CN102616773A - Method for purifying medium-carbon flake graphite to obtain high-purity graphite - Google Patents
Method for purifying medium-carbon flake graphite to obtain high-purity graphite Download PDFInfo
- Publication number
- CN102616773A CN102616773A CN201210102671XA CN201210102671A CN102616773A CN 102616773 A CN102616773 A CN 102616773A CN 201210102671X A CN201210102671X A CN 201210102671XA CN 201210102671 A CN201210102671 A CN 201210102671A CN 102616773 A CN102616773 A CN 102616773A
- Authority
- CN
- China
- Prior art keywords
- graphite
- carbon sheet
- kish
- hydrochloric acid
- high purity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a method for purifying medium-carbon flake graphite to obtain high-purity graphite. The method comprises the following steps: 1) selecting raw materials: selecting an alkaline matter, the medium-carbon flake graphite and hydrochloric acid according to the weight ratio of 2-3.5: 10: 20-30 for later use, wherein the concentration of hydrochloric acid is 10-20% by weight; 2) adding water into the alkaline matter for dissolving to obtain an alkaline solution, then uniformly mixing the medium-carbon flake graphite with the alkaline solution, further placing in a tubular furnace, introducing high-purity nitrogen, reacting at the temperature of 800-1000 DEG C for 1-3 hours, then cooling to room temperature, filtering, and washing with distilled water till the pH of filtrate is 7.0; 3) uniformly mixing the filtrate obtained in the step 2) with hydrochloric acid, stirring and reacting at the temperature of 20-80 DEG C for 1-3 hours, then filtering, and washing with the distilled water till the pH of the filtrate is 7.0; and 4) drying the filtrate obtained the step 3) till the water content is less than 0.2% to obtain the high-purity graphite. By adopting the method provided by the invention, the content of solid carbon in the medium-carbon graphite can be improved to 99.9%, which is the level of high-purity graphite; and the method further has the advantages of simple process, high production efficiency, low equipment investment and low cost.
Description
Technical field
The present invention relates to the graphite new material technology field, particularly relating to a kind of is the preparation method that 90% ~ 94% middle kish carbon sheet graphite purifies to 99.9% above high purity graphite with carbon content.
Background technology
Natural flake graphite is through behind the beneficiation enrichment, and grade can't satisfy industrial needs about about 90%-95%, thereby needs further to purify, and makes fixed carbon content reach the high-carbon level 98% or more respectively or reaches high-purity grade more than 99.9%.Graphite after purifying like this can be processed into soft graphite series product, serial aquadag goods, plumbago crucible, Graphite Electrodes, graphite cathode material etc., and its range of application can be expanded greatly.
The method of purification of graphite mainly contains alkali acid system, hydrofluoric acid method, chlorinating roasting, pyroprocess.Purity was high after pyroprocess was purified, but because its temperature of reaction high (being generally 2700 ℃ ~ 3500 ℃), therefore quite high to the conversion unit requirement, energy consumption is also high, is not suitable for carrying out industrialization promotion.Hydrofluoric acid method refining effect is better, but hydrofluoric acid has stronger volatility and corrodibility, is unfavorable for industrial application.Chlorinating roasting causes very big destruction owing to need to use virose chlorine to environment.The alkali acid system is the technology of comparative maturity, uses very extensive.The principle of purifying is sodium hydroxide and graphite to be mixed calcine, and at high temperature compositions such as the impurity in the graphite such as silicate, quartz react with sodium hydroxide, generate the water glass of solubility, and usefulness is washed and is removed to reach the purpose of desiliconization then; The oxide compounds of another part impurity such as metal etc. through still being retained in the graphite behind the alkali fusion, leach the product after the desiliconization with hydrochloric acid, make its metallic compound that is converted into solubility, again through filter, washing realizes and the separating of graphite.It is the graphite products more than 99% that the alkali acid system can obtain fixed carbon content, but the purity of utilizing this method to obtain graphite products does not at present all reach more than 99.9%.
Summary of the invention
The technical problem that the present invention will solve is: provide a kind of middle kish carbon sheet graphite is purified to the method for high purity graphite, this method can effectively be removed the impurity in the graphite, and the fixed carbon content of graphite is reached more than 99.9%.
The present invention solves the problems of the technologies described above the technical scheme of being taked to be:
A kind of middle kish carbon sheet graphite is purified to the method for high purity graphite, it is characterized in that it may further comprise the steps:
1) choosing of raw material: according to alkaline matter: middle kish carbon sheet graphite: the mass ratio of hydrochloric acid be 2-3.5:10:20-30 choose alkaline matter, middle kish carbon sheet graphite, and hydrochloric acid subsequent use, the concentration of wherein said hydrochloric acid is 10-20wt%;
2) alkaline matter is dissolved in water obtains alkaline solution, then middle kish carbon sheet graphite and alkaline solution mixing are placed in the tube furnace, feed high pure nitrogen; Under 800-1000 ℃ of condition, react 1-3h; Be cooled to room temperature afterwards, filter, be washed with distilled water to the pH to 7.0 of filtrating;
3) with step 2) behind the filtrating that obtains and the hydrochloric acid mixing under 20-80 ℃ of condition stirring reaction 1-3h, filter afterwards, be washed with distilled water to filtrating pH to 7.0;
4) filtrating that step 3) is obtained dry to moisture content less than 0.2%, promptly obtain fixed carbon content and reach the high purity graphite more than 99.9%.
In the such scheme, the fixed carbon content of said middle kish carbon sheet graphite is 90-94%, and particle diameter is+50 orders ~-100 orders.
The purity of the high pure nitrogen that feeds in the such scheme, said step 2) is 99.99%.
In the such scheme, the stir speed (S.S.) in the said step 3) is 200 ~ 1000 rev/mins.
In the such scheme, the bake out temperature in the said step 3) is 100-110 ℃.
In the such scheme, said alkaline matter is a sodium hydroxide.
Beneficial effect of the present invention is:
Adopt alkali fusion-acid wash under the nitrogen protection atmosphere of the present invention, can the fixed carbon content of middle kish carbon sheet graphite be increased to the level of 99.9% high purity graphite, effectively remove wherein silicate and iron contamination, added value of product improves greatly; In addition, this technology is simple, advanced, easy handling, and production efficiency is high, and facility investment is few, and is with low cost, and graphite products purity is high, can satisfy the requirement of high purity graphite.
Embodiment
Below in conjunction with embodiment the present invention is done further description, certain following embodiment should not be construed as limitation of the present invention.
Embodiment 1:
A kind of middle kish carbon sheet graphite is purified to the method for high purity graphite, it may further comprise the steps:
1) choosing of raw material: according to alkaline matter: middle kish carbon sheet graphite: the mass ratio of hydrochloric acid be 3.5:10:20 choose sodium hydroxide (being alkaline matter), middle kish carbon sheet graphite, and hydrochloric acid subsequent use; The concentration of wherein said hydrochloric acid is 10wt%; The fixed carbon content of kish carbon sheet graphite is 90% in said, and particle diameter is+50 orders;
2) sodium hydroxide is dissolved in water obtains alkaline solution, with the stirring of sizing mixing behind middle kish carbon sheet graphite and the alkaline solution mixing, process the mud shape then, change in the alumina crucible; Crucible is put into tube furnace, and feeding purity is 99.99% high pure nitrogen, is warming up to 1000 ℃ of insulation 1h, is cooled to room temperature, filters, with 5-10 pH to 7.0 to filtrating of distilled water wash;
3) with step 2) behind the filtrating that obtains and the hydrochloric acid mixing under 80 ℃ of conditions stirring reaction 3h, 200 rev/mins of stir speed (S.S.)s are filtered afterwards, with distilled water wash 5-10 time to the pH to 7.0 that filtrates;
4) filtrating that step 3) is obtained put into 100 ℃ of air dry ovens dry to moisture content less than 0.2%, promptly obtain high purity graphite.
According to the ash content and the fixed carbon content of GB GB/T3521-95 method mensuration high purity graphite sample, obtaining its fixed carbon content is 99.94%.
Embodiment 2:
A kind of middle kish carbon sheet graphite is purified to the method for high purity graphite, it may further comprise the steps:
1) choosing of raw material: according to alkaline matter: middle kish carbon sheet graphite: the mass ratio of hydrochloric acid be 2.5:10:25 choose sodium hydroxide (being alkaline matter), middle kish carbon sheet graphite, and hydrochloric acid subsequent use; The concentration of wherein said hydrochloric acid is 15wt%; The fixed carbon content of kish carbon sheet graphite is 92% in said, and particle diameter is+80 orders;
2) sodium hydroxide is dissolved in water obtains alkaline solution, with the stirring of sizing mixing behind middle kish carbon sheet graphite and the alkaline solution mixing, process the mud shape then, change in the alumina crucible; Crucible is put into tube furnace, and feeding purity is 99.99% high pure nitrogen, is warming up to 950 ℃ of insulation 3h, is cooled to room temperature, filters, with 5-10 pH to 7.0 to filtrating of distilled water wash;
3) with step 2) behind the filtrating that obtains and the hydrochloric acid mixing under 60 ℃ of conditions stirring reaction 2h, 500 rev/mins of stir speed (S.S.)s are filtered afterwards, with distilled water wash 5-10 time to the pH to 7.0 that filtrates;
4) filtrating that step 3) is obtained put into 105 ℃ of air dry ovens dry to moisture content less than 0.2%, promptly obtain high purity graphite.
According to the ash content and the fixed carbon content of GB GB/T3521-95 method mensuration high purity graphite sample, obtaining its fixed carbon content is 99.92%.
Embodiment 3:
A kind of middle kish carbon sheet graphite is purified to the method for high purity graphite, it may further comprise the steps:
1) choosing of raw material: according to alkaline matter: middle kish carbon sheet graphite: the mass ratio of hydrochloric acid be 2:10:30 choose sodium hydroxide (being alkaline matter), middle kish carbon sheet graphite, and hydrochloric acid subsequent use; The concentration of wherein said hydrochloric acid is 20wt%; The fixed carbon content of kish carbon sheet graphite is 94% in said, and particle diameter is-100 orders;
2) sodium hydroxide is dissolved in water obtains alkaline solution, with the stirring of sizing mixing behind middle kish carbon sheet graphite and the alkaline solution mixing, process the mud shape then, change in the alumina crucible; Crucible is put into tube furnace, and feeding purity is 99.99% high pure nitrogen, is warming up to 800 ℃ of insulation 2h, is cooled to room temperature, filters, with 5-10 pH to 7.0 to filtrating of distilled water wash;
3) with step 2) behind the filtrating that obtains and the hydrochloric acid mixing under 20 ℃ of conditions stirring reaction 1h, 1000 rev/mins of stir speed (S.S.)s are filtered afterwards, with distilled water wash 5-10 time to the pH to 7.0 that filtrates;
4) filtrating that step 3) is obtained put into 110 ℃ of air dry ovens dry to moisture content less than 0.2%, promptly obtain high purity graphite.
According to the ash content and the fixed carbon content of GB GB/T3521-95 method mensuration high purity graphite sample, obtaining its fixed carbon content is 99.91%.
Each raw material that the present invention is cited, and the bound value of each raw material, with and interval value, can both realize the present invention; And the bound value of each processing parameter (like temperature, time etc.), with and interval value, can both realize the present invention, do not enumerate embodiment one by one at this.
Claims (6)
1. one kind purifies to the method for high purity graphite with middle kish carbon sheet graphite, it is characterized in that it may further comprise the steps:
1) choosing of raw material: according to alkaline matter: middle kish carbon sheet graphite: the mass ratio of hydrochloric acid be 2-3.5:10:20-30 choose alkaline matter, middle kish carbon sheet graphite, and hydrochloric acid subsequent use, the concentration of wherein said hydrochloric acid is 10-20wt%;
2) alkaline matter is dissolved in water obtains alkaline solution, then middle kish carbon sheet graphite and alkaline solution mixing are placed in the tube furnace, feed high pure nitrogen; Under 800-1000 ℃ of condition, react 1-3h; Be cooled to room temperature afterwards, filter, be washed with distilled water to the pH to 7.0 of filtrating;
3) with step 2) behind the filtrating that obtains and the hydrochloric acid mixing under 20-80 ℃ of condition stirring reaction 1-3h, filter afterwards, be washed with distilled water to filtrating pH to 7.0;
4) filtrating that step 3) is obtained dry to moisture content less than 0.2%, promptly obtain fixed carbon content and reach the high purity graphite more than 99.9%.
2. as claimed in claim 1 middle kish carbon sheet graphite is purified to the method for high purity graphite, it is characterized in that, said in the fixed carbon content of kish carbon sheet graphite be 90-94%, particle diameter is+50 orders ~-100 orders.
3. as claimed in claim 1 middle kish carbon sheet graphite is purified to the method for high purity graphite, it is characterized in that said step 2) in the purity of the high pure nitrogen that feeds be 99.99%.
4. as claimed in claim 1 middle kish carbon sheet graphite is purified to the method for high purity graphite, it is characterized in that the stir speed (S.S.) in the said step 3) is 200 ~ 1000 rev/mins.
5. as claimed in claim 1 middle kish carbon sheet graphite is purified to the method for high purity graphite, it is characterized in that the bake out temperature in the said step 3) is 100-110 ℃.
6. as claimed in claim 1 middle kish carbon sheet graphite is purified to the method for high purity graphite, it is characterized in that said alkaline matter is a sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210102671XA CN102616773A (en) | 2012-04-10 | 2012-04-10 | Method for purifying medium-carbon flake graphite to obtain high-purity graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210102671XA CN102616773A (en) | 2012-04-10 | 2012-04-10 | Method for purifying medium-carbon flake graphite to obtain high-purity graphite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102616773A true CN102616773A (en) | 2012-08-01 |
Family
ID=46557059
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210102671XA Pending CN102616773A (en) | 2012-04-10 | 2012-04-10 | Method for purifying medium-carbon flake graphite to obtain high-purity graphite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102616773A (en) |
Cited By (5)
| 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 |
| CN108751188A (en) * | 2018-08-08 | 2018-11-06 | 青岛领军节能与新材料研究院 | A kind of graphite purification method |
| CN109336104A (en) * | 2018-11-23 | 2019-02-15 | 北京航空航天大学 | A kind of low temperature graphite purification method |
| CN109574003A (en) * | 2018-12-28 | 2019-04-05 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of method of ultrasonic wave auxiliary alkali acid system purification graphite |
| CN112093798A (en) * | 2020-10-29 | 2020-12-18 | 哈尔滨理工大学 | Outfield-assisted graphite rapid purification method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031512A (en) * | 1987-08-10 | 1989-03-08 | 化学工业部天津化工研究院 | Liquid phase method for purifying national graphite |
| RU2141449C1 (en) * | 1998-04-15 | 1999-11-20 | Общество с ограниченной ответственностью "ГраЭН" | Method of purification of natural graphite |
-
2012
- 2012-04-10 CN CN201210102671XA patent/CN102616773A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031512A (en) * | 1987-08-10 | 1989-03-08 | 化学工业部天津化工研究院 | Liquid phase method for purifying national graphite |
| RU2141449C1 (en) * | 1998-04-15 | 1999-11-20 | Общество с ограниченной ответственностью "ГраЭН" | Method of purification of natural graphite |
Non-Patent Citations (2)
| Title |
|---|
| 《新型炭材料》 20100228 葛鹏等 "加碱焙烧浸出法制备高纯石墨" 第22-27页 1-6 第25卷, 第1期 * |
| 葛鹏等: ""加碱焙烧浸出法制备高纯石墨"", 《新型炭材料》 * |
Cited By (6)
| 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 |
| CN108751188A (en) * | 2018-08-08 | 2018-11-06 | 青岛领军节能与新材料研究院 | A kind of graphite purification method |
| CN109336104A (en) * | 2018-11-23 | 2019-02-15 | 北京航空航天大学 | A kind of low temperature graphite purification method |
| CN109574003A (en) * | 2018-12-28 | 2019-04-05 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of method of ultrasonic wave auxiliary alkali acid system purification graphite |
| CN112093798A (en) * | 2020-10-29 | 2020-12-18 | 哈尔滨理工大学 | Outfield-assisted graphite rapid purification method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103359736A (en) | Method for purifying and preparing silicon carbide powder from crystalline silicon cutting waste mortar | |
| CN102616773A (en) | Method for purifying medium-carbon flake graphite to obtain high-purity graphite | |
| WO2017181759A1 (en) | Method for manufacturing anhydrous lithium chloride using lithium-containing wastewater | |
| WO2017215011A1 (en) | Ion sieve material, preparation method therefor and using method thereof | |
| CN103738990B (en) | A kind of method utilizing crystal aluminum chloride to produce aluminum oxide | |
| CN101885498A (en) | Method for preparing high-purity magnesium sulfate | |
| CN103991882A (en) | Method for preparing potassium fluoride by using fluoride in liquid phase of wet process phosphoric acid | |
| CN110963518A (en) | Method for preparing nano aluminum oxide by using fly ash | |
| CN110294473B (en) | Preparation process for purifying microcrystalline graphite by organic acid catalysis | |
| CN106348319A (en) | Method for utilizing serpentine for preparing high-purity magnesium oxide | |
| CN104129781A (en) | In-situ nitrogen-doped porous graphene and preparation method thereof | |
| CN104340967A (en) | High stability graphite purification method | |
| CN102774817A (en) | Process for recovery and purification of hexagonal boron nitride in cubic boron nitride synthetic tailings | |
| CN103420403A (en) | Process for preparing lithium fluoride | |
| CN101734667B (en) | Process for producing precipitated white carbon black by silicon tetrachloride | |
| CN109665534B (en) | Method for preparing mesoporous silicon oxide by using fly ash acid leaching residue | |
| CN108516565B (en) | Method for preparing P-type zeolite molecular sieve by using aluminum calcium powder reaction slag | |
| CN103803622A (en) | Method using aluminum chloride hexahydrate dehydration to prepare anhydrous aluminum chloride | |
| CN109482133B (en) | Method for preparing adsorbing material by using waste liquid of Hummers method | |
| CN108557881B (en) | Method for producing high-purity bismuth oxide from bismuth-containing material | |
| CN109319754A (en) | A kind of aluminum ions method in reduction phosphoric acid by wet process | |
| CN105776259A (en) | Production method for high-purity magnesium fluoride polycrystals for ultraviolet-level single crystal growth | |
| CN105217674A (en) | The preparation method of the pure nitrocalcite of a kind of top grade | |
| CN105621468B (en) | A kind of preparation method of high purity aluminium oxide | |
| CN104843696A (en) | Method for preparing high-carbon graphite by using middle-carbon crystalline flake graphite as raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120801 |