CN1075120C - Process for extracting manganese ore with sulfuric acid at ordinary temperature - Google Patents
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 72
- 239000011572 manganese Substances 0.000 title claims abstract description 72
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 35
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000000654 additive Substances 0.000 claims abstract description 19
- 230000000996 additive effect Effects 0.000 claims abstract description 15
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 11
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 11
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 11
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical group O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical group [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 3
- AOSFMYBATFLTAQ-UHFFFAOYSA-N 1-amino-3-(benzimidazol-1-yl)propan-2-ol Chemical compound C1=CC=C2N(CC(O)CN)C=NC2=C1 AOSFMYBATFLTAQ-UHFFFAOYSA-N 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims description 2
- 235000019252 potassium sulphite Nutrition 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 15
- 238000002386 leaching Methods 0.000 abstract description 14
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000007795 chemical reaction product Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 4
- 239000011656 manganese carbonate Substances 0.000 description 4
- 235000006748 manganese carbonate Nutrition 0.000 description 4
- 229940093474 manganese carbonate Drugs 0.000 description 4
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 4
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明涉及一种从锰矿石中提取锰的方法，它解决了目前蒸汽热法耗能及浸取率低和成本高的缺陷。本发明方法是用锰矿粉与废电解锰溶液或废电解二氧化锰溶液或水打浆后加入过量硫酸反应，加入工业软锰粉反应，再加入废电解锰溶液反应，加入添加剂亚硫酸盐反应后，再加入工业软锰矿粉反应，从反应溶液中收集反应生成物硫酸锰溶液。该方法适用于各类以锰矿粉和硫酸为原料生产锰制品的厂家采用。The invention relates to a method for extracting manganese from manganese ore, which solves the defects of low energy consumption, low leaching rate and high cost of the current steam heat method. The method of the present invention is to use manganese ore powder and waste electrolytic manganese solution or waste electrolytic manganese dioxide solution or water to make pulp, add excess sulfuric acid to react, add industrial soft manganese powder to react, then add waste electrolytic manganese solution to react, add additive sulfite to react , and then add industrial pyrolusite powder to react, and collect the reaction product manganese sulfate solution from the reaction solution. The method is applicable to various manufacturers who produce manganese products using manganese ore powder and sulfuric acid as raw materials.
Description
本发明涉及一种用硫酸浸取锰矿石的方法，特别是一种常温下硫酸浸取锰矿石的方法。The invention relates to a method for leaching manganese ore with sulfuric acid, in particular to a method for leaching manganese ore with sulfuric acid at normal temperature.
目前，所有用硫酸与锰矿粉为原料生产硫酸锰，电解金属锰，电解二氧化锰，碳酸锰等锰制品的生产厂家，均是采用蒸汽加温下硫酸与锰矿石反应浸取生成硫酸锰溶液的方法简称蒸汽热法，该方法不仅要蒸汽锅炉，管道等设施，能耗高而且锰矿石的浸取率也不高，一般在85％左右，生产成本高。At present, all manufacturers who use sulfuric acid and manganese ore powder as raw materials to produce manganese sulfate, electrolytic manganese metal, electrolytic manganese dioxide, manganese carbonate and other manganese products use steam heating to react sulfuric acid and manganese ore to generate manganese sulfate solution. The method is referred to as the steam heat method, and this method not only needs steam boilers, pipelines and other facilities, but also has high energy consumption and the leaching rate of manganese ore is not high, generally around 85%, and the production cost is high.
本发明的目的在于提供一种工艺简单，成本低廉，浸取率高的常温下硫酸浸取锰矿石的方法。The object of the present invention is to provide a method for leaching manganese ore with sulfuric acid at normal temperature with simple process, low cost and high leaching rate.
本发明是用如下方式完成的：常温下硫酸浸取锰矿石的方法是依次采用下述步骤：The present invention is accomplished in the following manner: the method for sulfuric acid leaching of manganese ore at normal temperatures is to adopt the following steps successively:
1)．将锰矿粉投入至反应罐中，加入反应罐体积25％-50％的废电解锰溶液或废电解二氧化锰溶液或水混合打成浆状液，再加入按测试出锰矿粉实际耗酸量过量5％-15％的工业浓硫酸反应0.5-1.5小时；1). Put the manganese ore powder into the reaction tank, add waste electrolytic manganese solution or waste electrolytic manganese dioxide solution or water mixed with 25%-50% of the volume of the reaction tank to make a slurry, then add the actual acid consumption of manganese ore powder according to the test Excessive 5%-15% industrial concentrated sulfuric acid reaction for 0.5-1.5 hours;
2)．加入按锰矿粉重量3％-4％的工业软锰矿粉反应0.5-1.5小时；2). Add 3%-4% industrial pyrolusite powder by weight of manganese ore powder and react for 0.5-1.5 hours;
3)．加入废电解锰溶液或废电解二氧化锰溶液或水至反应罐预定体积，反应0.5-1.5小时；3). Add waste electrolytic manganese solution or waste electrolytic manganese dioxide solution or water to the predetermined volume of the reaction tank, and react for 0.5-1.5 hours;
4)．加入添加剂为亚硫酸铵或亚硫酸氢铵或亚硫酸钠或亚硫酸氢钠或亚硫酸钾，辅助添加剂为甲醛或甲醇或双氧水反应2-4小时，添加剂加入量为锰矿粉重量的0.5％-5％；4). The additive is ammonium sulfite or ammonium bisulfite or sodium sulfite or sodium bisulfite or potassium sulfite, the auxiliary additive is formaldehyde or methanol or hydrogen peroxide for 2-4 hours, and the additive amount is 0.5%-5% of the weight of manganese ore powder ;
5)．加入按锰矿粉重量5％-15％的工业软锰矿粉反应0.5-1.5小时，从反应溶液中收集生成物硫酸锰溶液。5). 5%-15% of industrial pyrolusite powder by weight of manganese ore powder is added to react for 0.5-1.5 hours, and the resulting manganese sulfate solution is collected from the reaction solution.
加入的添加剂为液态含SO2250-300g/L时，其加入量为锰矿粉重量的1.6％-5％，当添加剂为固态时，其加入量为锰矿粉重量的0.5％-2％。When the added additive is in liquid state and contains SO 2 250-300g/L, the added amount is 1.6%-5% of the weight of the manganese ore powder; when the additive is solid, the added amount is 0.5%-2% of the weight of the manganese ore powder.
本发明常温下硫酸浸取锰矿石方法的工艺流程不仅操作简单，而且浸取率高，二价铁氧化完全，采用加入添加剂亚硫酸盐还原锰矿粉中所含的少量高价态锰，同时激活碳酸锰矿石与硫酸的反应，使锰矿粉中的锰能极大程度地被硫酸浸取转化成硫酸锰溶液，辅助添加剂抑制三价铁不被亚硫酸还原成二价铁，采用过量的硫酸能保证亚硫酸盐与高价态锰顺利反应，该方法锰浸取率达到和超过蒸汽热法技术，添加剂成本低廉，并且对后工序的生产没有任何不良影响，其生产稳定。它与蒸汽热法比较，节约了蒸汽和省除了锅炉与蒸汽管道等设备，大大地降低了生产成本，该方法适用于所有用硫酸与锰矿粉为原料生产硫酸锰、碳酸锰、电解金属锰、电解二氧化锰及所有锰制品的厂家使用。The process flow of the method for leaching manganese ore with sulfuric acid at normal temperature is not only simple to operate, but also has a high leaching rate, complete oxidation of ferrous iron, and a small amount of high-valent manganese contained in the manganese ore powder is reduced by adding additive sulfite, while activating carbonic acid The reaction between manganese ore and sulfuric acid enables the manganese in the manganese ore powder to be leached by sulfuric acid to a great extent and converted into manganese sulfate solution. The auxiliary additive prevents ferric iron from being reduced to ferrous iron by sulfurous acid. Excessive sulfuric acid can ensure Sulfite reacts smoothly with high-valence manganese. The manganese leaching rate of this method reaches or exceeds that of the steam thermal method. The cost of additives is low, and there is no adverse effect on the production of the subsequent process, and the production is stable. Compared with the steam thermal method, it saves steam and saves equipment such as boilers and steam pipes, and greatly reduces production costs. This method is suitable for all production of manganese sulfate, manganese carbonate, electrolytic metal manganese, etc. using sulfuric acid and manganese ore powder as raw materials. Manufacturers of electrolytic manganese dioxide and all manganese products.
下面用实施例对本发明作进一步详细的说明：The present invention is described in further detail below with embodiment:
本发明的工艺流程为：Process flow of the present invention is:
锰矿粉加部分废电解锰液(或废电解二氧化锰溶液或水)混合打成浆状液→加浓硫酸反应→加部分工业软锰矿粉反应→用废电解锰液加满反应罐→加入亚硫酸盐添加剂反应→加入工业软锰矿粉反应→石灰水中和加除杂剂与添加剂，过滤收集反应生成物硫酸锰溶液。Mix manganese ore powder with part of waste electrolytic manganese solution (or waste electrolytic manganese dioxide solution or water) to form a slurry → add concentrated sulfuric acid for reaction → add part of industrial pyrolusite powder for reaction → fill up the reaction tank with waste electrolytic manganese solution → add Sulfite additive reaction → adding industrial pyrolusite powder reaction → lime water neutralization, adding impurity remover and additives, filtering and collecting the reaction product manganese sulfate solution.
现以锰矿粉含锰20％，其中以碳酸锰形式存在的锰为19％，测试出锰矿粉的实际耗酸量为0.55吨/吨矿，硫酸浓度93％、电解锰废液中含锰12.5g/L，含H2SO4,20.0g/L原材料来实施本发明方法：Manganese ore powder now contains 20% manganese, of which the manganese in the form of manganese carbonate is 19%. The actual acid consumption of manganese ore powder is 0.55 tons per ton of ore, the concentration of sulfuric acid is 93%, and the manganese content in electrolytic manganese waste liquid is 12.5%. g/L, containing H 2 SO 4 , 20.0g/L raw material implements the inventive method:
实施例一：在22m3容积反应罐中加入废电解锰液总量20m3，按锰全部浸出浓度为40g/L计算锰矿粉的投料量2.75吨，按过量10％计算硫酸的加入量为1.36吨，以保证亚硫酸盐与高价态锰能顺利反应。Embodiment 1: Add 20m 3 of waste electrolytic manganese liquid total amount in 22m 3 capacity reaction tank, calculate the feeding amount of manganese ore powder as 40g/L according to the total manganese leaching concentration, calculate the addition amount of sulfuric acid as 1.36 according to excess 10%. tons to ensure the smooth reaction between sulfite and high-valence manganese.
将2.75吨锰矿粉与7m3废电解锰液投入反应罐中，搅拌成浆状液，然后加入1.36吨93％的工业硫酸，搅拌下反应1小时后，加入工业软锰矿粉100公斤反应1小时，然后加入13m3废电解锰液反应1小时，加入添加剂亚硫酸铵溶液(含SO2280g/L)80公斤，加入亚硫酸铵还原锰矿粉中所含的少量高价态锰(如Mn02)，同时激活碳酸锰与硫酸的反应，使锰矿粉中的锰能极大程度地被硫酸浸取转化成硫酸锰溶液，辅助添加剂为含量10％甲醇200ml，反应2.5小时，辅助添加剂抑制三价铁不被亚硫酸还原成二价铁，有些矿可以不加辅助添加剂，辅助添加剂加入量为每反应罐(22m3)200-500ml再加入工业软锰矿粉250公斤，反应半小时后，检测溶液中锰与亚铁的含量，亚铁含量达到≤0.01％的要求后，加入石灰水(氢氧化钙)中和至PH6.5-7.0即可，此时硫酸锰溶液浸取率一般为95％左右。Put 2.75 tons of manganese ore powder and 7m3 waste electrolytic manganese solution into the reaction tank, stir to form a slurry, then add 1.36 tons of 93% industrial sulfuric acid, and react for 1 hour under stirring, then add 100 kg of industrial pyrolus powder and react for 1 hour , then add 13m waste electrolytic manganese solution and react for 1 hour, add 80 kg of additive ammonium sulfite solution (containing SO 2 280g/L), add a small amount of high-valent manganese (such as Mn0 2 ) contained in ammonium sulfite reduction manganese ore powder , and activate the reaction between manganese carbonate and sulfuric acid at the same time, so that the manganese in the manganese ore powder can be leached by sulfuric acid to a great extent and converted into manganese sulfate solution. It will not be reduced to ferrous iron by sulfurous acid. Some minerals can not add auxiliary additives. The amount of auxiliary additives added is 200-500ml per reaction tank (22m 3 ), and then 250 kg of industrial pyrolusite powder is added. After half an hour of reaction, the detection solution The content of manganese and ferrous, after the ferrous content reaches the requirement of ≤0.01%, add lime water (calcium hydroxide) to neutralize to PH6.5-7.0, at this time, the leaching rate of manganese sulfate solution is generally about 95% .
实施例二：在22m3的反应罐中加入废电解锰液总量21m3，按锰全部浸出浓度为40g/L计算锰矿粉的投料量为2.89吨，按过量8％计算工业硫酸(93％)的加入量为1.39吨。将2.89吨锰矿粉与7m3废电解液投入反应罐中搅拌成浆后，加入93％的硫酸1.39吨，搅拌均匀反应1小时。再加入工业软锰矿粉100公斤，反应1小时。加入废电解锰溶液14m3，反应1小时，加入亚硫酸铵溶液(含SO2280g/L)100公斤，并同时加入10％的甲醇200ml，反应2.5小时。加入工业软锰矿粉250公斤，反应半小时后，检测反应生成物溶液中锰与亚铁的含量，当亚铁量达到≤0.01％的要求后，加入石灰水中和至PH:6.5-7.0，此时，硫酸锰溶液浸取率可达95％左右。Embodiment two: add spent electrolytic manganese liquid total amount 21m in the reaction tank of 22m 3 , be 40g/L to calculate the feed intake of manganese ore powder by manganese total leaching concentration is 2.89 tons, calculate industrial sulfuric acid (93% by excessive 8%) ) is added in an amount of 1.39 tons. Put 2.89 tons of manganese ore powder and 7m 3 waste electrolyte into a reaction tank and stir to form a slurry, then add 1.39 tons of 93% sulfuric acid, and stir for a uniform reaction for 1 hour. Then add 100 kg of industrial pyrolusite powder and react for 1 hour. Add 14 m 3 of spent electrolytic manganese solution, react for 1 hour, add 100 kg of ammonium sulfite solution (containing SO 2 280 g/L), and simultaneously add 200 ml of 10% methanol, and react for 2.5 hours. Add 250 kg of industrial pyrolusite powder and react for half an hour to detect the content of manganese and ferrous iron in the reaction product solution. When the ferrous iron content reaches the requirement of ≤0.01%, add lime water to neutralize to pH: 6.5-7.0. , the leaching rate of manganese sulfate solution can reach about 95%.
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| CN1295355C (en) * | 2004-07-19 | 2007-01-17 | 中南大学 | Method of manufacturing electrolytic metal manganese using titanium white waste acid and manganese dioxide ore |
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| CN101880767A (en) * | 2010-06-07 | 2010-11-10 | 姚茂君 | Process for reducing leached pyrolusite ore by iron powder |
| CN103757247A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching manganese carbonate ore |
| CN103757249A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching manganese carbonate ore |
| CN103757444B (en) * | 2013-12-29 | 2015-05-13 | 四川师范大学 | Method for leaching pyrolusite |
| CN103937973B (en) * | 2014-04-16 | 2016-01-06 | 广西民族大学 | A kind of method of Organic-inorganic composite reducing pyrolusite |
| CN113088999B (en) * | 2021-03-31 | 2021-12-31 | 广西桂柳新材料股份有限公司 | Preparation method of electrolytic manganese dioxide for mercury-free alkaline zinc-manganese battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086548A (en) * | 1992-11-02 | 1994-05-11 | 冶金工业部长沙冶金研究院 | Preparation of highly pure manganese sulfate with high yield rate |
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1997
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086548A (en) * | 1992-11-02 | 1994-05-11 | 冶金工业部长沙冶金研究院 | Preparation of highly pure manganese sulfate with high yield rate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295355C (en) * | 2004-07-19 | 2007-01-17 | 中南大学 | Method of manufacturing electrolytic metal manganese using titanium white waste acid and manganese dioxide ore |
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| CN1210893A (en) | 1999-03-17 |
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