CN108251663A - Utilize the method for tapioca reducing leaching manganese oxide ore - Google Patents
Utilize the method for tapioca reducing leaching manganese oxide ore Download PDFInfo
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- CN108251663A CN108251663A CN201711262557.2A CN201711262557A CN108251663A CN 108251663 A CN108251663 A CN 108251663A CN 201711262557 A CN201711262557 A CN 201711262557A CN 108251663 A CN108251663 A CN 108251663A
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- manganese
- manganese oxide
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B47/00—Obtaining manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
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Abstract
The invention belongs to manganese metallurgical technology fields, and in particular to a kind of method using tapioca reducing leaching manganese oxide ore, this method use tapioca as reducing agent, the reducing leaching manganese oxide ore in aqueous sulfuric acid medium；Reducing leaching is carried out to manganese oxide ore using this method, the cost of tapioca used is low, and source is wide, not only reduces leaching cost and Reducton Leaching of Pyrolusite speed is fast, efficient, manganese leaching rate is high, manganese leaching rate reaches more than 92%.And the relatively simple efficiency influence on follow-up electrolysis process of the less ingredient of leachate impurity content that the method using the present invention using tapioca reducing leaching manganese oxide ore obtains is small.
Description
Technical field
The invention belongs to manganese metallurgical technology fields, and in particular to a kind of side using tapioca reducing leaching manganese oxide ore
Method.
Background technology
Manganese ore is one of important basic raw material of industrial sector, in recent years, with increasing rapidly for China's steel industry,
China's manganese alloy and electrolytic manganese industry yield have ranked first in the world, and manganese has as a kind of strategic resource in national economy
Irreplaceable critical role.But at present, a large amount of electrolytic manganese industry is mainly using manganese carbonate ore as raw material, with electrolysis
The fast development of manganese industry, the resource reserve of manganese carbonate ore increasingly decline with the grade of ore, and very limits constrain electrolytic manganese
The sustainable development of industry, it is therefore, economical, reasonable, efficient to mitigate promoter manganese shortage using manganese oxide ore resource
The problem of bringing, and can ensure the sustainable development of electrolytic manganese industry, research and develop the efficient reducing leaching of manganese oxide ore
Method is the hot subject of China's manganese field of metallurgy.
In recent years, it is Low grade manganese ore, oceanic multi-metal manganese nodule, secondary with the sharp increase of manganese systems product consumption
Promoter manganese etc. is able to study and utilize as important resource, and economically, discomfort shares traditional pyrometallurgical smelting process.
Simultaneously, because fire reduction process energy consumption is big, environmental pollution is serious so that the wet reducing extract technology development of manganese oxide ore is fast
Speed.The essence of leaching is the valuable constituent in ore, concentrate or half product to be made preferentially to dissolve out using appropriate solvent, be able to
It is detached with gangue.The leaching process of manganese ore is a heterogeneous reaction process, and reaction speed depends on the area of boundary, reaction
The mass transfer velocity of the concentration of reactant and reactant on boundary on interface.MnO2It is very steady in acid and alkaline medium
It is fixed, it will not be dissolved under general condition, but his oxidizing potential is higher, when there is reducing agent, MnO2It can react, be reduced
Into Mn2+It is dissolved in leachate.Therefore, the wet reducing of manganese oxide ore is leached using suitable reducing agent most important.Also
Originality reducing agent that is strong, cheap, deriving from a wealth of sources is increasingly being applied to the reducing leaching technique of manganese oxide ore.Research is such as
What is economical, reasonably using Low grade manganese ore, the technical issues of particularly solving its reducing process the bottleneck that property, to slow
It solves current China's manganese resource contradiction in short supply, ensure manganese systems product industry value chain, and the hair of Economy of Western Areas
Exhibition all has highly important strategic importance.
Manganese oxide ore wet reducing leaching process research key technology be exactly search out it is a kind of meet industrial requirements also
Former agent, some researchers use sulfur dioxide gas as reducing agent.It is directly raw that patent CN1161936 discloses sulfur dioxide gas
Sulfur dioxide gas is passed through reaction generation manganese sulfate solution in manganese dioxide ore pulp, then routinely by the method for producing manganese sulfate
Method handles to obtain final products, and manganese leaching rate is up to more than 98%.But having side reaction in the reaction process, generation connects
Two manganese sulfates and the quality for influencing product.Patent CN101898798 discloses a kind of method for preparing manganese sulfate, in titanium dioxide
Sulphur, which leaches, adds in auxiliary agent and oxidant in low-grade manganese dioxide ore system, can effectively inhibit and eliminate the life of manganous dithionate
Into.
Biomass be a kind of source it is wide, without toxic element, cheap renewable resource, in acid condition can
It is enough that substance of the hydrolysis generation with reproducibility occurs, then with the main component MnO in manganese oxide ore2It is anti-that redox occurs
Should, achieve the purpose that leaching of manganese.And leaching process does not need to high-temperature roasting, consersion unit is simple, and equipment investment expense is low, and ring
Border pollution is small, is one of high-efficiency reducing agent that wet reducing leaches manganese oxide ore.Some researchers are had studied using biomass also
The leaching method of former agent.As patent CN1884099 discloses the side that blackstrap-sulfate reduction leaches manganese ore and prepare manganese sulfate
Method makees reducing agent using trade waste molasses alcohol waste liquid, is stirred to react to obtain leachate, the leaching of manganese at 40~100 DEG C
Extracting rate is about 93%.Patent CN101886168 discloses a kind of extract technology of semi-manganese oxide ore, utilizes trade waste cassava
Alcohol effluent makees reducing agent, and it is about 90% that 1~6 hour manganese leaching rate is stirred to react at a temperature of 70~98 DEG C.In addition, one
A little researchers also reported the result of study for leaching manganese oxide ore in acid condition using corncob, in manganese oxide ore/corn
Core mass ratio is 10: 3, and sulfuric acid concentration 1.9mol/L, 85 DEG C of extraction temperature, extraction time is under conditions of 1 hour, manganese
Leaching rate is up to 92.8%.Since biomass resource type is various, composition is complicated, and source is unstable, in leached mud organic matter and
Soluble manganese content is high, and ammonium acetate is complicated, after this limits the stability of leaching process and affects to a certain extent
The efficiency of continuous electrolysis process.
Patent CN1126245, CN1126246, CN1126247 and CN1155586 individually disclose the anti-of manganese oxide ore
Bad hematic acid, arylamine, polyhydroxy aromatic and phenol acids reduction leaching method, for marine manganese nodule raw material, sulfuric acid at normal temperatures and pressures
Reducing leaching manganese in medium, manganese leaching rate reach more than 98%.But these organic reducing agent costs are big, high toxicity.
In conclusion in the leaching process of manganese oxide ore, reducing agent is its key problem in technology.Existing method is in product matter
Amount, reducing agent source and cost etc. there are problems that in varying degrees some shortcomings and, need research and development more efficient
Reducton Leaching of Pyrolusite new method, to meet the active demand of China electrolytic manganese production.
Invention content
The problem of the present invention seeks to be directed to existing manganese oxide ore wet reducing leaching process and the one kind provided
Economical and efficient and the method using tapioca reducing leaching manganese oxide ore of environmental protection.Manganese oxide ore is gone back using this method
Original leaches, and the cost of tapioca used is low, and source is wide, not only reduces and leaches cost and Reducton Leaching of Pyrolusite speed
Spend fast, efficient, manganese leaching rate height.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method using tapioca reducing leaching manganese oxide ore includes the following steps：
（1）Take the concentrated sulfuric acid and ammonium sulfate prepare initial acidity be 200g/L, the mixed solution that ammonium sulfate concentrations are 100g/L,
After mixed solution is heated to 85~95 DEG C, tapioca is added in, acidolysis reaction is carried out under 85~95 DEG C of stirrings；
1.5-2.5 hours acidolysis time；
（2）Manganese oxide ore is crushed to more than 50 mesh, obtains manganese oxide powder, after acidolysis, adds in manganese oxide in the solution
Miberal powder, it is 8 that control pulp slurry, which consolidates mass ratio,:1~10:1；It leaches and is stirred to react 2-3 hours at 80~95 DEG C, reaction terminates
Afterwards, it is separated by filtration to obtain manganese sulfate leachate.
The above-mentioned method using tapioca reducing leaching manganese oxide ore, the dosage of the tapioca is according to wood
Sweet potato starch：Mn in manganese oxide ore4+The ratio of mass ratio >=0.35 of content be added.
The above-mentioned method using tapioca reducing leaching manganese oxide ore, the manganese oxide ore are with manganese dioxide
For the manganese raw material of main valuable constituent, manganese dioxide mass content is 10%~90%；As pyrolusite, psilomelane, hausmannite,
Braunite and manganite etc..
The method of the present invention generally carries out under normal pressure.
Beneficial effects of the present invention are：
In the research of manganese oxide ore is leached as reducing agent wet reducing based on glucose in the past, although glucose is to oxidation
The leaching effect of manganese ore is good, but relative price is higher.And the tapioca used in the present invention is at low cost, source is wide, the para arrowroot
Powder is strong by acidolysis generation hydrolysis generation organic reducing sugar reducing power, the effective reducing leaching manganese oxide ore of energy, with Portugal
Grape sugar, which is compared, has identical leaching effect, can reach certain leaching requirement.And the present invention is restored using tapioca
The method economical and efficient of manganese oxide ore and environmental protection are leached, reducing leaching, cassava used are carried out to manganese oxide ore using this method
The cost of starch is low, and source is wide, not only reduces and leaches cost and Reducton Leaching of Pyrolusite speed is fast, the leaching of efficient, manganese
Extracting rate is high, and manganese leaching rate reaches more than 92%.And the method using the present invention using tapioca reducing leaching manganese oxide ore
The obtained relatively simple efficiency on follow-up electrolysis process of the less ingredient of leachate impurity content influences small.
Specific embodiment
Embodiment 1
A kind of method using tapioca reducing leaching manganese oxide ore includes the following steps：
（1）Take the concentrated sulfuric acid (A.R) and ammonium sulfate (A.R) prepare initial acidity be 200g/L, ammonium sulfate concentrations 100g/L
Mixed solution, after mixed solution is heated to 85 DEG C, add in tapioca, under 85 DEG C of stirrings carry out acidolysis it is anti-
It should；2.5 hours acidolysis time；The dosage of tapioca is according to tapioca：Mn in manganese oxide ore4+Content mass ratio
Ratio for 0.35 is added；
（2）Manganese oxide ore is crushed to 50 mesh, obtains manganese oxide powder, after acidolysis, adds in manganese oxide powder in the solution,
It is 8 that control pulp slurry, which consolidates mass ratio,:1；It leaches and is stirred to react 3 hours at 80 DEG C, after reaction, be separated by filtration to obtain sulfuric acid
Manganese leachate；The leaching rate of manganese is 96.26%.Manganese oxide powder used is derived from thunder Manganese Ore District under Zhong Xin great Meng great Xin branch companies
Production manganese oxide powder, its composition analysis result is as shown in table 1 below after testing, aqueous data such as the following table 2 of manganese oxide powder
It is shown；The aqueous data of tapioca used are as shown in table 3 below.
Embodiment 2
A kind of method using tapioca reducing leaching manganese oxide ore includes the following steps：
（1）Take the concentrated sulfuric acid and ammonium sulfate prepare initial acidity be 200g/L, the mixed solution that ammonium sulfate concentrations are 100g/L,
After mixed solution is heated to 90 DEG C, tapioca is added in, acidolysis reaction is carried out under 90 DEG C of stirrings；The acidolysis time
2 hours；The dosage of tapioca is according to tapioca：Mn in manganese oxide ore4+Content mass ratio be 0.40 ratio
It is added；
（2）Manganese oxide ore is crushed to 100 mesh, obtains manganese oxide powder, after acidolysis, adds in manganese oxide ore in the solution
Powder, it is 9 that control pulp slurry, which consolidates mass ratio,:1；It leaches and is stirred to react 2.5 hours at 90 DEG C, after reaction, be separated by filtration
To manganese sulfate leachate；The leaching rate of manganese is 97.22%.Manganese oxide powder used is derived from thunder under Zhong Xin great Meng great Xin branch companies
Manganese Ore District production manganese oxide powder, the after testing Tables 1 and 2 in its composition analysis result and its aqueous data such as embodiment 1
It is shown；The aqueous data of tapioca used are as shown in the table 3 in embodiment 1.
Embodiment 3
A kind of method using tapioca reducing leaching manganese oxide ore includes the following steps：
（1）Take the concentrated sulfuric acid and ammonium sulfate prepare initial acidity be 200g/L, the mixed solution that ammonium sulfate concentrations are 100g/L,
After mixed solution is heated to 95 DEG C, tapioca is added in, acidolysis reaction is carried out under 95 DEG C of stirrings；The acidolysis time
1.5 hour；The dosage of tapioca is according to tapioca：Mn in manganese oxide ore4+Content mass ratio be 0.41 ratio
What example was added；
（2）Manganese oxide ore is crushed to more than 50 mesh, obtains manganese oxide powder, after acidolysis, adds in manganese oxide in the solution
Miberal powder, it is 10 that control pulp slurry, which consolidates mass ratio,:1；It leaches and is stirred to react 2 hours at 95 DEG C, after reaction, be separated by filtration
To manganese sulfate leachate；The leaching rate of manganese is 97.82%.Manganese oxide powder used is derived from thunder under Zhong Xin great Meng great Xin branch companies
Manganese Ore District production manganese oxide powder, the after testing Tables 1 and 2 in its composition analysis result and its aqueous data such as embodiment 1
It is shown；The aqueous data of tapioca used are as shown in the table 3 in embodiment 1.
Embodiment 4
A kind of method using tapioca reducing leaching manganese oxide ore includes the following steps：
（1）Take the concentrated sulfuric acid and ammonium sulfate prepare initial acidity be 200g/L, the mixed solution that ammonium sulfate concentrations are 100g/L,
After mixed solution is heated to 85 DEG C, tapioca is added in, acidolysis reaction is carried out under 85 DEG C of stirrings；The acidolysis time
2.5 hour；The dosage of tapioca is according to tapioca：Mn in manganese oxide ore4+Content mass ratio be 0.37 ratio
What example was added；
（2）Manganese oxide ore is crushed to more than 50 mesh, obtains manganese oxide powder, after acidolysis, adds in manganese oxide in the solution
Miberal powder, it is 9 that control pulp slurry, which consolidates mass ratio,:1；It leaches and is stirred to react 2 hours at 95 DEG C, after reaction, be separated by filtration
To manganese sulfate leachate；The leaching rate of manganese is 96.60%.Manganese oxide powder used is derived from thunder under Zhong Xin great Meng great Xin branch companies
Manganese Ore District production manganese oxide powder, the after testing Tables 1 and 2 in its composition analysis result and its aqueous data such as embodiment 1
It is shown；The aqueous data of tapioca used are as shown in the table 3 in embodiment 1.
Embodiment 5
A kind of method using tapioca reducing leaching manganese oxide ore includes the following steps：
（1）Take the concentrated sulfuric acid and ammonium sulfate prepare initial acidity be 200g/L, the mixed solution that ammonium sulfate concentrations are 100g/L,
After mixed solution is heated to 90 DEG C, tapioca is added in, acidolysis reaction is carried out under 90 DEG C of stirrings；The acidolysis time
2.5 hour；The dosage of the tapioca is according to tapioca：The mass ratio of the content of Mn4+ is in manganese oxide ore
What 0.36 ratio was added；
（2）Manganese oxide ore is crushed to 150 mesh, obtains manganese oxide powder, after acidolysis, adds in manganese oxide ore in the solution
Powder, it is 10 that control pulp slurry, which consolidates mass ratio,:1；It leaches and is stirred to react 2.5 hours at 95 DEG C, after reaction, be separated by filtration
To manganese sulfate leachate；The leaching rate of manganese is 96.41%.Manganese oxide powder used is derived from thunder under Zhong Xin great Meng great Xin branch companies
Manganese Ore District production manganese oxide powder, the after testing Tables 1 and 2 in its composition analysis result and its aqueous data such as embodiment 1
It is shown；The aqueous data of tapioca used are as shown in the table 3 in embodiment 1.
Claims (3)
- A kind of 1. method using tapioca reducing leaching manganese oxide ore, it is characterised in that：Include the following steps：（1）Take the concentrated sulfuric acid and ammonium sulfate prepare initial acidity be 200g/L, the mixed solution that ammonium sulfate concentrations are 100g/L, After mixed solution is heated to 85~95 DEG C, tapioca is added in, acidolysis reaction is carried out under 85~95 DEG C of stirrings； 1.5-2.5 hours acidolysis time；（2）Manganese oxide ore is crushed to more than 50 mesh, obtains manganese oxide powder, after acidolysis, adds in manganese oxide in the solution Miberal powder, it is 8 that control pulp slurry, which consolidates mass ratio,:1~10:1；It leaches and is stirred to react 2-3 hours at 80~95 DEG C, reaction terminates Afterwards, it is separated by filtration to obtain manganese sulfate leachate.
- 2. the method using tapioca reducing leaching manganese oxide ore according to claim 1, which is characterized in that described The dosage of tapioca be according to tapioca：Mn in manganese oxide ore4+Content mass ratio >=0.35 ratio carry out Addition.
- 3. the method using tapioca reducing leaching manganese oxide ore according to claim 1, which is characterized in that described Manganese oxide ore be manganese raw material using manganese dioxide as main valuable constituent, manganese dioxide mass content is 10%~90%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108928853A (en) * | 2018-08-15 | 2018-12-04 | 广西锰华新能源科技发展有限公司 | A kind of comprehensive reutilization method of manganese ore leaching slag |
| CN114162872A (en) * | 2021-12-31 | 2022-03-11 | 湖南烯富环保科技有限公司 | Method for preparing battery-grade manganese sulfate from manganese oxide ore |
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| CN108928853A (en) * | 2018-08-15 | 2018-12-04 | 广西锰华新能源科技发展有限公司 | A kind of comprehensive reutilization method of manganese ore leaching slag |
| CN114162872A (en) * | 2021-12-31 | 2022-03-11 | 湖南烯富环保科技有限公司 | Method for preparing battery-grade manganese sulfate from manganese oxide ore |
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