content after the drying less than 0.03% low-phosphorous pyrite cinder.
2. require the method for phosphorus in the 1 described titanium white waste acid solution-treated pyrite cinder according to claim, it is characterized in that: titanium white waste acid liquid is the waste sulfuric acid solution that produces in the production process of titanium pigment, and its sulfuric acid concentration is 15%～25%.
3. require the method for phosphorus in the 1 described titanium white waste acid solution-treated pyrite cinder according to claim; It is characterized in that: it is the solid slag that raw material is produced when fluidized bed roasting is produced sulfuric acid that pyrite cinder is gone up with the sulfurous iron ore for industry; Its iron level is more than 55%; Phosphorus content is greater than 0.4%, and wherein granularity is that 100 purposes burning slag accounts for 75～90% of total burning slag amount.
4. require the method for phosphorus in the 1 described titanium white waste acid solution-treated pyrite cinder according to claim; It is characterized in that: after the filtered liq after the solid-liquid separation used titanium white waste acid solution adjusting concentration to mass percent concentration to be 7～12%, circulation was used to handle pyrite cinder.
5. require the method for phosphorus in the 1 described titanium white waste acid solution-treated pyrite cinder according to claim, it is characterized in that: filter residue adopts syllogic countercurrent washing mode to wash.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101277309A CN102660674A (en) | 2012-04-27 | 2012-04-27 | Method for using titanium white waste acid to treat phosphorus in sulfurous iron ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101277309A CN102660674A (en) | 2012-04-27 | 2012-04-27 | Method for using titanium white waste acid to treat phosphorus in sulfurous iron ore |
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| Publication Number | Publication Date |
|---|---|
| CN102660674A true CN102660674A (en) | 2012-09-12 |
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|---|---|---|---|
| CN2012101277309A Pending CN102660674A (en) | 2012-04-27 | 2012-04-27 | Method for using titanium white waste acid to treat phosphorus in sulfurous iron ore |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471959A (en) * | 2021-12-20 | 2022-05-13 | 中南大学 | Method for improving ilmenite flotation by using titanium dioxide waste liquid |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1115949A (en) * | 1965-12-28 | 1968-06-06 | Foraco Y Proyectos S A | Method and means for removing the phosphorous out of iron ore |
| GB1150325A (en) * | 1965-12-28 | 1969-04-30 | Foraco Y Proyectos Sa | Method and Means for Removing Phosphorus Out of Iron Ore. |
| JPS5767136A (en) * | 1980-10-09 | 1982-04-23 | Sumitomo Metal Ind Ltd | Dephosphorizing method for ore |
| SE8103114L (en) * | 1981-05-18 | 1982-11-19 | Ingmar Grenthe | PROCEDURE FOR EXTRACTION OF ORAL PHOSPHORUS |
| CN101618365A (en) * | 2009-07-24 | 2010-01-06 | 昭通天元实业有限责任公司 | Processing method for removing phosphorus and arsenic in pyrite cinder |
| CN102168174A (en) * | 2011-04-07 | 2011-08-31 | 中国地质大学（武汉） | Method for dephosphorizing high-phosphorus hematite |
-
2012
- 2012-04-27 CN CN2012101277309A patent/CN102660674A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1115949A (en) * | 1965-12-28 | 1968-06-06 | Foraco Y Proyectos S A | Method and means for removing the phosphorous out of iron ore |
| GB1150325A (en) * | 1965-12-28 | 1969-04-30 | Foraco Y Proyectos Sa | Method and Means for Removing Phosphorus Out of Iron Ore. |
| JPS5767136A (en) * | 1980-10-09 | 1982-04-23 | Sumitomo Metal Ind Ltd | Dephosphorizing method for ore |
| SE8103114L (en) * | 1981-05-18 | 1982-11-19 | Ingmar Grenthe | PROCEDURE FOR EXTRACTION OF ORAL PHOSPHORUS |
| CN101618365A (en) * | 2009-07-24 | 2010-01-06 | 昭通天元实业有限责任公司 | Processing method for removing phosphorus and arsenic in pyrite cinder |
| CN102168174A (en) * | 2011-04-07 | 2011-08-31 | 中国地质大学（武汉） | Method for dephosphorizing high-phosphorus hematite |
Non-Patent Citations (1)
| Title |
|---|
| 舒均杰: "从钛白废酸和硫铁矿烧渣制备饲料级硫酸亚铁", 《化学工程师》, vol. 157, no. 10, 30 October 2008 (2008-10-30), pages 54 - 56 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471959A (en) * | 2021-12-20 | 2022-05-13 | 中南大学 | Method for improving ilmenite flotation by using titanium dioxide waste liquid |
| CN114471959B (en) * | 2021-12-20 | 2024-05-24 | 中南大学 | Method for improving ilmenite floatation by utilizing titanium white waste liquid |
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Application publication date: 20120912 |