CN102115209B - Method for producing ferrous nitrate and barium sulfate by using waste acid obtained by producing titanium white by sulfuric acid method - Google Patents
Method for producing ferrous nitrate and barium sulfate by using waste acid obtained by producing titanium white by sulfuric acid method Download PDFInfo
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- CN102115209B CN102115209B CN2010106154734A CN201010615473A CN102115209B CN 102115209 B CN102115209 B CN 102115209B CN 2010106154734 A CN2010106154734 A CN 2010106154734A CN 201010615473 A CN201010615473 A CN 201010615473A CN 102115209 B CN102115209 B CN 102115209B
- Authority
- CN
- China
- Prior art keywords
- ferrous
- nitrate
- sulfuric acid
- barium sulfate
- titanium white
- 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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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002253 acid Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 235000010215 titanium dioxide Nutrition 0.000 title claims abstract description 15
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title claims abstract description 13
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 title claims abstract 16
- 229910002651 NO3 Inorganic materials 0.000 title claims abstract 13
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 title claims abstract 12
- 239000002699 waste material Substances 0.000 title abstract description 4
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 14
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract 4
- 239000002244 precipitate Substances 0.000 claims abstract 4
- 239000000047 product Substances 0.000 claims abstract 4
- 238000001035 drying Methods 0.000 claims abstract 3
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims abstract 3
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims abstract 3
- 238000001816 cooling Methods 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims abstract 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 10
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 10
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 3
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims 3
- 229910001864 baryta Inorganic materials 0.000 claims 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 2
- 238000004821 distillation Methods 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 2
- 229910052717 sulfur Inorganic materials 0.000 claims 2
- 239000011593 sulfur Substances 0.000 claims 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000012535 impurity Substances 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- -1 supersaturated ferrous nitrate Chemical class 0.000 abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract description 2
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 abstract 4
- 239000012295 chemical reaction liquid Substances 0.000 abstract 2
- 239000000706 filtrate Substances 0.000 abstract 2
- 229910052788 barium Inorganic materials 0.000 abstract 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 238000005292 vacuum distillation Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000001038 titanium pigment Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229940095054 ammoniac Drugs 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for producing ferrous nitrate and barium sulfate by using waste acid obtained by producing titanium white by a sulfuric acid method. The method comprises the following steps: mixing the waste acid obtained by producing the titanium white by utilizing the sulfuric acid method with excess ferrous hydroxide for reaction, so as to generate ferrous sulphate; filtering the reaction liquid so as to obtain a filtrate which mainly contains the ferrous sulphate; adding excess barium nitrate to the filtrate which mainly contains the ferrous sulphate for reaction, so that the ferrous nitrate and the barium sulfate are generated, filtering the reaction liquid, and separating out the ferrous nitrate and barium sulfate; washing, drying and smashing barium the sulfate precipitate, so as to obtain the barium sulfate product; and adding less ferrous sulphate to the ferrous nitrate solution for neutralizing the barium nitrate, then feeding into a vacuum distiller for vacuum distillation so as to obtain a supersaturated ferrous nitrate solution, cooling, crystallizing and drying, so as to obtain the ferrous nitrate product.
Description
Technical field
The present invention relates to the comprehensive utilization of Titanium White Production By Sulfuric Acid Process gained spent acid, particularly, relate to the method for producing Iron nitrate and permanent white with Titanium White Production By Sulfuric Acid Process gained spent acid.
Background technology
The main raw material of sulfuric acid method titanium pigment is titanium ore and sulfuric acid, and its reaction principle is:
Fe
2O
3+3H
2SO
4==Fe
2(SO
4)
3+3H
2O;
TiO
2+2H
2SO
4==Ti(SO
4)
2+2H
2O;
Fe+Fe
2(SO
4)
3==3FeSO
4，
PH value of solution is transferred to 5-6, make Ti (SO
4)
2Hydrolysis:
Ti(SO
4)
2+3H
2O==H
2TiO
3↓+2H
2SO
4，
The filtering-depositing heating obtains white titanium pigment:
H
2TiO
3==TiO
2+H
2O
Titanium White Production By Sulfuric Acid Process; Mainly contain sulfuric acid and ferrous sulfate in the spent acid in its production process; Also contain a small amount of metatitanic acid and other metals ions, wherein sulfuric acid content is 18-23%, and ferrous sulfate content is 80g/L (ferrous in anhydrous slufuric acid); Only have a spot of spent acid can return recycling, most of waste material can't directly utilize.
At present, more to the method for comprehensive utilization of Titanium White Production By Sulfuric Acid Process gained spent acid, mainly contain and utilize the reaction of spent acid and iron, generate ferrous sulfate and produce iron pigments such as iron oxide black, iron oxide red with ferrous sulfate; Or, produce sulfate of ammoniac and ferrous sulfate ammonia fertilizer material with in the ammonia and spent acid.
Yet because Titanium White Production By Sulfuric Acid Process gained spent acid output is huge, aforesaid method can not completely consumed, therefore, is necessary to explore the novel method of the spent acid comprehensive regulation of Titanium White Production By Sulfuric Acid Process gained and application.
Summary of the invention
Mainly contain sulfuric acid and ferrous sulfate in the Titanium White Production By Sulfuric Acid Process gained spent acid, also contain a small amount of metatitanic acid and other metals ions, wherein sulfuric acid content is 18-23%; Ferrous sulfate content is 80g/L (ferrous in anhydrous slufuric acid), and for it is fully utilized, the applicant provides the method for producing Iron nitrate and permanent white with Titanium White Production By Sulfuric Acid Process gained spent acid; This method is simple to operate; Facility investment is few, and sulfuric acid and ferrous sulfate recovery utilization rate are high, are worthy of popularization.
Technical scheme of the present invention is following: with the method that Titanium White Production By Sulfuric Acid Process gained spent acid is produced Iron nitrate and permanent white, this method comprises following concrete steps:
Steps A: Titanium White Production By Sulfuric Acid Process gained spent acid is mixed with the excessive hydrogen iron protoxide, make the reaction of sulfuric acid and ferrous hydroxide, generate ferrous sulfate; Filtering reacting liquid obtains main sulfur acid ferrous filtrating, contains the filter residue of a small amount of unreacted ferrous hydroxide and insoluble impurities, and filter residue is buried;
Step B: in the main sulfur acid ferrous filtrating of steps A gained, add excessive nitrate of baryta, stir reaction down, generate Iron nitrate and permanent white, filtering reacting liquid separates barium sulfate precipitate and ferrous nitrate solution; In this step, a small amount of unreacted nitrate of baryta is also in ferrous nitrate solution;
Step C: step B gained barium sulfate precipitate through washing, dry and pulverizing, is obtained the barium sulfate precipitate product;
Step D: with adding in a small amount of ferrous sulfate in the step B gained ferrous nitrate solution and nitrate of baryta, send into then that underpressure distillation is the Iron nitrate supersaturated solution in the underpressure distillation device, crystallisation by cooling, drying obtains the Iron nitrate product.
Method of producing Iron nitrate and permanent white with Titanium White Production By Sulfuric Acid Process gained spent acid according to the invention; The sulfuric acid and the ferrous sulfate that contain in the Titanium White Production By Sulfuric Acid Process gained spent acid have been made full use of; Its step is simple; Facility investment is few, and Iron nitrate and permanent white productive rate are higher, are methods that is worthy of popularization.
Embodiment
Embodiment 1: with the method that Titanium White Production By Sulfuric Acid Process gained spent acid is produced Iron nitrate and permanent white, this method comprises following concrete steps:
Steps A: Titanium White Production By Sulfuric Acid Process gained spent acid is mixed with the excessive hydrogen iron protoxide, make the reaction of sulfuric acid and ferrous hydroxide, generate ferrous sulfate; Filtering reacting liquid obtains main sulfur acid ferrous filtrating, contains the filter residue of a small amount of unreacted ferrous hydroxide and insoluble impurities, and filter residue is buried;
Step B: in the main sulfur acid ferrous filtrating of steps A gained, add excessive nitrate of baryta, stir reaction down, generate Iron nitrate and permanent white, filtering reacting liquid separates barium sulfate precipitate and ferrous nitrate solution; In this step, a small amount of unreacted nitrate of baryta is also in ferrous nitrate solution;
Step C: step B gained barium sulfate precipitate through washing, dry and pulverizing, is obtained the barium sulfate precipitate product;
Step D: with adding in a small amount of ferrous sulfate in the step B gained ferrous nitrate solution and nitrate of baryta, send into then that underpressure distillation is the Iron nitrate supersaturated solution in the underpressure distillation device, crystallisation by cooling, drying obtains the Iron nitrate product.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, under the prerequisite that does not break away from the present invention's design, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be regarded as belonging to the scope of patent protection that the present invention is confirmed by claims of being submitted to.
Claims (1)
1. produce the method for Iron nitrate and permanent white with Titanium White Production By Sulfuric Acid Process gained spent acid, it is characterized in that this method comprises following concrete steps:
Steps A: Titanium White Production By Sulfuric Acid Process gained spent acid is mixed with the excessive hydrogen iron protoxide, make the reaction of sulfuric acid and ferrous hydroxide, generate ferrous sulfate; Filtering reacting liquid obtains main sulfur acid ferrous filtrating, contains the filter residue of a small amount of unreacted ferrous hydroxide and insoluble impurities, and filter residue is buried;
Step B: in the main sulfur acid ferrous filtrating of steps A gained, add excessive nitrate of baryta, stir reaction down, generate Iron nitrate and permanent white, filtering reacting liquid separates barium sulfate precipitate and ferrous nitrate solution; In this step, a small amount of unreacted nitrate of baryta is also in ferrous nitrate solution;
Step C: step B gained barium sulfate precipitate through washing, dry and pulverizing, is obtained the barium sulfate precipitate product;
Step D: with adding in a small amount of ferrous sulfate in the step B gained ferrous nitrate solution and nitrate of baryta, send into then that underpressure distillation is the Iron nitrate supersaturated solution in the underpressure distillation device, crystallisation by cooling, drying obtains the Iron nitrate product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106154734A CN102115209B (en) | 2010-12-31 | 2010-12-31 | Method for producing ferrous nitrate and barium sulfate by using waste acid obtained by producing titanium white by sulfuric acid method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106154734A CN102115209B (en) | 2010-12-31 | 2010-12-31 | Method for producing ferrous nitrate and barium sulfate by using waste acid obtained by producing titanium white by sulfuric acid method |
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| Publication Number | Publication Date |
|---|---|
| CN102115209A CN102115209A (en) | 2011-07-06 |
| CN102115209B true CN102115209B (en) | 2012-08-01 |
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| CN2010106154734A Expired - Fee Related CN102115209B (en) | 2010-12-31 | 2010-12-31 | Method for producing ferrous nitrate and barium sulfate by using waste acid obtained by producing titanium white by sulfuric acid method |
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| CN103663536A (en) * | 2013-09-28 | 2014-03-26 | 赵同甫 | Process for preparing precipitated barium sulfate by pretreatment of waste acid of sulfuric acid process titanium dioxide |
| CN105271310B (en) * | 2015-10-13 | 2017-05-10 | 锦州钛业有限公司 | Chlorination-process titanium-white high-salt wastewater comprehensive utilization method |
| CN118307023B (en) * | 2024-04-08 | 2024-10-18 | 广东尚宸环境科技有限公司 | Method and treatment system for recycling titanium dioxide waste acid by sulfuric acid process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699224A (en) * | 2005-06-29 | 2005-11-23 | 刘世琦 | Comprehensive utilization method of titanium white waste acid |
| CN101289711A (en) * | 2008-05-04 | 2008-10-22 | 谭新乔 | Recycling method of titanium white waste acid in manganese industry |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0676218B2 (en) * | 1988-02-10 | 1994-09-28 | 石原産業株式会社 | Method for producing cobalt-containing ferromagnetic iron oxide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699224A (en) * | 2005-06-29 | 2005-11-23 | 刘世琦 | Comprehensive utilization method of titanium white waste acid |
| CN101289711A (en) * | 2008-05-04 | 2008-10-22 | 谭新乔 | Recycling method of titanium white waste acid in manganese industry |
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| Publication number | Publication date |
|---|---|
| CN102115209A (en) | 2011-07-06 |
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Owner name: SUZHOU DANFANG TEXTILE RESEARCH + DEVELOPMENT CO., Free format text: FORMER OWNER: XIE SHANQING Effective date: 20150104 |
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Free format text: CORRECT: ADDRESS; FROM: 523008 DONGGUAN, GUANGDONG PROVINCE TO: 215228 SUZHOU, JIANGSU PROVINCE |
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Effective date of registration: 20150104 Address after: 215228 Jiangsu City, Wujiang Province, Shengze Town, No. two West Ring Road, No. Shengze Textile Science and Technology Park, building 10, 1188 Patentee after: Suzhou Danfang Textile Research & Development Co., Ltd. Address before: 10, Guangdong, Dongguan province Dongcheng District vortex mountain commercial street, No. 523008, ladder 703 Patentee before: Xie Shanqing |
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Effective date of registration: 20160106 Address after: 215228 Jiangsu City, Wujiang Province, Shengze Town, No. two West Ring Road, No. Shengze Textile Science and Technology Park, building 10, 1188 Patentee after: Wujiang Yisheng Textile Co., Ltd. Address before: 215228 Jiangsu City, Wujiang Province, Shengze Town, No. two West Ring Road, No. Shengze Textile Science and Technology Park, building 10, 1188 Patentee before: Suzhou Danfang Textile Research & Development Co., Ltd. |
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Granted publication date: 20120801 Termination date: 20181231 |
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| CF01 | Termination of patent right due to non-payment of annual fee |