CN110272073A - A kind of ferrous disulfide pickling method of purification - Google Patents
A kind of ferrous disulfide pickling method of purification Download PDFInfo
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- CN110272073A CN110272073A CN201910505417.6A CN201910505417A CN110272073A CN 110272073 A CN110272073 A CN 110272073A CN 201910505417 A CN201910505417 A CN 201910505417A CN 110272073 A CN110272073 A CN 110272073A
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- ferrous disulfide
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- mineral dust
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- pickling method
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention patent discloses a kind of ferrous disulfide pickling method of purification, the technical field of particular compound preparation method.A kind of ferrous disulfide pickling method of purification includes the following steps: the ore containing ferrous disulfide being ground into mineral dust by grinding device；Mineral dust is put into container, hydrochloric acid is then added into container, and heat to the solution in container, is stirred continuously mineral dust during heating；Solution after reaction is outwelled, tap water is then added into container and mineral dust is stirred repeatedly；Tap water is changed to pure water, is then stirred repeatedly again；Then the pure water in container is extracted out by vacuum pump, the mineral dust after pure water discharge is ferrous disulfide powder.Other substances can be introduced by overcoming existing ferrous disulfide production technology using technical solution of the present invention, and the problem of lead to ferrous disulfide product purity is low, it can be used for the purification of ferrous disulfide.
Description
Technical field
The present invention relates to the technical field of compounds process for production thereof, in particular to a kind of ferrous disulfide pickling method of purification.
Background technique
In battery industry, lithium battery is excellent since high with energy density, voltage is high, operating temperature range is wide, the service life is long etc.
Point, by the concern and attention of more and more people.In the past more than ten years, lithium battery primary (not chargeable) and
Leading position is occupied in secondary (chargeable) Battery Market, is widely used in mobile phone, laptop and number
In the portable electronic devices such as camera.
In lithium battery, battery of lithium-iron disulphide is one kind with FeS2It lives for positive electrode active materials, by cathode of metal Li
Property material and using organic electrolyte as the one-shot battery of electrolyte.The voltage of the one-shot battery can achieve 1.5V, therefore can be with
Substitute existing frequently-used alkaline battery and as the portable energy source of ordinary consumption electronic equipment carry out using.In addition, the primary electricity
Pond also has a specific discharge capacity more much higher than alkaline battery, and low temperature performance well, safety are good, light-weight, therefore its conduct
The high-power battery of a new generation, just more and more welcomed by the people, market prospects are boundless.
Primary raw material ferrous disulfide as battery of lithium-iron disulphide, and the surface of ferrous disulfide ore is often contained
Other a small amount of substances (such as fe or iron chloride) generally require in current production technology that part medicament is added to improve
The purity of product, but be introduced into after medicament and can generate environmentally harmful waste liquid in production process, and the moieties in medicament
It is difficult to reject, influence is produced on the purity of product.
Summary of the invention
The invention is intended to provide a kind of ferrous disulfide pickling method of purification, to solve existing ferrous disulfide production technology meeting
The problem of introducing other substances, and leading to ferrous disulfide product purity is low.
In order to achieve the above object, base case of the invention is as follows: a kind of ferrous disulfide pickling method of purification, including such as
Lower step: the ore containing ferrous disulfide step 1: is ground into mineral dust by grinding device；Step 2: by step 1
In mineral dust be put into container, hydrochloric acid is then added into container, and heat to the solution in container, heated
Mineral dust is stirred continuously in journey；Step 3: after the hydrochloric acid fully reacting in step 2, make container stop heating and stand one
Section time, the mineral dust after reacting are sunken to container bottom；Step 4: the solution after reacting in step 3 is outwelled, then
Tap water is added into container and mineral dust is stirred repeatedly；Step 5: the tap water in step 4 is changed to pure
Then water purification is stirred repeatedly again；Step 6: one layer of filter paper will be covered on container, and will be in container by vacuum pump
Pure water extraction, the mineral dust after pure water discharge is ferrous disulfide powder.
The principle and effect of technical solution: tiny mineral powder will be ground by grinding device containing ferrous disulfide
Subsequent reaction is convenient at end；The mineral dust after grinding is put into container again, and into container be added hydrochloric acid and to mixing after
Solution heated, hydrochloric acid can dissolve the impurity (fe) on mineral dust surface, and by heating can also accelerate salt
The reaction speed of acid and mineral dust, so as to shorten process time；A period of time is stood after reaction makes mineral dust be sunken to appearance
Device bottom, convenient for filtering out the solution after reaction；Solution in container is outwelled, tap water is then added, mineral dust is carried out instead
Multiple stirring, can wash mineral dust remained on surface or the raffinate depended on, moreover it is possible to clean the chlorination dissolved ferric iron of mineral surface
Fall；Finally the solution after cleaning is outwelled and pure water is added into container, secondary agitation, purpose are carried out to mineral dust at this time
It is repeatedly to be rinsed by pure water and cation will not be brought into during flushing；It will by vacuum pump and filter paper
Pure water in container is taken away, to improve the purity of ferrous disulfide product.
Further, the heating temperature in step 2 is 25 DEG C -100 DEG C.
Further, the heating time in step 2 is 1-5 hours.
By above-mentioned setting, the purity of ferrous disulfide can be improved by improving heating temperature or extension heating time.
Further, the volume ratio of the hydrochloric acid and mineral dust in step 2 is 1:1, and the concentration of the hydrochloric acid is
1.19g/mL.It is mixed by hydrochloric acid with mineral dust equal proportion, accelerates the dissolution of mineral dust.
Further, the mixing time of the tap water in step 3 is 10 minutes.Mine is dissolved by originally water energy
The iron chloride on stone powder surface, and the raffinate after the reacting with hydrochloric acid of mineral dust surface can be washed, pass through control punching
The time washed can ensure that the impurity on mineral dust surface is rinsed out completely.
Further, the mixing time of the pure water in step 4 is 5 minutes.Secondary punching is carried out by pure water
It washes, avoids the purity brought cation in flushing process into and influence product.
This programme the utility model has the advantages that compared with prior art, 1, this programme do not introduce new impurity, and by hydrochloric acid and from
Water can reject the other impurities in mineral dust, to improve the purity to ferrous disulfide；2, this programme is added by control
The temperature and time of heat, greatly improves the purity of product；3, this programme technological operation is simple, and equipment requirement is low, greatly
Reduce the processing cost of product.
Detailed description of the invention
Fig. 1 is a kind of process flow chart of ferrous disulfide pickling method of purification of the present invention.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
Embodiment 1:
A kind of ferrous disulfide pickling method of purification, includes the following steps:
Step 1: the ore containing ferrous disulfide is ground into the mineral dust that granularity is 80-320 mesh by grinder；
Powdered ore can increase the reaction speed between hydrochloric acid in subsequent dedoping step, improve the efficiency of operation.
Step 2: the mineral dust in step 1 is put into glassware, and hydrochloric acid (its is then added into glassware
The volume ratio of middle hydrochloric acid and mineral dust is 1:1, and the concentration of hydrochloric acid is 1.19g/mL), then the solution in glassware is carried out
The mineral dust for being heated to 95 DEG C, and being stirred continuously in solution during heating is obtained by heating the different time to solution
Arrive the result of table 1:
Table 1 (heating temperature is 95 DEG C):
| Heating time | 1 hour | 3 hours | 5 hours |
| The purity of ferrous disulfide | 96.2% | 97.8% | 98.5% |
Step 3: after the hydrochloric acid fully reacting in step 2, making glassware stop heating and standing a period of time, to
Mineral dust after reaction is sunken to container bottom.
Step 4: solution in glassware is outwelled, and tap water is added into glassware and carries out to mineral dust
It stirs repeatedly, mixing time is 10 minutes；It can be clear by the remaining hydrochloric acid of mineral dust surface institute by the repeated flushing of tap water
It washes off and washes the chlorination dissolved ferric iron on mineral dust surface, avoid influence of the hydrochloric acid residues to product purity.
Step 5: the tap water in step 4 is changed to pure water, is then stirred repeatedly again, mixing time is
5 minutes；Secondary flushing is carried out by pure water, the mineral ion brought into tap water can be rinsed out, and it will not be introduced
His ion, improves the purity of product.
Step 6: the opening of glassware is covered into upper filter paper, then passes through vacuum pump for glassware in step 5
Interior pure water extraction, the mineral dust after pure water discharge is ferrous disulfide powder.
It is compared and is found by the above method, when one timing of heating temperature, the pure of product can be improved by extending heating time
Degree, and the flushing of tap water and pure water can effectively reduce influence of other impurity to product purity in product.
Embodiment 2:
A kind of ferrous disulfide pickling method of purification, includes the following steps:
Step 1: the ore containing ferrous disulfide is ground into the mineral dust that granularity is 80-320 mesh by grinder；
Powdered ore can increase the reaction speed between hydrochloric acid in subsequent dedoping step, improve the efficiency of operation.
Step 2: the mineral dust in step 1 is put into glassware, and hydrochloric acid (its is then added into glassware
The volume ratio of middle hydrochloric acid and mineral dust is 1:1, and the concentration of hydrochloric acid is 1.19g/mL), then to the solution heating 4 in glassware
Hour and the temperature for gradually rising solution, and the mineral dust being stirred continuously in solution during heating, by adding to solution
The change of hot temperature has obtained the result of table 2:
Table 2 (heating time is 4 hours):
| Heating temperature | 25℃ | 60℃ | 100℃ |
| The purity of ferrous disulfide | 94% | 97% | 98.5% |
Step 3: after the hydrochloric acid fully reacting in step 2, making glassware stop heating and standing a period of time, to
Mineral dust after reaction is sunken to container bottom.
Step 4: solution in glassware is outwelled, and tap water is added into glassware and carries out to mineral dust
It stirs repeatedly, mixing time is 10 minutes；It can be clear by the remaining hydrochloric acid of mineral dust surface institute by the repeated flushing of tap water
It washes off and washes the chlorination dissolved ferric iron on mineral dust surface, avoid influence of the hydrochloric acid residues to product purity.
Step 5: the tap water in step 4 is changed to pure water, is then stirred repeatedly again, mixing time is
5 minutes；Secondary flushing is carried out by pure water, the mineral ion brought into tap water can be rinsed out, and it will not be introduced
His ion, improves the purity of product.
Step 6: the opening of glassware is covered into upper filter paper, then passes through vacuum pump for glassware in step 5
Interior pure water extraction, the mineral dust after pure water discharge is ferrous disulfide powder.
Compared and found by the above method, when heated between a timing, improve the pure of product by improving heating temperature
Degree, and the flushing of tap water and pure water can effectively reduce influence of other impurity to product purity in product.
Claims (6)
1. a kind of ferrous disulfide pickling method of purification, characterized by the following steps:
Step 1: the ore containing ferrous disulfide is ground into mineral dust by grinding device；
Step 2: the mineral dust in step 1 is put into container, hydrochloric acid is then added into container, and to molten in container
Liquid is heated, and is stirred continuously mineral dust during heating；
Step 3: after the hydrochloric acid fully reacting in step 2, container is made to stop heating and standing a period of time, after reacting
Mineral dust is sunken to container bottom；
Step 4: the solution after reacting in step 3 is outwelled, and tap water is then added into container and carries out to mineral dust
It stirs repeatedly；
Step 5: the tap water in step 4 is changed to pure water, is then stirred repeatedly again；
Step 6: one layer of filter paper will be covered on container, and is extracted out the pure water in container by vacuum pump, after pure water discharge
Mineral dust be ferrous disulfide powder.
2. a kind of ferrous disulfide pickling method of purification according to claim 1, it is characterised in that: described in step 2 plus
Hot temperature is 25 DEG C -100 DEG C.
3. a kind of ferrous disulfide pickling method of purification according to claim 2, it is characterised in that: described in step 2 plus
The hot time is 1-5 hours.
4. a kind of ferrous disulfide pickling method of purification according to claim 2 or 3, it is characterised in that: the institute in step 2
The volume ratio for stating hydrochloric acid and mineral dust is 1:1, and the concentration of the hydrochloric acid is 1.19g/mL.
5. a kind of ferrous disulfide pickling method of purification according to claim 1, it is characterised in that: in step 3 it is described from
The mixing time of water is 10 minutes.
6. a kind of ferrous disulfide pickling method of purification according to claim 5, it is characterised in that: described pure in step 4
The mixing time of water purification is 5 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910505417.6A CN110272073A (en) | 2019-06-12 | 2019-06-12 | A kind of ferrous disulfide pickling method of purification |
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| CN201910505417.6A CN110272073A (en) | 2019-06-12 | 2019-06-12 | A kind of ferrous disulfide pickling method of purification |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006127872A (en) * | 2004-10-28 | 2006-05-18 | Dowa Mining Co Ltd | Iron disulfide for battery and its manufacturing method |
| CN102320668A (en) * | 2011-06-03 | 2012-01-18 | 合肥工业大学 | Pyrite nano mineral material and preparation method thereof |
| CN102751489A (en) * | 2012-06-29 | 2012-10-24 | 上海交通大学 | Method for preparing anode material of lithium ion battery |
| CN103972502A (en) * | 2014-04-02 | 2014-08-06 | 芜湖浙鑫新能源有限公司 | Modified cathode material for lithium battery |
| US8877136B1 (en) * | 2012-09-05 | 2014-11-04 | Andrei Razumau | Method of producing synthesis gas from coal |
-
2019
- 2019-06-12 CN CN201910505417.6A patent/CN110272073A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006127872A (en) * | 2004-10-28 | 2006-05-18 | Dowa Mining Co Ltd | Iron disulfide for battery and its manufacturing method |
| CN102320668A (en) * | 2011-06-03 | 2012-01-18 | 合肥工业大学 | Pyrite nano mineral material and preparation method thereof |
| CN102751489A (en) * | 2012-06-29 | 2012-10-24 | 上海交通大学 | Method for preparing anode material of lithium ion battery |
| US8877136B1 (en) * | 2012-09-05 | 2014-11-04 | Andrei Razumau | Method of producing synthesis gas from coal |
| CN103972502A (en) * | 2014-04-02 | 2014-08-06 | 芜湖浙鑫新能源有限公司 | Modified cathode material for lithium battery |
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Application publication date: 20190924 |
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