CN1616346A - Process for preparing nano graphite powder - Google Patents
Process for preparing nano graphite powder Download PDFInfo
- Publication number
- CN1616346A CN1616346A CN 200310108540 CN200310108540A CN1616346A CN 1616346 A CN1616346 A CN 1616346A CN 200310108540 CN200310108540 CN 200310108540 CN 200310108540 A CN200310108540 A CN 200310108540A CN 1616346 A CN1616346 A CN 1616346A
- Authority
- CN
- China
- Prior art keywords
- graphite
- graphite powder
- colloidal sol
- preparing nano
- nano
- 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 64
- 238000004519 manufacturing process Methods 0.000 title description 2
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 38
- 239000010439 graphite Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 239000010936 titanium Substances 0.000 claims abstract description 3
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 239000000523 sample Substances 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 239000008151 electrolyte solution Substances 0.000 claims description 5
- 206010013786 Dry skin Diseases 0.000 claims description 3
- 239000008399 tap water Substances 0.000 claims description 3
- 235000020679 tap water Nutrition 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract 2
- 230000008021 deposition Effects 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000002003 electrode paste Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention discloses ultrasonic electrolysis process of preparing graphite powder. The graphite electrode inside filtering plastic net as positive electrode and stainless steel or titanium plate as negative electrode are soaked inside water electrolyte in electrolytic bath and power supply is applied for ultrasonic electrolysis to obtain graphite gel; and graphite gel is processed through natural deposition, filtering and low temperature drying to obtain nanometer graphite powder of 100 nm below size. The present invention has the features of low power consumption, high efficiency and high product purity.
Description
Technical field
The present invention relates to graphite, relate in particular to a kind of preparation process of graphite powder, more particularly, the present invention relates to a kind of method for preparing Nano graphite powder.
Background technology
Graphite Powder 99 is a kind of widely used material, can be used as the raw material of cast material, refractory materials, dyestuff, electrode paste etc.According to the difference that graphite material is required, also there is very big difference in the particle diameter of Graphite Powder 99.
Nano graphite powder is the type material of technology such as high conduction, heat conduction, high lubricated, latent type, shielding battery, and the preparation Nano graphite powder is the developing direction of carbon materials.
In the prior art, there is several different methods can obtain the Graphite Powder 99 of ultrafine powder, as disclosed preparation of superfine graphite powder among the patent publication No. CN1244495A: use jets collision and auxiliary physical influence to pulverize, make purity height, graphite granule that impurity is few, and the superfine graphite yield of median size＜2um is improved greatly.But the graphite powder particle diameter that uses this method to obtain does not reach nano level, is restricted on some purposes.
In addition, also have report to utilize the TNT explosive to come the research (as XI AN JIAOTONG UNIVERSITY Subject Index, in July, 2003, the pass brocade is clear etc.) of detonation synthesis of nano Graphite Powder 99.But, use these method energy consumptions and cost is higher, complex process, and in preparation process, may have instability, the unmanageable situation of result.
In patent publication No. is in two patents of CN1378975 and CN1378976, discloses a kind of method and a kind of method with preparing nano graphite carbon powder from nano graphite sol of preparing nano graphite carbon sol with dual graphite electrodes respectively.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing Nano graphite powder that need not any coating agent, controllable granularity system, described method adopts ultrasonic electrolytic process to prepare, and this method comprises:
(1) is filled in plastic filter screen with Graphite Powder 99 or is positive pole with the Graphite Electrodes, with stainless steel plate or titanium plate is negative pole, it is in the electrolyzer of electrolytic solution that the two poles of the earth are immersed in water, ultrasonic electrolysis is carried out in energising, regularly insert ultra-sonic dispersion in the electrolyzer, obtain the ultrasonic electrolysis oxidation nanometer graphite colloidal sol of 3-5WT% with ultrasonic probe;
(2), filter and obtain nano-graphite colloidal sol with graphite colloidal sol natural sedimentation certain hour.
(3) adopt the dry dry method of low temperature that the dry thing of nano-graphite colloidal sol is ground into fine powder, be the Graphite Powder 99 below the 100NM.
Further, the electrolytic condition for preparing the method for Nano graphite powder of the present invention is: all-wave or half-wave rectified current 2-10A, voltage during electrolysis electrolytic oxidation 40-60 hour, inserted with ultrasonic probe every 3-5 hour in the electrolyzer ultra-sonic dispersion 10-30 minute between 4-10V.Power supply adopts all-wave or half-wave, and electrolytic efficiency improves.
In the method for the invention, the electrolytic solution that uses can be pure water, tap water, distilled water or deionized water.Select for use which kind of water to require according to difference to decide to Nano graphite powder purity.
In the method for the invention, the time of graphite colloidal sol natural sedimentation is between 10-30 hour.
In the method for the invention, adopt filter paper that graphite colloidal sol is filtered, the granularity of control Nano graphite powder obtains granularity and more segments the narrower nano-graphite colloidal sol of cloth.This graphite colloidal sol is placed sediment-free generation half a year.
In the method for the invention, adopt 45 ℃ of-52 ℃ of cold dryings that the dry thing of nano-graphite colloidal sol is ground into the following graphite fine powder of 100NM.
Method of the present invention is regularly inserted in the electrolyzer with ultrasonic probe and is carried out ultra-sonic dispersion in electrolytic process, can quicken electrolytic oxidation, slows down precipitation and further pulverizes Graphite Powder 99.
Method of the present invention is filled in the plastic filter screen Graphite Powder 99 as anodal, or with Graphite Electrodes as positive pole, need not separators.
The present invention compares with the disclosed technology of prior art, have less energy-consumption, high-level efficiency, cost is low, purity is high, impurity is few characteristics, and need not any coating agent, controllable granularity system, therefore processing method is easy, reliability is high, be suitable for plant-scale production, has good economic benefit and social benefit.
Embodiment
Embodiment 1
The first step, with the Graphite Powder 99 of particle diameter about 0.8mm, be filled in diameter 30MM, long 120MM, thick 0.5-1MM, in the plastic filter screen more than 500 orders, compress the back for anodal, can be anodal also with Graphite Electrodes, with the stainless steel of 2 * 30 * 120MM is negative pole, they are immersed in the tap water is in single groove electrolyzer of electrolytic solution, by all-wave or half-wave rectified current 2-7A, voltage control is between 4-10V, and temperature is controlled at 30 ℃-70 ℃, electrolytic oxidation 48 hours, insert in the electrolyzer ultra-sonic dispersion with ultrasonic probe every 3-5 hour 20 minutes, obtain the ultrasonic electrolysis oxidation nanometer graphite colloidal sol of 3-5WT%.
Second step, when granular graphite during at 3-5WT%, graphite colloidal sol is carried out natural sedimentation, learn from else's experience graphite colloidal sol after the natural sedimentation in 10 hours, the diameter that adopts Hangzhou Paper Co., Ltd of Xinhua is that two circle board qualitative filter papers of 11cm filter to such an extent that granularity is more segmented the narrower nano-graphite colloidal sol of cloth, and this graphite colloidal sol is placed sediment-free half a year.
The 3rd step, adopt 45 ℃ of-52 ℃ of cold dryings that the dry thing of nano-graphite colloidal sol is ground into fine powder, be the Graphite Powder 99 below the 100NM.
Claims (7)
1. a method for preparing Nano graphite powder is characterized in that, it adopts ultrasonic electrolytic process to prepare, and comprising:
(1) is filled in plastic filter screen with Graphite Powder 99 or is positive pole with the Graphite Electrodes, with stainless steel plate or titanium plate is negative pole, the two poles of the earth are immersed in the electrolyzer that contains electrolytic solution, ultrasonic electrolysis is carried out in energising, regularly insert ultra-sonic dispersion in the electrolyzer, obtain the ultrasonic electrolysis oxidation nanometer graphite colloidal sol of 3-5WT% with ultrasonic probe;
(2), filter and obtain nano-graphite colloidal sol with graphite colloidal sol natural sedimentation certain hour.
(3) adopt cold drying that the dry thing of nano-graphite colloidal sol is ground into fine powder, obtain Nano graphite powder.
2. the method for preparing Nano graphite powder according to claim 1, it is characterized in that, electrolytic condition is: all-wave or half-wave rectified current 2-10A, electrolytic oxidation 40-60 hour, inserted with ultrasonic probe every 3-5 hour in the electrolyzer ultra-sonic dispersion 10-30 minute.
3. the method for preparing Nano graphite powder according to claim 1 is characterized in that the voltage during electrolysis is between 4-10V.
4. the method for preparing Nano graphite powder according to claim 1 is characterized in that, electrolytic solution is pure water, tap water, distilled water or deionized water.
5. the method for preparing Nano graphite powder according to claim 1 is characterized in that the natural sedimentation time is between 10-30 hour.
6. the method for preparing Nano graphite powder according to claim 1 is characterized in that, adopts filter paper that graphite colloidal sol is filtered.
7. the method for preparing Nano graphite powder according to claim 1 is characterized in that, adopts 45 ℃ of-52 ℃ of cold dryings, and the dry thing of nano-graphite colloidal sol is ground into the following graphite fine powder of 100NM.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108540 CN1274591C (en) | 2003-11-10 | 2003-11-10 | Process for preparing nano graphite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108540 CN1274591C (en) | 2003-11-10 | 2003-11-10 | Process for preparing nano graphite powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1616346A true CN1616346A (en) | 2005-05-18 |
| CN1274591C CN1274591C (en) | 2006-09-13 |
Family
ID=34758619
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310108540 Expired - Fee Related CN1274591C (en) | 2003-11-10 | 2003-11-10 | Process for preparing nano graphite powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1274591C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249218A (en) * | 2010-09-15 | 2011-11-23 | 北京奈艾斯新材料科技有限公司 | Method for quickly precipitating and drying nano graphite sol |
| CN103172058A (en) * | 2013-03-11 | 2013-06-26 | 同济大学 | Method for preparing three-dimensional netty graphene |
| CN103395777A (en) * | 2013-08-07 | 2013-11-20 | 大同市普朔科技有限责任公司 | Preparation method of nano-graphite carbon powder |
| CN106544689A (en) * | 2016-10-03 | 2017-03-29 | 北京奈艾斯新材料科技有限公司 | A kind of method that utilization mineral carbon prepares nano carbon sol |
| CN104760949B (en) * | 2014-01-08 | 2017-04-05 | 奈创科技股份有限公司 | Graphene generating means |
| CN106676563A (en) * | 2017-01-11 | 2017-05-17 | 肇庆学院 | Ultrasonic electrolytic preparation method for carboxylated carbon nanosheet |
| CN107500285A (en) * | 2017-09-30 | 2017-12-22 | 湖南国盛石墨科技有限公司 | The preparation method of superfine graphite |
| CN109092218A (en) * | 2018-09-03 | 2018-12-28 | 曹明辉 | A kind of nano-graphite colloidal sol preparation facilities and preparation method |
-
2003
- 2003-11-10 CN CN 200310108540 patent/CN1274591C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249218B (en) * | 2010-09-15 | 2013-07-03 | 北京奈艾斯新材料科技有限公司 | Method for quickly precipitating and drying nano graphite sol |
| CN102249218A (en) * | 2010-09-15 | 2011-11-23 | 北京奈艾斯新材料科技有限公司 | Method for quickly precipitating and drying nano graphite sol |
| CN103172058A (en) * | 2013-03-11 | 2013-06-26 | 同济大学 | Method for preparing three-dimensional netty graphene |
| CN103172058B (en) * | 2013-03-11 | 2015-01-14 | 同济大学 | Method for preparing three-dimensional netty graphene |
| CN103395777A (en) * | 2013-08-07 | 2013-11-20 | 大同市普朔科技有限责任公司 | Preparation method of nano-graphite carbon powder |
| CN103395777B (en) * | 2013-08-07 | 2014-07-30 | 大同市普朔科技有限责任公司 | Preparation method of nano-graphite carbon powder |
| CN104760949B (en) * | 2014-01-08 | 2017-04-05 | 奈创科技股份有限公司 | Graphene generating means |
| CN106544689A (en) * | 2016-10-03 | 2017-03-29 | 北京奈艾斯新材料科技有限公司 | A kind of method that utilization mineral carbon prepares nano carbon sol |
| CN106676563A (en) * | 2017-01-11 | 2017-05-17 | 肇庆学院 | Ultrasonic electrolytic preparation method for carboxylated carbon nanosheet |
| CN106676563B (en) * | 2017-01-11 | 2018-08-10 | 肇庆学院 | A kind of ultrasonic electrolysis preparation method of carboxylated carbon nanosheet |
| CN107500285A (en) * | 2017-09-30 | 2017-12-22 | 湖南国盛石墨科技有限公司 | The preparation method of superfine graphite |
| CN109092218A (en) * | 2018-09-03 | 2018-12-28 | 曹明辉 | A kind of nano-graphite colloidal sol preparation facilities and preparation method |
| CN109092218B (en) * | 2018-09-03 | 2023-11-21 | 曹明辉 | Nanometer graphite sol preparation device and preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1274591C (en) | 2006-09-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1172404C (en) | Method for recovering metal from used Li ion cell | |
| CN1274591C (en) | Process for preparing nano graphite powder | |
| CN107628609B (en) | Method for manufacturing graphene with controllable layer number and graphene | |
| JP5949663B2 (en) | Method for producing indium hydroxide powder, method for producing indium oxide powder, and sputtering target | |
| CN111470499A (en) | Method for electrochemically preparing graphene | |
| CN103276412A (en) | Method for preparing copper or nickel powder and electrolysis device based on same | |
| CN112110466B (en) | Method for removing iron impurities in fly ash and intermediate product thereof | |
| CN109706467B (en) | Method for preparing high-activity indium oxide by electrolysis | |
| CN110359062A (en) | The method for preparing high purity indium | |
| CN100342060C (en) | Preparation of superfine metal oxide by electrolytic method | |
| CN109609978B (en) | Method for electrodepositing flaky zinc in alkaline medium | |
| CN103866352A (en) | Producing method of electrolytic copper powder | |
| CN108707920B (en) | Method for preparing manganese dioxide through photoelectrochemistry metallurgy | |
| JP6048329B2 (en) | Method for producing indium hydroxide powder and method for producing indium oxide powder | |
| CN105683089B (en) | indium hydroxide powder and indium oxide powder | |
| CN103422124A (en) | Preparation of nanometer silver sol through pulse type electrode method | |
| CN116315213A (en) | Disassembly and recycling process of lithium iron phosphate battery | |
| CN110863216B (en) | Method for preparing high-purity indium through step cyclone electrodeposition | |
| Wang et al. | The effects of Mg2+ concentration,(NH4) 2SO4 concentration and current density on electrolytic manganese process | |
| KR100370401B1 (en) | Method for preparing indium tin oxide powder from indium tin oxide scrap | |
| CN102534659A (en) | Method for improving current efficiency of high purity zinc obtained by zinc chloride electrolysis | |
| BE1025151B9 (en) | Manufacturing process for Titanium dioxide (TiO₂), from Ilmenite using solar energy and seawater | |
| CN1011247B (en) | Rare-earth hexaboronide synthesized by melted salt electrolysis technique | |
| RU2208585C1 (en) | Nickel(ii) hydroxide production process | |
| Yang et al. | Hyperchaotic power with wide current variation for efficient manganese electrodeposition |
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 | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20091002 Address after: No. 21, building 1, Changan building, 1001 Changan Road, Shanghai, 200070 Co-patentee after: Shanghai Kai space Nano Technology Co., Ltd. Patentee after: Meng Guo Jun Address before: Room 602, building 4, Changan building, No. 1001, Changan Road, Shanghai, 200070 Patentee before: Meng Guojun |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060913 Termination date: 20121110 |