CN1657423A - Method of recovering manganese sulfate from low-grade manganese carbonate and manganese oxide - Google Patents
Method of recovering manganese sulfate from low-grade manganese carbonate and manganese oxide Download PDFInfo
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- CN1657423A CN1657423A CN 200510020339 CN200510020339A CN1657423A CN 1657423 A CN1657423 A CN 1657423A CN 200510020339 CN200510020339 CN 200510020339 CN 200510020339 A CN200510020339 A CN 200510020339A CN 1657423 A CN1657423 A CN 1657423A
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Abstract
A process for recovering mangnese sulfate from low-grade mangnese carbonate (or oxide) ore includes such steps as grinding, mixing with pyrite or ferrous sulfate, adding concentrated sulfuric acid, stirring, calcining, extracting in water, removing impurities from the liquid extract, evaporating and crystallizing to obtain MnSO4.H2O.
Description
(1) technical field:
The present invention relates to a kind of from manganese ore the method for reclaim(ed) sulfuric acid manganese, particularly a kind of method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese.
(2) background technology:
Manganese exists in the earth's crust in a large number, and average content is about 0.1%, and its content is big to account for the 15th in known elements, and manganese is only second to iron and occupies second in heavy metal.The purposes of manganese is very extensive, almost relates to the every aspect of human being's production life, and in Iron And Steel Industry, manganese is to occupy iron deputy important metallic element afterwards, and almost the manganese more than 90% is consumed in Iron And Steel Industry.China's accumulative total is verified 6.4 hundred million tons of manganese ore reserves, 4,000 ten thousand tons of manganese metal reserves, be only second to South Africa, Ukraine and Gabon, occupy the 4th in the world, and it is concentrated relatively to distribute, 90% manganese resource concentrates on 6 provinces and regions, wherein Guangxi accounts for 38.6%, the Hunan accounts for 18.5%, and Guizhou accounts for 13.1%, is easy to scale development.But the manganese resource characteristics of China are poor, thin, assorted, and average grade contains manganese about 21%, and low grade ore accounts for 94% of total reserves, and rich ore only accounts for 6.43% of reserves; The manganese ore genetic type accounts for total reserves more than 80% based on the appositional pattern manganese ore, and sedimentary metamorphic type, layer charge type, weathering type manganese are less.And the manganese ore ore type accounts for 73% of total reserves based on manganese carbonate ore, and inferior is ferrimanganic ore deposit and manganese oxide ore, and spartaite and ferromanganese ore are very few.The ore of producing 70% is a manganese oxide ore at present, along with exploitation for many years, the manganese oxide rich ore falls sharply, many old mine manganese resources are petered out, therefore need a large amount of manganese ore of import could satisfy the needs of the national economic development, but develop rapidly along with industry such as China's iron and steel in recent years, the rich manganese ore of China can not satisfy the needs of the national economic development generally, need be from Australia, the rich manganese ore of state such as Burma and Gabon import, therefore, China has become maximum in the world manganese ore importer, but along with China will realize the ambitious goal that gross national product quadruples again, China can be more outstanding to the demand contradictory of rich manganese ore, therefore is necessary the poor manganese resource of China is developed and utilized.The recovery technology of both at home and abroad low-grade manganese being taked mainly is the mechanical beneficiation method at present, abroad the ore-dressing technique to poor manganese ore is basic screen work with washup and gravity treatment mainly, as washup-gravity treatment, washup-gravity treatment-strong magnetic, washup-gravity treatment-strong magnetic-flotation, washup-gravity treatment-roasting, gravity treatment-strong magnetic, washup-strong magnetic-flotation, gravity treatment-flotation, dense medium-flotation-Qiang Ci etc.Other technology that is adopted is also seen autogenous grinding-magnetic-high-gradient magnetic separation, single flotation, roasting-screening, roasting-magnetic separation-flow processs such as pelletizing by force.From the ore dressing effect, the selected grade in external mine is many about 20%, concentrate grade 27.8～47 42%, and generally about 35, concentration ratio about 1.8, the rate of recovery is many more than 70%.The mechanical beneficiation method that China adopts poor manganese ore is then based on weight-magnetic current journey or single washing.Because the grade of China's poor manganese ore is lower, the ore complex structure, the manganese mineral granularity is tiny, so the effect of mechanical beneficiation is not satisfactory, the concentrate grade increase rate is little.According to the test and the actual production result in some mines, concentrate grade does not often reach 30%, and the beneficiation cost height, and economic feasibility is poor.This kind result still is considered to adopt the mechanical beneficiation free-milling ore at those, and is more undesirable for the ore enriching and recovering effect of difficulty choosing, therefore adopt the existing machinery beneficiating method reclaim manganese be exist very big circumscribed.
(3) summary of the invention:
The present invention will disclose a kind of rate of recovery height, non-environmental-pollution, simple to operate, from the method for low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese.
Method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese of the present invention, its step is as follows:
1) low-grade manganese carbonate and manganese oxide raw ore is levigate, as it being milled to below-100 orders so that mix with other partition;
2) levigated manganese carbonate ore or manganese oxide ore are mixed with pyrite or ferrous sulfate; Wherein the weight ratio of manganous carbonate or manganese oxide ore and pyrite or ferrous sulfate is generally 0.1: 0.05～0.19; And the blending means that is adopted should be decided according to practical situation, above-mentioned material can be adopted and grind the body ground and mixed, mixes at the industrial ball mill that then can adopt, and also can adopt other method to carry out the mixing of material certainly;
3) in the material that mixes, add the vitriol oil; The sulfuric acid weight ratio of described manganous carbonate or manganese oxide ore and adding is generally between 1: 0.4～1.0; And the weight concentration of the selected vitriol oil is preferably between 80～98%;
4) material that mixes is put into and is carried out roasting; When carrying out calcining process, its temperature should be controlled at 100 ℃～600 ℃; Roasting time was generally 0.5～3 hour, and for reaching the best effect that bakes, the temperature of roasting is preferably 500 ℃; Roasting time is preferably 1 hour; Because of producing a large amount of sulfur dioxide gas in the roasting process, sulfur dioxide gas escapes, then can cause environmental pollution, so for preventing that sulfur dioxide gas from escaping, the sulfur dioxide gas that roasting process produces can be fed in the leach liquor of low-grade manganese oxide ore, leach the manganese in the low-grade manganese oxide ore, so both prevented from escaping of sulfur dioxide gas from also to have made full use of reactive material; For reaching best effect, preferably leach manganese in the low-grade manganese oxide ores down 20～60 ℃ of temperature, until the manganese oxide ore leaching yield greater than 90%;
5) calcining that obtains of sulfation adopts 20～90 ℃ of water extractions, obtains the manganous sulfate infusion solution of pH=6～7; The solvent and solute weight ratio of wherein said calcining and water is generally 3～10: 1, and leaching time is generally between 10～20 minutes;
6) leach liquor is carried out removal of impurities and handle, get cleansing soln; Described leach liquor is the manganous sulfate leach liquor in the above-mentioned steps, but if in step 4), carried out sulfur dioxide gas is fed the operation of the leach liquor of low-grade manganese oxide ore, then manganese oxide leach liquor behind the feeding sulfurous gas and manganous sulfate leach liquor should be filtered, mix, the mixed solution to gained carries out the removal of impurities processing again; When carrying out the removal of impurities processing, can adopt the barium sulphide removal of impurities, the weight ratio of barium sulphide that is added and manganous carbonate or manganese oxide ore is generally 0.1～5: 100;
8) with the scavenging solution evaporation concentration, crystallization under 80～100 ℃ temperature obtains MnSO
4H
2O.
The present invention is from the method for low-grade manganese carbonate ore and manganese oxide reclaim(ed) sulfuric acid manganese, be that the mode that adopts the vitriol oil to strengthen roasting makes that manganese is selectively converted to solubility manganous sulfate salt in the mineral, calcining is directly used water extraction, the leach liquor evaporative crystallization directly obtains manganous sulfate, its production process is comparatively simple, and the rate of recovery of manganous sulfate is higher; And bake the sulfurous gas that sulfuric acid excessive in the technology resolves into, can be used for further leaching manganese oxide mineral, so both realized the maximum utilization of reaction reagent, prevented that again sulfurous gas from escaping the environment dirt that will cause and mixing, whole process of production is except that a small amount of leached mud discharging, not having any waste gas and waste water produces, it is the production technique of an environmental protection, and it is that feedstock conversion becomes manganous sulfate that this technology not only can directly adopt low-grade manganous carbonate and manganese oxide raw ore, the calcining that obtains in its production technique, also directly water logging goes out separating of impurity such as can realizing the iron sial and manganese, valuable elements such as the cobalt nickel in the mineral have entered leach liquor, can further recycle, reaction process does not have any waste gas and discharging of waste liquid yet simultaneously.Therefore, adopting chemical mineral processing method of the present invention is the novel method that low-grade manganese resource practical large-scale is recycled, and also is simultaneously the new way that reaches the comprehensive utilization ratio that improves low-grade manganese resource utilization and associated resources.
(4) embodiment:
Embodiment 1:
1), levigate to below-100 orders with the manganous carbonate concentrate (manganese content is about 21%) of the big new manganese ore in Guangxi;
2) take by weighing the manganous carbonate concentrate of 50 grams after levigate and restrain FeSO with 5
4H
2O ground and mixed in mortar is even, obtains mixture;
3) adding 30 gram weight concentration at the said mixture material again is 98% the vitriol oil;
4) material that mixes is put into the 100ml quartz boat at 500 ℃ of following roasting 1h of tube furnace; And the sulfur dioxide gas that roasting process produces fed in the leach liquor of low-grade manganese oxide ore, at 50 ℃ of manganese that leach down in the low-grade manganese oxide ores of temperature, can reach more than 98% to the leaching yield of manganese oxide ore manganese;
5) calcining that obtains of sulfation at 60 ℃ of following agitation leach 20min, obtains the manganous sulfate infusion solution of pH=6～7 with 200ml water; With a small amount of (20ml) water washing 3 times, the concentration of manganese concentration and cobalt in the analysis filtrate is calculated manganese recovery ratio and is about 95%, and the leaching yield of cobalt is about 82%;
6) the manganese oxide leach liquor and the manganous sulfate leach liquor that will feed behind the sulfurous gas filters, mixes, and obtains mixed solution;
7) adopting barium sulphide to carry out removal of impurities to mixed solution handles, gets cleansing soln; The weight ratio of barium sulphide that is added and manganous carbonate or manganese oxide ore was generally 0.5: 100;
8) with the scavenging solution evaporation concentration, crystallization under 80 ℃ temperature obtains MnSO
4H
2O.
Embodiment 2:
1), levigate to below-100 orders with Guangxi Gui Bei manganese oxide raw ore (manganese content is about 24%);
2) taking by weighing the manganese oxide raw ore of 50 grams after levigate and 2, to restrain pyrite ground and mixed in mortar even, obtains mixture;
3) adding 28 gram weight concentration at the said mixture material again is 80% the vitriol oil;
4) material that mixes is put into the 100ml quartz boat 600 ℃ of following roastings of tube furnace 40 minutes; And the sulfur dioxide gas that roasting process produces fed in the leach liquor of low-grade manganese oxide ore, at 60 ℃ of manganese that leach down in the low-grade manganese oxide ores of temperature, can reach more than 96% to the leaching yield of manganese oxide ore manganese;
5) calcining that obtains of sulfation at 90 ℃ of following agitation leach 20min, obtains the manganous sulfate infusion solution of PH=6～7 with 200ml water; With 20ml water washing 3 times, the concentration of manganese concentration and cobalt in the analysis filtrate is calculated manganese recovery ratio and is about 96%, and the leaching yield of cobalt is about 86%;
6) the manganese oxide leach liquor and the manganous sulfate leach liquor that will feed behind the sulfurous gas filters, mixes, and obtains mixed solution;
7) adopting barium sulphide to carry out removal of impurities to mixed solution handles, gets cleansing soln; The weight ratio of barium sulphide that is added and manganous carbonate or manganese oxide ore was generally 0.5: 100;
8) with the scavenging solution evaporation concentration, crystallization under 100 ℃ temperature obtains MnSO
4H
2O.
Embodiment 3:
1), levigate to below-100 orders with the manganous carbonate concentrate (manganese content is about 20%) of the big new manganese ore in Guangxi;
2) taking by weighing the manganous carbonate concentrate of 50 grams after levigate and 3, to restrain pyrite ground and mixed in mortar even, obtains mixture;
3) adding 32 gram weight concentration at the said mixture material again is 98% the vitriol oil;
4) material that mixes is put into the 100ml quartz boat 550 ℃ of following roastings of tube furnace 30 minutes;
5) calcining that obtains of sulfation at 60 ℃ of following agitation leach 10min, obtains the manganous sulfate infusion solution of pH=6～7 with 200ml water; With 20ml water washing 3 times, the concentration of manganese concentration and cobalt in the analysis filtrate is calculated manganese recovery ratio and is about 96%, and the leaching yield of cobalt is about 84%;
6) add barium sulphide at the manganous sulfate leach liquor and carry out the removal of impurities processing, get cleansing soln; The weight ratio of barium sulphide that is added and manganous carbonate or manganese oxide ore was generally 0.3: 100;
7) with the scavenging solution evaporation concentration, crystallization under 80 ℃ temperature obtains MnSO
4H
2O.
Claims (9)
1, a kind of method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese, its step is as follows:
1) low-grade manganese carbonate and manganese oxide raw ore is levigate;
2) levigated manganese carbonate ore or manganese oxide ore are mixed with pyrite or ferrous sulfate;
3) in the material that mixes, add the vitriol oil;
4) material that mixes is put into and is carried out roasting;
5) calcining that obtains of sulfation adopts 20～90 ℃ of water extractions, obtains the manganous sulfate infusion solution of pH=6～7;
6) infusion solution is carried out removal of impurities and handle, get cleansing soln;
7) with the scavenging solution evaporation concentration, crystallization under 80～100 ℃ temperature obtains MnSO
4H
2O.
2, the method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese according to claim 1, it is characterized in that: the sulfur dioxide gas that roasting process in the step 4) is produced feeds in the leach liquor of low-grade manganese oxide ore, leaches the manganese in the low-grade manganese oxide ore; And will feed manganese oxide leach liquor behind the sulfurous gas and the manganous sulfate leach liquor filters, mixes, obtain mixed solution; Then mixed solution is carried out the processing of step 6) and step 7).
3, the method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese according to claim 1 and 2 is characterized in that: manganous carbonate and manganese oxide raw ore are levigate to below-100 orders.
4, the method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese according to claim 1 and 2 is characterized in that: step 2) in, the weight ratio of manganous carbonate or manganese oxide ore and pyrite or ferrous sulfate is 1: 0.05～0.19.
5, the method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese according to claim 1 and 2, it is characterized in that: in the step 3), manganous carbonate or manganese oxide ore and vitriolic weight ratio are 1: 0.4～1.0.
6, the method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese according to claim 1 and 2 is characterized in that: in the step 4), the temperature of roasting is 100 ℃～600 ℃; Roasting time is 0.5～3 hour.
7, the method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese according to claim 1 and 2, it is characterized in that: in the step 7), adopt barium sulphide to carry out removal of impurities, the weight ratio of barium sulphide that is added and manganous carbonate or manganese oxide ore is 0.1～5: 100.
8, the method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese according to claim 1 and 2 is characterized in that: in the step 5), be to leach 10～20 minutes under 3～10: 1 the condition at solvent and solute weight ratio with calcining.
9, the method from low-grade manganese carbonate and manganese oxide ore reclaim(ed) sulfuric acid manganese according to claim 2 is characterized in that: in the step 4), leach manganese in the low-grade manganese oxide ores down 20～60 ℃ of temperature, to the manganese oxide ore leaching yield greater than 90%.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100436332C (en) * | 2006-11-08 | 2008-11-26 | 孙光辉 | Continuous conduit method for producing manganese sulfate |
| CN101914684A (en) * | 2010-08-24 | 2010-12-15 | 湖南广义科技有限公司 | Method for harmless treatment and comprehensive utilization of manganese metallurgical leached residue |
| CN103014320A (en) * | 2012-12-07 | 2013-04-03 | 中信大锰矿业有限责任公司 | Method for preparing manganese sulfate by using sulfur-containing carbonaceous manganese carbonate ore |
| CN101716556B (en) * | 2010-01-11 | 2013-04-24 | 花垣县强桦矿业有限责任公司 | Floating and enriching method of low-grade manganese dioxide ore |
| CN103613141A (en) * | 2013-12-12 | 2014-03-05 | 徐万铭 | Method for co-production of feed manganese sulfate by using wastewater of crude indium production |
| CN108728634A (en) * | 2018-06-08 | 2018-11-02 | 中南大学 | The method for innocent treatment of electrolytic manganese residues |
| CN108910958A (en) * | 2018-07-17 | 2018-11-30 | 重庆上甲电子股份有限公司 | A method of manganese sulfate is produced using aniline reduction electrolytic manganese anode mud |
| CN110819797A (en) * | 2019-11-21 | 2020-02-21 | 武汉理工大学 | Carbonate mineral leaching method |
| CN111111419A (en) * | 2020-01-02 | 2020-05-08 | 四川大学 | Method for removing high-concentration SO in flue gas by utilizing manganese carbonate ore2Method for producing manganese sulfate solution |
| CN115043434A (en) * | 2022-08-03 | 2022-09-13 | 贵州金瑞新材料有限责任公司 | Manganese sulfate production system based on manganese oxide ore |
| CN115386722A (en) * | 2022-08-30 | 2022-11-25 | 苏州金之翼新材料科技有限公司 | Method for separating rare earth and iron from pyrite roasting neodymium iron boron waste |
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| GB1405038A (en) * | 1973-07-26 | 1975-09-03 | Mitsui Mining & Smelting Co | Process for the continuous preparation of aqueous manganous sulphate solution for use in the production of electrolytic manganese dioxide |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100436332C (en) * | 2006-11-08 | 2008-11-26 | 孙光辉 | Continuous conduit method for producing manganese sulfate |
| CN101716556B (en) * | 2010-01-11 | 2013-04-24 | 花垣县强桦矿业有限责任公司 | Floating and enriching method of low-grade manganese dioxide ore |
| CN101914684A (en) * | 2010-08-24 | 2010-12-15 | 湖南广义科技有限公司 | Method for harmless treatment and comprehensive utilization of manganese metallurgical leached residue |
| CN103014320A (en) * | 2012-12-07 | 2013-04-03 | 中信大锰矿业有限责任公司 | Method for preparing manganese sulfate by using sulfur-containing carbonaceous manganese carbonate ore |
| CN103613141A (en) * | 2013-12-12 | 2014-03-05 | 徐万铭 | Method for co-production of feed manganese sulfate by using wastewater of crude indium production |
| CN108728634A (en) * | 2018-06-08 | 2018-11-02 | 中南大学 | The method for innocent treatment of electrolytic manganese residues |
| CN108910958A (en) * | 2018-07-17 | 2018-11-30 | 重庆上甲电子股份有限公司 | A method of manganese sulfate is produced using aniline reduction electrolytic manganese anode mud |
| CN110819797A (en) * | 2019-11-21 | 2020-02-21 | 武汉理工大学 | Carbonate mineral leaching method |
| CN111111419A (en) * | 2020-01-02 | 2020-05-08 | 四川大学 | Method for removing high-concentration SO in flue gas by utilizing manganese carbonate ore2Method for producing manganese sulfate solution |
| CN111111419B (en) * | 2020-01-02 | 2021-03-23 | 四川大学 | Method for removing high-concentration SO in flue gas by utilizing manganese carbonate ore2Method for producing manganese sulfate solution |
| CN115043434A (en) * | 2022-08-03 | 2022-09-13 | 贵州金瑞新材料有限责任公司 | Manganese sulfate production system based on manganese oxide ore |
| CN115386722A (en) * | 2022-08-30 | 2022-11-25 | 苏州金之翼新材料科技有限公司 | Method for separating rare earth and iron from pyrite roasting neodymium iron boron waste |
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