CN1699156A - Preparation process for purifying graphite by liquid phase method - Google Patents
Preparation process for purifying graphite by liquid phase method Download PDFInfo
- Publication number
- CN1699156A CN1699156A CN 200410010264 CN200410010264A CN1699156A CN 1699156 A CN1699156 A CN 1699156A CN 200410010264 CN200410010264 CN 200410010264 CN 200410010264 A CN200410010264 A CN 200410010264A CN 1699156 A CN1699156 A CN 1699156A
- Authority
- CN
- China
- Prior art keywords
- graphite
- liquid phase
- phase method
- preparation technology
- strong oxidizer
- 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.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 34
- 239000010439 graphite Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000007791 liquid phase Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 235000011837 pasties Nutrition 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000007800 oxidant agent Substances 0.000 claims description 16
- 238000000746 purification Methods 0.000 claims description 15
- 238000005516 engineering process Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000008139 complexing agent Substances 0.000 claims description 11
- 229910021382 natural graphite Inorganic materials 0.000 claims description 10
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- QCGGXGCODUUTLZ-UHFFFAOYSA-N [Na].[Na].[Na].[Na] Chemical compound [Na].[Na].[Na].[Na] QCGGXGCODUUTLZ-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000007935 neutral effect Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000012535 impurity Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
Disclosed is a preparation process for purifying graphite by liquid phase method, which comprises charging water into native graphite to obtain a pasty state, charging strong oxidation agent, heating, stirring and reacting, filtering and rinshing to neutral, finally drying to obtain the high purity native graphite.
Description
Affiliated technical field
The invention belongs to the purification techniques field of graphite, that relate generally to is a kind of preparation technology of liquid phase method purification graphite.
Background technology
Graphite has critical role as a kind of industrial raw material in some special industries or high-tech area, as industry such as nuclear industry, automotive industry, spationautics, biotechnologys.Its carbon content of graphite that these industries are used must be at the high purity graphite more than 99.9%, and the carbon content of the natural graphite after the general ore dressing is up to 96%, can't satisfy the requirement of using the high purity graphite industry far away, must purify to natural graphite for this reason.
The method of purification that natural graphite is taked is to improve graphite purity with the high-temperature electric heat method at present, the high-temperature electric heat method is to utilize the resistance to elevated temperatures of graphite, be placed in the airtight high-temperature electric resistance furnace, secluding air is heated to more than 2500 ℃, make the ash volatilization in the graphite, thereby make the high purity graphite of fixed carbon more than 99.9%.Because this complex process needs to build large-scale electric furnace, power consumption is also quite big, and needs constantly to feed rare gas element, thereby with high costs.Being even more important a bit, is when graphite purity reaches 99.93%, has reached the purification limit, can't make fixed carbon content continue to improve.
Summary of the invention
Task of the present invention promptly produces thus, proposes a kind of preparation technology of liquid phase method purification graphite.Its carbon content of natural graphite of purifying with this method can reach 99.9%～99.998%, and generation technology is simple, low, the steady quality of generation cost.
The present invention finishes the technical scheme that above-mentioned task takes: add entry and make it become pasty state in natural graphite, add strong oxidizer then, the ratio of strong oxidizer and graphite is 3-15: 100, the stirring reaction of heating after filtration, is washed to neutrality, drying obtains high-purity natural graphite.
The strong oxidizer that the present invention adopts is dense HCL, dense H
2SO
4, dense HNO
3Deng, the purpose that adds strong oxidizer is to utilize the strong oxidizing property of acid, the impurity composition in the graphite is removed in dissolving.The size range of considering the natural graphite that this technology is directly used is big, to between 20 orders, and the material carbon weight range is wide at 10000 orders, and 80% all can to 99%, therefore its concentration range of oxygenant of selecting high density for use is lower than 96% reaction not exclusively more than 96%.Because the temperature during acidolysis directly has influence on the speed of acidolysis reaction, thereby its temperature of reaction is controlled at 180 ℃～220 ℃, is lower than 180 ℃, and reaction not exclusively is higher than 220 ℃, to the fast reaction speed DeGrain, causes energy dissipation.The acidolysis reaction time generally was controlled at 4～6 hours.
Because some impurity in the graphite of the present invention, as Mo, Zn, Mg etc. when carrying out acid-respons with strong oxidizer, be difficult for acidolysis, influence the carbon content of graphite, thereby can add complexing agent, react with strong oxidizer again after making itself and chelating agent reaction generate chromium complex, generate soluble substance, thereby reach the purpose of purification.The complexing agent that the present invention adds is [EDTA (a disodium salt disodium)], and the ratio of its add-on and reinforcer is 1: 1, and the ratio of strong oxidizer and complexing agent and graphite is 6-30: 100.
The water that the present invention adds can be ordinary water, also can be pure water.
Be not contain Ca when the present invention washs with what cross through ion exchange resin treatment
2+, Mg
2+, Cl
-The soluble impurity that produces behind the acidolysis reaction is removed in pure water washing Deng foreign ion, and filter cake must be washed till neutrality, to guarantee to remove the soluble impurity that produces through acidolysis reaction.
The present invention recycles after adding strong oxidizer and complexing agent through filtering filtrate.Waste collection after purifying in withdrawing can, is replenished new strong oxidizer and complexing agent, be reused for purification, both reduced cost, environmental protection again simultaneously.
Technology of the present invention is simple, not strict to ingredient requirement, be applicable to processing granularity at 10000 orders to 20 orders, each specification raw material of purity 80%～99%, and do not need specific installation and material gets final product a step to purify to 99.9～99.998% high-purity-grade natural graphite, can satisfy nuclear industry, high-tech area service requirementss such as spationautics, cost is low, steady quality.
The specific examples mode
Embodiment 1
Get natural flake graphite breeze 400kg, (material purity 85%) adds entry and (do not contain Ca with what cross through ion exchange resin treatment
2+, Mg
2+, Cl
-Pure water Deng foreign ion) 300kg, stir evenly and make it become pasty state, add HCL and EDTA (1: 1) 80kg altogether then, the 200 ℃ of stirring reactions 4.5 hours of heating, after filtration, reclaim chemical reagent 23.5kg, consume 56.5kg, filter cake is washed till neutrality, dry, obtain finished product 336kg, the rate of recovery 84%, product purity 99.95%.
Embodiment 2
Getting nodularization graphite 500kg granularity 800 orders (carbon content 96%) adds entry and (utilizes through what ion exchange resin treatment was crossed and do not contain Ca
2+, Mg
2+, Cl
-Pure water Deng foreign ion) 420kg, stir evenly and make it become pasty state, add strong oxidizer and complexing agent (1: 1) 40kg altogether then, heat 200 ℃ of stirring reactions 3.5 hours through washing and filtering, reclaim chemical reagent 5.8kg, consume the 34.2kg filter cake washing to neutral, drying obtains product purity 99.98%, obtains product 477.5kg, the rate of recovery 95.5%.
Claims (7)
1, a kind of preparation technology of liquid phase method purification graphite is characterized in that: add entry and make it become pasty state in natural graphite, add strong oxidizer then, the stirring reaction of heating after filtration, is washed to neutrality, and drying obtains high-purity natural graphite.
2, the preparation technology of liquid phase method purification graphite according to claim 1 is characterized in that: also can add complexing agent, the ratio of this complexing agent and strong oxidizer is 1: 1; The ratio of complexing agent and strong oxidizer and graphite is 6: 30: 100.
3, the preparation technology of liquid phase method purification graphite according to claim 1 and 2 is characterized in that: strong oxidizer is dense HCL, dense H
2SO
4, dense HNO
3
4, the preparation technology of liquid phase method purification graphite according to claim 1 and 2 is characterized in that: complexing agent is [EDTA (a disodium salt disodium)].
5, according to the preparation technology of claim 1 or 2 or 3 described liquid phase method purification graphite, it is characterized in that: its concentration range of oxygenant is more than 96%.
6, the preparation technology of liquid phase method purification graphite according to claim 1 and 2 is characterized in that: the acidolysis reaction temperature of strong oxidizer and graphite was controlled at 4～6 hours 180 ℃～220 ℃ times.
7, the preparation technology of liquid phase method purification graphite according to claim 2 is characterized in that: the acidolysis reaction temperature of strong oxidizer and complexing agent and graphite was controlled at 4～6 hours 180 ℃～220 ℃ times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100102641A CN1317185C (en) | 2004-05-17 | 2004-05-17 | Preparation process for purifying graphite by liquid phase method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100102641A CN1317185C (en) | 2004-05-17 | 2004-05-17 | Preparation process for purifying graphite by liquid phase method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1699156A true CN1699156A (en) | 2005-11-23 |
| CN1317185C CN1317185C (en) | 2007-05-23 |
Family
ID=35475442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100102641A Expired - Lifetime CN1317185C (en) | 2004-05-17 | 2004-05-17 | Preparation process for purifying graphite by liquid phase method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1317185C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219207A (en) * | 2011-03-25 | 2011-10-19 | 浙江合盛硅业有限公司 | Removal method for Ca from carbon material |
| CN109160511A (en) * | 2018-09-17 | 2019-01-08 | 厦门大学 | A kind of device and method of graphite purification |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001649B (en) * | 2010-11-25 | 2012-07-25 | 洛阳市冠奇工贸有限责任公司 | Purification method for high-purity natural graphite |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1020089C (en) * | 1990-11-30 | 1993-03-17 | 中国科学院西安光学精密机械研究所 | Purification of graphite |
-
2004
- 2004-05-17 CN CNB2004100102641A patent/CN1317185C/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219207A (en) * | 2011-03-25 | 2011-10-19 | 浙江合盛硅业有限公司 | Removal method for Ca from carbon material |
| CN102219207B (en) * | 2011-03-25 | 2012-10-31 | 浙江合盛硅业有限公司 | Removal method for Ca from carbon material |
| CN109160511A (en) * | 2018-09-17 | 2019-01-08 | 厦门大学 | A kind of device and method of graphite purification |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1317185C (en) | 2007-05-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113061723B (en) | Method for recovering lithium from waste lithium iron phosphate batteries and preparing iron phosphate | |
| CN102001649B (en) | Purification method for high-purity natural graphite | |
| CN105695751B (en) | A kind of purification technique of electrolytic manganese anode mud | |
| CN101362600B (en) | Method for removing boron from polysilicon by wet metallargy | |
| CN103359736A (en) | Method for purifying and preparing silicon carbide powder from crystalline silicon cutting waste mortar | |
| CN102897810B (en) | Method for producing aluminum oxide by using fly ash | |
| CN101367517B (en) | Method for preparing high pure graphite with steam heating | |
| CN106882805A (en) | A kind of micro crystal graphite purifies preparation technology | |
| CN102701198A (en) | Method for purifying natural aphanitic graphite | |
| CN110294473B (en) | Preparation process for purifying microcrystalline graphite by organic acid catalysis | |
| CN1557704A (en) | Method for purifying natural crystalline flake graphite of high purity | |
| CN111254283B (en) | Process for deeply purifying and decontaminating zinc leachate by wet method | |
| CN1317185C (en) | Preparation process for purifying graphite by liquid phase method | |
| CN111268718A (en) | Method for directly preparing mercury oxide from mercury-containing organic sludge | |
| CN108793170B (en) | Industrial silicon acid pickling process after ventilation, slagging, smelting and pretreatment | |
| CN113603119B (en) | Method for recovering lithium from waste lithium iron phosphate material | |
| CN103466667B (en) | A kind of using plasma high temperature pyrolytic cracking (HTP) prepares the method for nano magnesia | |
| CN101830484A (en) | Method for recovering lithium hydroxide from waste filtrate generated in preparation of LiFePO4 material by liquid-phase method | |
| CN107827135A (en) | A kind of preparation method of high-purity superfine alumina powder | |
| CN115340075A (en) | Method for preparing battery-grade iron phosphate by adopting iron oxide and dilute phosphoric acid | |
| CN114920299A (en) | Method for purifying manganese dioxide | |
| CN114421042A (en) | Method for recovering metal aluminum, lithium carbonate and sodium nitrate from waste lithium iron phosphate material and application thereof | |
| CN107324328A (en) | A kind of new method of purification of micro crystal graphite | |
| CN1830805A (en) | Method of preparing tribasic lead sulphate utilizing spent lead battery plate grid and connecting piece | |
| CN114853074B (en) | NaFeF production by utilizing semiconductor waste acid 3 Is a method of (2) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20070523 |