CN102115209A - Method for producing ferrous nitrate and barium sulfate from waste acid obtained by producing titanium dioxide by sulfuric acid method - Google Patents
Method for producing ferrous nitrate and barium sulfate from waste acid obtained by producing titanium dioxide by sulfuric acid method Download PDFInfo
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- CN102115209A CN102115209A CN 201010615473 CN201010615473A CN102115209A CN 102115209 A CN102115209 A CN 102115209A CN 201010615473 CN201010615473 CN 201010615473 CN 201010615473 A CN201010615473 A CN 201010615473A CN 102115209 A CN102115209 A CN 102115209A
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- ferrous
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- barium sulfate
- sulfuric acid
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 53
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 title claims abstract description 46
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000002253 acid Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 24
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910002651 NO3 Inorganic materials 0.000 title claims abstract description 22
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 239000002699 waste material Substances 0.000 title abstract description 18
- 239000004408 titanium dioxide Substances 0.000 title abstract description 16
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 21
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 21
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims abstract description 9
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000002244 precipitate Substances 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract 4
- 239000003513 alkali Substances 0.000 claims abstract 2
- 238000001816 cooling Methods 0.000 claims abstract 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims 4
- 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
- 239000007788 liquid Substances 0.000 claims 2
- 229910052717 sulfur Inorganic materials 0.000 claims 2
- 239000011593 sulfur Substances 0.000 claims 2
- 235000010215 titanium dioxide Nutrition 0.000 claims 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 238000004821 distillation 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
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 abstract description 12
- 239000004277 Ferrous carbonate Substances 0.000 abstract 1
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 abstract 1
- 235000019268 ferrous carbonate Nutrition 0.000 abstract 1
- 229960004652 ferrous carbonate Drugs 0.000 abstract 1
- 229910000015 iron(II) carbonate Inorganic materials 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 229910011006 Ti(SO4)2 Inorganic materials 0.000 description 3
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 description 3
- 229910003890 H2TiO3 Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- CZSABVBCTRZESY-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].OS(O)(=O)=O Chemical compound [O-2].[O-2].[Ti+4].OS(O)(=O)=O CZSABVBCTRZESY-UHFFFAOYSA-N 0.000 description 1
- 229940010514 ammonium ferrous sulfate Drugs 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 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
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 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
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
技术领域technical field
本发明涉及硫酸法生产钛白粉所得废酸的综合利用，具体地，涉及用硫酸法生产钛白粉所得废酸生产硝酸亚铁和硫酸钡的方法。The invention relates to the comprehensive utilization of waste acid obtained by sulfuric acid production of titanium dioxide, in particular to a method for producing ferrous nitrate and barium sulfate from the waste acid obtained by sulfuric acid production of titanium dioxide.
背景技术Background technique
硫酸法钛白粉的主要原料是钛矿和硫酸，其反应原理为：The main raw materials of sulfuric acid titanium dioxide are titanium ore and sulfuric acid, and the reaction principle is as follows:
Fe2O3+3H2SO4==Fe2(SO4)3+3H2O;Fe2O3+3H2SO4==Fe2(SO4)3+3H2O;
TiO2+2H2SO4==Ti(SO4)2+2H2O;TiO2+2H2SO4==Ti(SO4)2+2H2O;
Fe+Fe2(SO4)3==3FeSO4，Fe+Fe2(SO4)3==3FeSO4,
将溶液pH调至5-6，使Ti(SO4)2水解：Adjust the pH of the solution to 5-6 to hydrolyze Ti(SO4)2:
Ti(SO4)2+3H2O==H2TiO3↓+2H2SO4，Ti(SO4)2+3H2O==H2TiO3↓+2H2SO4,
过滤沉淀 加热得到钛白粉：Filter the precipitate and heat to obtain titanium dioxide:
H2TiO3==TiO2+H2OH2TiO3==TiO2+H2O
硫酸法生产钛白粉，其生产过程中的废酸中主要含有硫酸和硫酸亚铁，也含有少量偏钛酸和其他金属离子，其中硫酸含量为18-23%，硫酸亚铁含量为80g/L（以无水硫酸亚铁计），仅有少量的废酸可以返回重复利用，大部分废料无法直接利用。Titanium dioxide is produced by sulfuric acid method. The waste acid in the production process mainly contains sulfuric acid and ferrous sulfate, and also contains a small amount of metatitanic acid and other metal ions. The content of sulfuric acid is 18-23%, and the content of ferrous sulfate is 80g/L (calculated as anhydrous ferrous sulfate), only a small amount of waste acid can be returned for reuse, and most of the waste cannot be used directly.
目前，针对硫酸法生产钛白粉所得废酸的综合利用方法较多，主要有利用废酸与铁反应，生成硫酸亚铁、并用硫酸亚铁生产氧化铁黑、铁红等铁系颜料；或用氨中和废酸，生产硫酸氨和硫酸亚铁氨肥料。At present, there are many comprehensive utilization methods for the waste acid obtained from the production of titanium dioxide by the sulfuric acid method, mainly using the waste acid to react with iron to generate ferrous sulfate, and using ferrous sulfate to produce iron pigments such as iron oxide black and iron red; Ammonia neutralizes spent acid to produce ammonium sulfate and ferrous sulfate ammonia fertilizers.
然而，由于硫酸法生产钛白粉所得废酸产量巨大，上述方法并不能完全消耗，因此，有必要探索硫酸法生产钛白粉所得废酸综合治理和应用的新方法。However, due to the huge amount of waste acid produced by sulfuric acid production of titanium dioxide, the above methods cannot be completely consumed. Therefore, it is necessary to explore new methods for comprehensive treatment and application of waste acid obtained by sulfuric acid production of titanium dioxide.
发明内容Contents of the invention
硫酸法生产钛白粉所得废酸中主要含有硫酸和硫酸亚铁，也含有少量偏钛酸和其他金属离子，其中硫酸含量为18-23%，硫酸亚铁含量为80g/L（以无水硫酸亚铁计），为了对其综合利用，本申请人提供了用硫酸法生产钛白粉所得废酸生产硝酸亚铁和硫酸钡的方法，该方法操作简单，设备投资少，硫酸和硫酸亚铁回收利用率高，值得推广应用。The waste acid obtained from sulfuric acid production of titanium dioxide mainly contains sulfuric acid and ferrous sulfate, and also contains a small amount of metatitanic acid and other metal ions. The content of sulfuric acid is 18-23%, and the content of ferrous sulfate is 80g/L (as anhydrous sulfuric acid Ferrous meter), in order to its comprehensive utilization, the applicant has provided the method for producing ferrous nitrate and barium sulfate with the waste acid gained from producing titanium dioxide by the sulfuric acid method, the method is simple to operate, less equipment investment, sulfuric acid and ferrous sulfate recovery The utilization rate is high, and it is worth popularizing and applying.
本发明的技术方案如下:用硫酸法生产钛白粉所得废酸生产硝酸亚铁和硫酸钡的方法，该方法包括如下具体步骤：Technical scheme of the present invention is as follows: produce the method for ferrous nitrate and barium sulfate with sulfuric acid process production titanium dioxide gained waste acid, this method comprises following specific steps:
步骤A:将硫酸法生产钛白粉所得废酸与过量氢氧化亚铁溶液混合，使硫酸与氢氧化亚铁反应，生成硫酸亚铁；过滤反应液，得到主要含硫酸亚铁的滤液，含少量未反应的氢氧化亚铁和不溶性杂质的滤渣，滤渣深埋或经其他的工艺处理；Step A: mix the waste acid obtained by the sulfuric acid method to produce titanium dioxide with excess ferrous hydroxide solution, react sulfuric acid with ferrous hydroxide to generate ferrous sulfate; filter the reaction solution to obtain a filtrate mainly containing ferrous sulfate, containing a small amount of The filter residue of unreacted ferrous hydroxide and insoluble impurities, the filter residue is deeply buried or processed by other processes;
步骤B:向步骤A所得的主要含硫酸亚铁的滤液中加入过量的硝酸钡，搅拌下反应，生成硝酸亚铁和硫酸钡，过滤反应液，分离硫酸钡沉淀和硝酸亚铁溶液；该步骤中，少量未反应的硝酸钡也在硝酸亚铁溶液中；Step B: add excessive barium nitrate in the filtrate mainly containing ferrous sulfate of step A gained, react under stirring, generate ferrous nitrate and barium sulfate, filter reaction solution, separate barium sulfate precipitation and ferrous nitrate solution; This step In, a small amount of unreacted barium nitrate is also in the ferrous nitrate solution;
步骤C：将步骤B所得硫酸钡沉淀经洗涤、干燥和粉碎，得到硫酸钡沉淀产品；Step C: washing, drying and pulverizing the barium sulfate precipitate obtained in step B to obtain the barium sulfate precipitate product;
步骤D: 将步骤B所得硝酸亚铁溶液中加入少量硫酸亚铁中和硝酸钡，而后送入碱压蒸馏器中减压蒸馏为硝酸亚铁过饱和溶液，冷却结晶，干燥，得到硝酸亚铁产品。Step D: Add a small amount of ferrous sulfate to the ferrous nitrate solution obtained in step B to neutralize barium nitrate, then send it to an alkaline pressure still to distill under reduced pressure to be a supersaturated solution of ferrous nitrate, crystallize by cooling, and dry to obtain ferrous nitrate product.
本发明所述用硫酸法生产钛白粉所得废酸生产硝酸亚铁和硫酸钡的方法，充分利用了硫酸法生产钛白粉所得废酸中含有的硫酸和硫酸亚铁，其步骤简单，设备投资少，而硝酸亚铁和硫酸钡产率较高，是一个值得推广应用的方法。The method for producing ferrous nitrate and barium sulfate from the waste acid obtained by the production of titanium dioxide by the sulfuric acid method of the present invention fully utilizes the sulfuric acid and ferrous sulfate contained in the waste acid obtained by the production of titanium dioxide by the sulfuric acid method, the steps are simple, and the equipment investment is small , and the ferrous nitrate and barium sulfate yields are higher, which is a method worthy of popularization and application.
具体实施方式Detailed ways
实施例1：用硫酸法生产钛白粉所得废酸生产硝酸亚铁和硫酸钡的方法，该方法包括如下具体步骤：Embodiment 1: the method for producing ferrous nitrate and barium sulfate with sulfuric acid process to produce titanium dioxide gained waste acid, the method comprises following specific steps:
步骤A:将硫酸法生产钛白粉所得废酸与过量氢氧化亚铁溶液混合，使硫酸与氢氧化亚铁反应，生成硫酸亚铁；过滤反应液，得到主要含硫酸亚铁的滤液，含少量未反应的氢氧化亚铁和不溶性杂质的滤渣，滤渣深埋或经其他的工艺处理；Step A: mix the waste acid obtained by the sulfuric acid method to produce titanium dioxide with excess ferrous hydroxide solution, react sulfuric acid with ferrous hydroxide to generate ferrous sulfate; filter the reaction solution to obtain a filtrate mainly containing ferrous sulfate, containing a small amount of The filter residue of unreacted ferrous hydroxide and insoluble impurities, the filter residue is deeply buried or processed by other processes;
步骤B:向步骤A所得的主要含硫酸亚铁的滤液中加入过量的硝酸钡，搅拌下反应，生成硝酸亚铁和硫酸钡，过滤反应液，分离硫酸钡沉淀和硝酸亚铁溶液；该步骤中，少量未反应的硝酸钡也在硝酸亚铁溶液中；Step B: add excessive barium nitrate in the filtrate mainly containing ferrous sulfate of step A gained, react under stirring, generate ferrous nitrate and barium sulfate, filter reaction solution, separate barium sulfate precipitation and ferrous nitrate solution; This step In, a small amount of unreacted barium nitrate is also in the ferrous nitrate solution;
步骤C：将步骤B所得硫酸钡沉淀经洗涤、干燥和粉碎，得到硫酸钡沉淀产品；Step C: washing, drying and pulverizing the barium sulfate precipitate obtained in step B to obtain the barium sulfate precipitate product;
步骤D: 将步骤B所得硝酸亚铁溶液中加入少量硫酸亚铁中和硝酸钡，而后送入碱压蒸馏器中减压蒸馏为硝酸亚铁过饱和溶液，冷却结晶，干燥，得到硝酸亚铁产品。Step D: Add a small amount of ferrous sulfate to the ferrous nitrate solution obtained in step B to neutralize barium nitrate, then send it to an alkaline pressure still to distill under reduced pressure to be a supersaturated solution of ferrous nitrate, crystallize by cooling, and dry to obtain ferrous nitrate product.
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，其架构形式能够灵活多变，可以派生系列产品。只是做出若干简单推演或替换，都应当视为属于本发明由所提交的权利要求书确定的专利保护范围。The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be assumed that the specific implementation of the present invention is limited to these descriptions. For those of ordinary skill in the technical field to which the present invention belongs, without departing from the concept of the present invention, its architecture can be flexible and changeable, and series of products can be derived. Just making some simple deductions or replacements should be deemed to belong to the patent protection scope of the present invention determined by the submitted claims.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105271310A (en) * | 2015-10-13 | 2016-01-27 | 锦州钛业有限公司 | Chlorination-process titanium-white high-salt wastewater comprehensive utilization method |
| CN118307023A (en) * | 2024-04-08 | 2024-07-09 | 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01203226A (en) * | 1988-02-10 | 1989-08-16 | Ishihara Sangyo Kaisha Ltd | Production of ferromagnetic iron oxide containing cobalt |
| 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 |
-
2010
- 2010-12-31 CN CN2010106154734A patent/CN102115209B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01203226A (en) * | 1988-02-10 | 1989-08-16 | Ishihara Sangyo Kaisha Ltd | Production of ferromagnetic iron oxide containing cobalt |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105271310A (en) * | 2015-10-13 | 2016-01-27 | 锦州钛业有限公司 | Chlorination-process titanium-white high-salt wastewater comprehensive utilization method |
| CN118307023A (en) * | 2024-04-08 | 2024-07-09 | 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 |
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