CN103757203A - Iron and titanium leaching agent as well as process and application thereof in removing iron and titanium from flotation tailings of iron pyrite - Google Patents
Iron and titanium leaching agent as well as process and application thereof in removing iron and titanium from flotation tailings of iron pyrite Download PDFInfo
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- CN103757203A CN103757203A CN201310751214.8A CN201310751214A CN103757203A CN 103757203 A CN103757203 A CN 103757203A CN 201310751214 A CN201310751214 A CN 201310751214A CN 103757203 A CN103757203 A CN 103757203A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 98
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000010936 titanium Substances 0.000 title claims abstract description 50
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 50
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 49
- 238000002386 leaching Methods 0.000 title claims abstract description 43
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 32
- 238000005188 flotation Methods 0.000 title claims abstract description 30
- 229910052683 pyrite Inorganic materials 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 30
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011028 pyrite Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 10
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 10
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 10
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011737 fluorine Substances 0.000 claims abstract description 7
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 7
- 239000003930 superacid Substances 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000000919 ceramic Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 6
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 5
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
本发明公开了一种铁和钛浸出剂及其除硫铁矿浮选尾矿中铁和钛的工艺和应用，该铁和钛浸出剂由含氟有机超强酸或碳硼烷酸、Na2S2O4、草酸、硫酸铵和水组成；用该浸出剂除硫铁矿浮选尾矿中铁和钛的工艺是将硫铁矿浮选尾矿与所述浸出剂混合，在搅拌条件下浸出后，冷却，过滤，将滤渣洗涤，即得除铁和钛的浸出渣；该工艺能有效同时浸出除去硫铁矿浮选尾矿中的铁和钛制得优质陶瓷材料，该工艺变废为宝，使资源得到综合利用，环境保护得到有效提高。The invention discloses an iron and titanium leaching agent and its technology and application for removing iron and titanium in pyrite flotation tailings. The iron and titanium leaching agent is composed of fluorine-containing organic super acid or carborane acid, Na 2 S 2 O 4 , oxalic acid, ammonium sulfate and water; the process of using this leaching agent to remove iron and titanium in pyrite flotation tailings is to mix pyrite flotation tailings with the leaching agent, and leaching under stirring conditions After cooling, filtering, and washing the filter residue, the leaching residue for removing iron and titanium can be obtained; this process can effectively leaching and removing iron and titanium in pyrite flotation tailings at the same time to obtain high-quality ceramic materials, and this process turns waste into Treasure, so that resources can be comprehensively utilized, and environmental protection has been effectively improved.
Description
技术领域technical field
本发明涉及一种铁和钛浸出剂及其除硫铁矿浮选尾矿中铁和钛的工艺和应用，属于新型资源利用和环境保护领域。The invention relates to an iron and titanium leaching agent and its technology and application for removing iron and titanium in pyrite flotation tailings, belonging to the fields of new resource utilization and environmental protection.
背景技术Background technique
随着矿产资源的不断开发利用，富矿易处理矿石日益减少，同时产生的低品位尾矿处理不得不开发利用。目前，大部分的尾矿被排放到尾矿库中囤积，但是尾矿库存在的安全隐患大，且尾矿库都有一定的使用年限，近几年尾矿库事故时有发生，国家政策对尾矿的排放要求也比较严格，对尾矿库的审批也比较严格。硫铁矿经过浮选以后，会产生大量的尾矿，如果不适当处理，不仅增大了尾矿库的囤积成本，使尾矿库的安全隐患扩大，而且还会产生一些列的环境问题，譬如尾矿的重金属或放射性元素对生态环境的污染破坏。目前已经有过一些高岭土除铁增白作为陶瓷原料的一些报道，而硫铁矿浮选尾矿同时进行除铁除钛用来作陶瓷材料还未见报道。With the continuous development and utilization of mineral resources, the rich ore and easy-to-handle ore are decreasing day by day, and the low-grade tailings produced at the same time have to be developed and utilized. At present, most of the tailings are discharged into tailings ponds for hoarding, but the safety hazards of tailings stockpiles are large, and tailings ponds have a certain service life. In recent years, tailings pond accidents have occurred from time to time. The national policy The discharge requirements for tailings are also relatively strict, and the approval for tailings ponds is also relatively strict. After pyrite is flotation, a large amount of tailings will be produced. If it is not handled properly, it will not only increase the storage cost of tailings ponds, but also increase the potential safety hazards of tailings ponds, and will also cause a series of environmental problems. For example, heavy metals or radioactive elements in tailings pollute and damage the ecological environment. At present, there have been some reports of kaolin removing iron and whitening as ceramic raw materials, but there is no report on pyrite flotation tailings being used for ceramic materials by simultaneously removing iron and titanium.
发明内容Contents of the invention
为了克服现有技术中对硫铁矿浮选尾矿的处理存在的缺陷，本发明的目的是在于提供一种对能高效同时浸出硫铁矿浮选尾矿中的铁和钛获得优质陶瓷原料的铁和钛浸出剂。In order to overcome the defects existing in the treatment of pyrite flotation tailings in the prior art, the purpose of the present invention is to provide a method for efficiently simultaneously leaching iron and titanium in pyrite flotation tailings to obtain high-quality ceramic raw materials iron and titanium leaching agent.
本发明的另一个目的是在于提供一种用所述铁和钛浸出剂有效去除硫铁矿浮选尾矿中铁和钛制备陶瓷原材料的工艺，该工艺变废为宝，使资源得到综合利用，环境保护得到有效提高。Another object of the present invention is to provide a process for effectively removing iron and titanium in the pyrite flotation tailings to prepare ceramic raw materials by using the iron and titanium leaching agent. This process turns waste into treasure and makes comprehensive utilization of resources. Environmental protection has been effectively improved.
本发明的第三个目的是在于提供所述铁和钛浸出剂的应用，所述铁和钛浸出剂能有效同时浸出硫铁矿浮选尾矿中的铁和钛，获得优质陶瓷原材料。The third object of the present invention is to provide the application of the iron and titanium leaching agent, which can effectively and simultaneously leach iron and titanium in pyrite flotation tailings to obtain high-quality ceramic raw materials.
本发明提供了一种铁和钛浸出剂，该浸出剂由以下质量份组分组成：含氟有机超强酸或碳硼烷酸0.5～5份；Na2S2O40.2～2份；草酸0.2～2份；硫酸铵0.2～2份；水1～6份。The invention provides an iron and titanium leaching agent, which is composed of the following components in parts by mass: 0.5-5 parts of fluorine-containing organic super acid or carborane acid; 0.2-2 parts of Na 2 S 2 O 4 ; oxalic acid 0.2 to 2 parts; 0.2 to 2 parts of ammonium sulfate; 1 to 6 parts of water.
优选的浸出剂由以下质量份组分组成：含氟有机超强酸或碳硼烷酸0.5～3份；Na2S2O40.5～1份；草酸0.5～1份；硫酸铵0.5～1份；水2～5份。The preferred leaching agent is composed of the following components by mass: 0.5-3 parts of fluorine-containing organic superacid or carborane acid; 0.5-1 part of Na 2 S 2 O 4 ; 0.5-1 part of oxalic acid; 0.5-1 part of ammonium sulfate ; 2 to 5 parts of water.
所述的含氟有机超强酸为RfSO3H、(RfSO2)2NH、(RfSO2)3CH中一种或几种，其中，Rf为全氟烷基，如C1～C10全氟烷基。The fluorine-containing organic superacid is one or more of R f SO 3 H, (R f SO 2 ) 2 NH, (R f SO 2 ) 3 CH, wherein R f is a perfluoroalkyl group, such as C 1 -C 10 perfluoroalkyl.
本发明还提供了一种用所述铁和钛浸出剂除硫铁矿浮选尾矿中铁和钛的工艺，该工艺是将硫铁矿浮选尾矿与所述浸出剂以固液体积比2～8:1～4混合，控制温度在50～110℃，在速率为100～600转/分的搅拌条件下，浸出0.5～5小时后，冷却，过滤，将滤渣洗涤，即得除铁和钛的浸出渣。The present invention also provides a process for removing iron and titanium in pyrite flotation tailings by using the iron and titanium leaching agent. Mix 2～8:1～4, control the temperature at 50～110℃, under the stirring condition of 100～600 rev/min, leaching for 0.5～5 hours, cooling, filtering, washing the filter residue to obtain iron removal and titanium leaching residue.
所述的除铁和钛的浸出渣在50～180℃下恒温干燥0.5～7小时，得到陶瓷原料。The leached slag from iron and titanium removal is dried at a constant temperature of 50-180° C. for 0.5-7 hours to obtain ceramic raw materials.
所述的冷却是将温度降低到不大于30℃。The cooling is to reduce the temperature to not more than 30°C.
本发明还提供了所述铁和钛浸出剂的应用，该应用是将所述铁和钛浸出剂应用于同时浸出去除硫铁矿浮选尾矿中的铁和钛制备陶瓷原材料。The present invention also provides the application of the iron and titanium leaching agent. The application is to apply the iron and titanium leaching agent to simultaneously leaching and removing iron and titanium in pyrite flotation tailings to prepare ceramic raw materials.
本发明的有益效果：本发明经过大量实验复配得到一种能够同时浸出硫化矿浮选尾矿中铁和钛的浸出剂，通过对硫化矿浮选尾矿中铁和钛的有效浸出去除，能获得优质的陶瓷原材料。大量实验研究表明：硫化矿浮选尾矿使用本发明铁和钛浸出剂处理后的尾矿中含铁和钛总量降低至0.5wt%以下，将废弃的硫铁矿浮选尾矿变废为宝，使资源得到综合利用，环境保护得到有效提高。Beneficial effects of the present invention: the present invention obtains a leaching agent capable of simultaneously leaching iron and titanium in sulfide ore flotation tailings through a large number of experiments, and can obtain High-quality ceramic raw materials. A large number of experimental studies have shown that: the total amount of iron and titanium in the sulfide ore flotation tailings treated with the iron and titanium leaching agent of the present invention is reduced to below 0.5wt%, and the discarded pyrite flotation tailings become waste It is a treasure, so that resources can be comprehensively utilized and environmental protection can be effectively improved.
具体实施方式Detailed ways
以下实施例旨在进一步保护本发明，而不是限制本发明保护的范围。The following examples are intended to further protect the present invention, but not to limit the scope of protection of the present invention.
实施例1Example 1
将硫铁矿浮选尾矿（含铁量1.6wt%，含钛量3.8wt%）与新型浸取剂按液固体积比5:2混合。新型浸取剂由2份C4F9SO3H、1份Na2S2O4、1份草酸、1份硫酸铵和5份水组成。在温度为80℃，速度为350转/分的搅拌条件下，浸出3小时，然后过滤，用蒸馏水清洗三次，滤饼在110℃条件下干燥5小时。处理后的硫铁矿浮选尾矿含铁量为0.34wt%，含钛量为0.14wt%，含铁和钛总量低于0.5wt%，满足生产优质陶瓷的原料要求。The pyrite flotation tailings (1.6wt% iron content, 3.8wt% titanium content) were mixed with the new leaching agent at a liquid-solid volume ratio of 5:2. The new leaching agent is composed of 2 parts of C 4 F 9 SO 3 H, 1 part of Na 2 S 2 O 4 , 1 part of oxalic acid, 1 part of ammonium sulfate and 5 parts of water. The temperature was 80 DEG C, and the speed was 350 rev/min stirring conditions, leached for 3 hours, then filtered, washed three times with distilled water, and the filter cake was dried at 110 DEG C for 5 hours. The treated pyrite flotation tailings contain 0.34wt% iron and 0.14wt% titanium, and the total iron and titanium content is less than 0.5wt%, which meets the raw material requirements for producing high-quality ceramics.
实施例2Example 2
将硫铁矿浮选尾矿（含铁量1.6wt%，含钛量3.8wt%）与新型浸取剂按液固体积比6:2混合。新型浸取剂由3份(C3F7SO2)2NH、0.5份Na2S2O4、1份草酸、1份硫酸铵和4.5份水组成。在温度为90℃，在速度为400转/分的搅拌条件下，浸出3小时，然后过滤，用水清洗三次，滤饼干100℃干燥5小时。处理后的硫铁矿浮选尾矿含铁量为0.28wt%，含钛量为0.10wt%，含铁和钛总量低于0.5wt%，满足生产优质陶瓷的原料要求。The pyrite flotation tailings (1.6wt% iron content, 3.8wt% titanium content) were mixed with the new leaching agent at a liquid-solid volume ratio of 6:2. The new leaching agent is composed of 3 parts of (C 3 F 7 SO 2 ) 2 NH, 0.5 parts of Na 2 S 2 O 4 , 1 part of oxalic acid, 1 part of ammonium sulfate and 4.5 parts of water. At a temperature of 90°C and a stirring condition of 400 rpm, the filter was leached for 3 hours, then filtered, washed with water three times, and the filter cake was dried at 100°C for 5 hours. The iron content of the treated pyrite flotation tailings is 0.28wt%, the titanium content is 0.10wt%, and the total iron and titanium content is less than 0.5wt%, which meets the raw material requirements for the production of high-quality ceramics.
实施例3Example 3
将硫铁矿浮选尾矿（含铁量1.6wt%，含钛量3.8wt%）与新型浸取剂按液固体积比5:3混合，新型浸取剂由2份(C3F7SO2)3CH、0.5份Na2S2O4、0.5份草酸、0.5份硫酸铵和6份水组成。在温度为90℃，在速度为400转/分的搅拌条件下，浸出3小时，然后过滤，用蒸馏水清洗三次（每次80毫升），滤饼在110℃条件下干燥5小时。处理后的硫铁矿浮选尾矿含铁量为0.31wt%，含钛量为0.15wt%，含铁和钛总量低于0.5wt%，满足生产优质陶瓷的原料要求。Mix pyrite flotation tailings (1.6wt% iron content, 3.8wt% titanium content) with a new leaching agent at a liquid-solid volume ratio of 5:3, and the new leaching agent consists of 2 parts (C 3 F 7 SO 2 ) 3 CH, 0.5 parts of Na 2 S 2 O 4 , 0.5 parts of oxalic acid, 0.5 parts of ammonium sulfate and 6 parts of water. At a temperature of 90°C and a stirring speed of 400 rpm, leaching was performed for 3 hours, then filtered, washed three times with distilled water (80 ml each time), and the filter cake was dried at 110°C for 5 hours. The iron content of the treated pyrite flotation tailings is 0.31wt%, the titanium content is 0.15wt%, and the total iron and titanium content is less than 0.5wt%, which meets the raw material requirements for the production of high-quality ceramics.
实施例4Example 4
将硫铁矿浮选尾矿（含铁量1.6wt%，含钛量3.8wt%）与新型浸取剂按液固体积比5:3混合。新型浸取剂由3份(C3F7SO2)3CH、0.5份Na2S2O4、1份草酸、0.5份硫酸铵和5份水组成。控制反应条件为：温度为95℃、搅拌转速350转/分、浸出时间2小时。反应结束后，待其温度降至30℃后过滤，用水清洗三次。最后将过滤后的滤饼于烘箱中（控制温度为110℃）干燥5小时。处理后的硫铁矿浮选尾矿含铁量为0.25wt%，含钛量为0.11wt%，含铁含钛总量低于0.5wt%。实施例5The pyrite flotation tailings (1.6wt% iron content, 3.8wt% titanium content) were mixed with the new leaching agent at a liquid-solid volume ratio of 5:3. The new leaching agent consists of 3 parts of (C 3 F 7 SO 2 ) 3 CH, 0.5 part of Na 2 S 2 O 4 , 1 part of oxalic acid, 0.5 part of ammonium sulfate and 5 parts of water. The controlled reaction conditions are as follows: the temperature is 95° C., the stirring speed is 350 rpm, and the leaching time is 2 hours. After the reaction, the temperature was lowered to 30° C., filtered, and washed with water three times. Finally, the filtered filter cake was dried in an oven (controlling the temperature at 110° C.) for 5 hours. The iron content of the treated pyrite flotation tailings is 0.25wt%, the titanium content is 0.11wt%, and the total iron and titanium content is less than 0.5wt%. Example 5
将硫铁矿浮选尾矿（含铁量1.6wt%，含钛量3.8wt%）与新型浸取剂按液固比5:3混合。新型浸取剂由3份碳硼烷酸、0.5份保险粉Na2S2O4、1份草酸、0.5份硫酸铵和5份水组成。控制反应条件为：温度75℃、搅拌转速250转/分、浸出时间3小时。反应结束后，待其温度降至30℃后过滤，用水清洗三次。最后将过滤后的滤饼于烘箱中（控制温度为110℃）干燥5小时。处理后的硫铁矿浮选尾矿含铁量为0.27wt%，含钛量为0.09wt%，含铁含钛总量低于0.5wt%。The pyrite flotation tailings (1.6wt% iron content, 3.8wt% titanium content) were mixed with the new leaching agent at a liquid-solid ratio of 5:3. The new leaching agent is composed of 3 parts of carborane acid, 0.5 part of sodium hydrosulfite Na 2 S 2 O 4 , 1 part of oxalic acid, 0.5 part of ammonium sulfate and 5 parts of water. The controlled reaction conditions are: temperature 75° C., stirring speed 250 rpm, and leaching time 3 hours. After the reaction, the temperature was lowered to 30° C., filtered, and washed with water three times. Finally, the filtered filter cake was dried in an oven (controlling the temperature at 110° C.) for 5 hours. The iron content of the treated pyrite flotation tailings is 0.27wt%, the titanium content is 0.09wt%, and the total iron and titanium content is less than 0.5wt%.
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| CN110468285A (en) * | 2019-09-11 | 2019-11-19 | 中南大学 | A kind of Ti-containing slag produces TiO2The method of powder |
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| CN102312102A (en) * | 2010-07-02 | 2012-01-11 | 成都理工大学 | Comprehensive utilization method for titanium-contained blast furnace slag |
| CN102674643A (en) * | 2011-03-16 | 2012-09-19 | 北京化工大学 | Method for recovering ferric oxide from red mud by leaching-photocatalysis by oxalic acid |
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| CN102312102A (en) * | 2010-07-02 | 2012-01-11 | 成都理工大学 | Comprehensive utilization method for titanium-contained blast furnace slag |
| CN102674643A (en) * | 2011-03-16 | 2012-09-19 | 北京化工大学 | Method for recovering ferric oxide from red mud by leaching-photocatalysis by oxalic acid |
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| 董强等: ""用废盐酸从钛铁精矿中浸出钛和铁的试验研究"", 《湿法冶金》, vol. 32, no. 1, 28 February 2013 (2013-02-28), pages 38 - 40 * |
| 蔡丽娜等: ""高岭土除铁技术进展"", 《矿冶》, vol. 17, no. 4, 31 December 2008 (2008-12-31), pages 51 - 54 * |
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| CN110468285A (en) * | 2019-09-11 | 2019-11-19 | 中南大学 | A kind of Ti-containing slag produces TiO2The method of powder |
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