CN106517177A - Method for purifying graphite by using high-pressure alkaline leaching - Google Patents
Method for purifying graphite by using high-pressure alkaline leaching Download PDFInfo
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- CN106517177A CN106517177A CN201610970864.5A CN201610970864A CN106517177A CN 106517177 A CN106517177 A CN 106517177A CN 201610970864 A CN201610970864 A CN 201610970864A CN 106517177 A CN106517177 A CN 106517177A
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- graphite
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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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Abstract
The invention discloses a method for purifying graphite by using high-pressure alkaline leaching, belongs to the field of preparation of high-purity graphite, and aims to solve the problems that a large amount of waste acid and waste alkali can be produced and high consumption is caused in an existing production process. The method comprises the following steps: performing ore grinding on flake graphite concentrates till the particle size is of 300 meshes and over 90 percent, preparing a sodium hydroxide alkaline solution with the concentration of 6 mol/L, mixing the alkaline solution and the graphite concentrates subjected to ore grinding according to a ratio of 6 to 1 to obtain a mixed solution, putting the mixed solution into a high-pressure kettle, controlling the temperature at 250 DEG C, preserving the heat under a continuously stirring state for 1 hour, obtaining leachate at the end of leaching, filtering the leachate, putting an obtained graphite mixture into alkali, washing till the graphite mixture is neutralized, adding about 40 to 50 percent of hydrochloric acid with the concentration of 31 percent into the washed graphite mixture to enable reaction between residual impurities in the graphite and the hydrochloric acid, performing acid leaching and filtering, performing acid washing on the graphite till the graphite is neutralized, and dehydrating and drying the obtained graphite to obtain the high-purity graphite.
Description
Technical field
The present invention relates to a kind of method that utilization high pressure base leaches purification graphite, belongs to the preparation field of high purity graphite.
Background technology
High purity graphite is the material with carbon element that a kind of technology content is very high, application potential is very big, in semiconductor industry, photovoltaic
The traditional fields such as industry, lithium ion battery, space flight, military project, display of new generation and emerging field are all widely used, graphite
Elementary step of the industry in China still in industrialization.
Graphite purification is exactly to take effective means to remove impurity therein.Graphite purification includes chemical purification and Physical
Purification, chemical purification have alkali acid system, hydrogen fluoride, chlorinating roasting；Physical purification has high temperature method.
The advantage of alkali acid system is：One-time investment is few, product grade is higher, equipment is easily realized, highly versatile, and which has the disadvantage
Energy consumption is big, response time length, equipment corrosion are serious, produce a large amount of waste water.The high purity graphite fixed carbon that Fluohydric acid. method of purification is obtained
Content reaches as high as 99.95%.The advantage of hydrogen fluoride is：Dust removal rate is high, and product grade is high, the performance shadow to graphite products
Ring little, energy consumption low.Have the disadvantage that Fluohydric acid. has severe toxicity and severe corrosive, it is necessary to have strict safety prevention measure, the waste water of generation
Could discharge after needing strict process.Carbon content is fixed using the high purity graphite that chlorinating roasting is obtained and reaches as high as 99.95%.
Chlorinating roasting have energy-conservation, purification efficiency it is high (>98%) the advantages of, response rate is high.But chlorine is poisonous, corrosivity are strong, it is desirable to
Strict seal, must deal carefully with to tail gas, while chlorine is relatively costly, and chlorination process there is also defect in itself, produce
Product purity is only capable of reaching 99.95% reluctantly.And extremely unstable, its popularization and application is limited to a certain extent.High temperature method can be by
Graphite purification such as further improves process conditions to 99.99%, and purity can reach 99.995%.The advantage of high temperature method is：Product
Very high purity, has the disadvantage equipment investment at most, and energy consumption is big, and production cost is high, and working condition is strict, also limit which and applies model
Enclose.
Country's tradition alkali acid system (《The As-Is analysis of domestic and international graphite purification technology》Li Zhiyuan) be using graphite in it is miscellaneous
Matter (silicate etc.) more than 500 DEG C at a high temperature of react with sodium hydroxide, a part is generated and is dissolved in the product of water, quilt
Water logging goes out to remove, and oxide of other impurity, such as ferrum etc. is neutralized with hydrochloric acid after alkali fusion, and generation is dissolved in iron chloride of water etc.,
Removed by washing.SiO2The Na for generating is reacted with NaOH2SiO3.Water soluble, in subsequent water logging, major part is removed
Go.In addition, during alkali soluble, except generating Na2SiO3.[A1 (OH)] can be also generated, it can also be dissolved in water, remove in water logging
Go.The method is applied to containing the less graphite concentrate of Muscovitum.In production technology, as the addition of soda acid can produce substantial amounts of giving up
Sour salkali waste, due to high temperature alkali fuse, consumes the substantial amounts of energy.
The content of the invention
The present invention in order to solve in existing production technology, as the addition of soda acid can produce substantial amounts of spent acid salkali waste, due to
High temperature alkali fuse consumes the problem of the substantial amounts of energy, there is provided a kind of method that what method was simple, of reduced contamination prepare high purity graphite.
The present invention is achieved by the following technical programs：
A kind of method that utilization high pressure base leaches purification graphite, is characterized in that, the method includes following step：
Crystalline flake graphite concentrate is carried out ore grinding process by step one so as to which granularity reaches more than 300 mesh more than 90%；
Step 2, sodium hydroxide lye of the configuration concentration more than or equal to 6mol/L, by sodium hydroxide lye and graphite concentrate
It is 6 in proportion:1 mixing；
Mixed liquid is placed in autoclave, by temperature control at 250 DEG C, 1 is incubated in the state of being stirred continuously
Hour；
Gained leachate is filtered；
Step 3, graphite mixture obtained by step 2 is added water carries out neutralizing treatment operation, is washed to neutrality；
Graphite mixture obtained by step 3 is added the hydrochloric acid that concentration is more than 15%, makes the residue in graphite by step 4
Impurity and hydrochloric acid reaction, the addition of hydrochloric acid is the 40%～50% of graphite, carries out Acid leaching；
Step 5, after the completion of step 4 reaction, adds water into acid elution operation, is washed to neutrality；
Step 6, graphite obtained by step 5 is carried out being dehydrated, is dried and is obtained high purity graphite, graphite grade 99.9% with
On.
Beneficial effects of the present invention：The method technological operation is simple, and original 500 DEG C are leached with high-temperature alkali, 250 are optimized for
DEG C condition of high voltage, has saved energy consumption, and the high pressure base acid system after improving has been more conducive to the leaching of impurity, and leaching rate is high, prepares
Go out high purity graphite impurity content few, excellent performance；For sewage yield, traditional acid-base method produces large amount of sewage, pollution
Larger, the sewage quantity produced by this technique is less, all can recycle, and reduces the pollution of environment.
The present invention is improved for alkali acid system, is leached with high pressure base and is replaced alkali roasting, has been saved the energy, reduced into
This, and soda acid washing liquid be neutralized process do not produce spent acid salkali waste, all recycle.
Description of the drawings
Fig. 1 is the method process chart that a kind of utilization high pressure base of the invention leaches purification graphite.
Specific embodiment
The present invention is further described with reference to instantiation.
As shown in figure 1, a kind of utilization high pressure base leaches the method for purifying graphite, the method includes following step：
Crystalline flake graphite concentrate is carried out ore grinding process by step one so as to which granularity reaches more than 300 mesh more than 90%.
Step 2, sodium hydroxide lye of the configuration concentration more than or equal to 6mol/L, by sodium hydroxide lye and graphite concentrate
It is 6 in proportion:1 mixing.
Mixed liquid is placed in autoclave, by temperature control at 250 DEG C, 1 is incubated in the state of being stirred continuously
Hour.
Gained leachate is filtered.
Step 3, graphite mixture obtained by step 2 is added water carries out neutralizing treatment operation, is washed to neutrality.Described
The neutralizing treatment water of neutralizing treatment operation is retained, and carries out follow-up neutralisation treatment.
Graphite mixture obtained by step 3 is added the hydrochloric acid that concentration is more than 15%, makes the residue in graphite by step 4
Impurity and hydrochloric acid reaction, the addition of hydrochloric acid is the 40%～50% of graphite, carries out Acid leaching.Its Acid leaching liquid is reused.
Step 5, after the completion of step 4 reaction, adds water into acid elution operation, is washed to neutrality.Acid elution is made
In industry in acid elution water and the neutralizing treatment water and and place of settling postpone, the liquid circulation after all processing is utilized.
Step 6, graphite obtained by step 5 is carried out being dehydrated, is dried and is obtained high purity graphite, graphite grade 99.9% with
On.
A kind of method that utilization high pressure base leaches purification graphite, specific embodiment are as follows：
1) graphite raw material typical composition such as table used by：
| Element | Fixed carbon | S | CaO | Al2O3 | MgO | SiO2 | Fe |
| Content % | 95.64 | 0.0007 | 0.35 | 0.30 | 0.18 | 0.85 | 0.58 |
2) the production technology operation of high purity graphite
(1) ore grinding：By crystalline flake graphite concentrate ore grinding to granularity be 300 mesh (>90%).
(2) high pressure base is leached
Sodium hydroxide lye of the configuration concentration for 6mol/L, is 6 by alkali liquor and ore deposit in proportion:1 mixing, liquid after mixing
Body, is placed in autoclave, by temperature control at 250 DEG C, is incubated 1 hour in the state of being stirred continuously.
Gained leachate is filtered, and gained graphite adds water carries out neutralizing treatment operation (washings retention), washs to neutrality.
(3) Ore Leaching
Graphite mixture after washing is added into 31% concentration hydrochloric acid, residual impurity and salt in graphite is made in a kettle.
Acid reaction, reaction temperature are 60 DEG C, and the response time is 1.5 hours, and the addition of hydrochloric acid is about the 40%～50% of graphite, carries out
Acid leaching (recycling of Acid leaching liquid), after the completion of Acid leaching reaction, Jing is filtered, and the graphene deionization water after filtration is washed
Wash operation (in acid elution water and neutralizing treatment water and and place of settling postpone, all recycled), by residual pickling net to neutral.
(4) graphite after pickling is carried out into centrifuge dewatering, is then dried using 120 DEG C of drying bakers, finally obtained
High purity graphite, graphite grade is more than 99.9%.
Claims (4)
1. a kind of method that utilization high pressure base leaches purification graphite, is characterized in that, the method includes following step：
Crystalline flake graphite concentrate is carried out ore grinding process by step one so as to which granularity reaches more than 300 mesh more than 90%；
Step 2, sodium hydroxide lye of the configuration concentration more than or equal to 6mol/L, by sodium hydroxide lye and graphite concentrate by than
Example is 6:1 mixing；
Mixed liquid is placed in autoclave, by temperature control at 250 DEG C, 1 hour is incubated in the state of being stirred continuously；
Gained leachate is filtered；
Step 3, graphite mixture obtained by step 2 is added water carries out neutralizing treatment operation, is washed to neutrality；
Graphite mixture obtained by step 3 is added the hydrochloric acid that concentration is more than 15%, makes the residual impurity in graphite by step 4
With hydrochloric acid reaction, the addition of hydrochloric acid is the 40%～50% of graphite, carries out Acid leaching；
Step 5, after the completion of step 4 reaction, adds water into acid elution operation, is washed to neutrality；
Step 6, graphite obtained by step 5 is carried out being dehydrated, is dried and is obtained high purity graphite, and graphite grade is more than 99.9%.
2. the method that a kind of utilization high pressure base according to claim 1 leaches purification graphite, it is characterised in that step 3 institute
The neutralizing treatment water of the neutralizing treatment operation stated is retained, and carries out follow-up neutralisation treatment.
3. the method that a kind of utilization high pressure base according to claim 1 leaches purification graphite, it is characterised in that step 4 institute
The Acid leaching stated, its Acid leaching liquid are reused.
4. the method that a kind of utilization high pressure base according to claim 2 leaches purification graphite, it is characterised in that step 5 institute
In the acid elution operation stated in acid elution water and the neutralizing treatment water and and place of settling postpone, by the liquid circulation after all processing
Utilize.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610970864.5A CN106517177A (en) | 2016-11-04 | 2016-11-04 | Method for purifying graphite by using high-pressure alkaline leaching |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107462452A (en) * | 2017-09-25 | 2017-12-12 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of method for determining crystalline flake graphite ore deposit particle size distribution characteristics |
| CN108203092A (en) * | 2018-02-06 | 2018-06-26 | 青岛晶莹石墨有限公司 | Graphite powder impurity removal process and sewage treatment process |
| CN110342508A (en) * | 2019-07-31 | 2019-10-18 | 黑龙江工业学院 | A kind of method of discharge plasma activation graphite collaborative method purification |
| CN114873592A (en) * | 2022-06-10 | 2022-08-09 | 苏州中材非金属矿工业设计研究院有限公司 | Purification process of natural graphite |
| CN115432700A (en) * | 2022-10-13 | 2022-12-06 | 苏州中材非金属矿工业设计研究院有限公司 | Efficient chemical purification and washing equipment and process for nonmetallic ore |
| CN115490230A (en) * | 2022-10-25 | 2022-12-20 | 苏州中材非金属矿工业设计研究院有限公司 | Efficient alkaline-acid purification system and process for graphite |
| US11702342B2 (en) | 2020-05-18 | 2023-07-18 | Ecograf Limited | Method of producing purified graphite |
| CN118579776A (en) * | 2024-08-06 | 2024-09-03 | 陕西汉唐森源实业发展集团有限责任公司 | Two-step alkali acid purification method of natural graphite |
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| CN101973545A (en) * | 2010-11-08 | 2011-02-16 | 昆明冶金研究院 | Method for purifying high-purity graphite |
| CN102583360A (en) * | 2012-04-16 | 2012-07-18 | 丁慧贤 | Method for purifying graphite by using microwave |
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| CN104229788A (en) * | 2014-09-24 | 2014-12-24 | 攀枝花学院 | Method for purifying high-purity graphite |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107462452A (en) * | 2017-09-25 | 2017-12-12 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of method for determining crystalline flake graphite ore deposit particle size distribution characteristics |
| CN107462452B (en) * | 2017-09-25 | 2020-07-07 | 苏州中材非金属矿工业设计研究院有限公司 | Method for measuring particle size distribution characteristics of flake graphite ore |
| CN108203092A (en) * | 2018-02-06 | 2018-06-26 | 青岛晶莹石墨有限公司 | Graphite powder impurity removal process and sewage treatment process |
| CN110342508A (en) * | 2019-07-31 | 2019-10-18 | 黑龙江工业学院 | A kind of method of discharge plasma activation graphite collaborative method purification |
| CN110342508B (en) * | 2019-07-31 | 2023-01-10 | 黑龙江工业学院 | Method for purifying graphite by discharge plasma activation and chemical method |
| US11702342B2 (en) | 2020-05-18 | 2023-07-18 | Ecograf Limited | Method of producing purified graphite |
| CN114873592A (en) * | 2022-06-10 | 2022-08-09 | 苏州中材非金属矿工业设计研究院有限公司 | Purification process of natural graphite |
| CN115432700A (en) * | 2022-10-13 | 2022-12-06 | 苏州中材非金属矿工业设计研究院有限公司 | Efficient chemical purification and washing equipment and process for nonmetallic ore |
| CN115432700B (en) * | 2022-10-13 | 2024-02-20 | 苏州中材非金属矿工业设计研究院有限公司 | Efficient chemical purification and washing equipment and process for nonmetallic ores |
| CN115490230A (en) * | 2022-10-25 | 2022-12-20 | 苏州中材非金属矿工业设计研究院有限公司 | Efficient alkaline-acid purification system and process for graphite |
| CN115490230B (en) * | 2022-10-25 | 2024-02-20 | 苏州中材非金属矿工业设计研究院有限公司 | System and process for purifying graphite by high-efficiency alkali acid method |
| CN118579776A (en) * | 2024-08-06 | 2024-09-03 | 陕西汉唐森源实业发展集团有限责任公司 | Two-step alkali acid purification method of natural graphite |
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Application publication date: 20170322 |
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