CN1557700A - Preparation of nano-graphite carbon sol by anode graphite electrode oxidation method - Google Patents
Preparation of nano-graphite carbon sol by anode graphite electrode oxidation method Download PDFInfo
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- CN1557700A CN1557700A CNA2004100026281A CN200410002628A CN1557700A CN 1557700 A CN1557700 A CN 1557700A CN A2004100026281 A CNA2004100026281 A CN A2004100026281A CN 200410002628 A CN200410002628 A CN 200410002628A CN 1557700 A CN1557700 A CN 1557700A
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Abstract
The graphite anode oxidizing process to prepare nano graphite carbon sol includes connecting graphite anode and stainless steel plate cathode separated with plastic net to power supply; adding electrolytic solution with electrolyte content lower than 0.1 wt% of electrolytic solution into oxidizing tank; turning on the power supply for oxidation at current density of 5-150 mA/sq cm, voltage of 10 V, temperature below 60 deg.c, and once stirring each 4-12 hr. The graphite carbon density in the tank is detected, and when it reaches 0.1-5 %, the reaction is finished to obtain the nano graphite carbon sol inside the tank. The process of the present invention has low production cost, high product stability and no pollution, and is suitable for large scale production.
Description
Technical field
The present invention relates to a kind of method for preparing nano carbon sol.
Background technology
Carbon materials is a crucial part in the non-metallic material, and because of its atomic arrangement mode difference, performance difference is very big, and carbon materials is very big because of its atomic arrangement mode difference performance difference equally in nano-scale range.Studies show that in large quantities the graphite-structure carbon of nano-scale range has the characteristic that many stock size scope graphite carbons are not had, its range of application is very extensive.But, when the graphite carbon size reaches nano-scale range, because it has the intensive adsorptivity and has negative electricity, thereby makes the very easy reunion of nano-graphite carbon materials, the difficult dispersion, so become the difficult problem of preparation nano-graphite carbon materials and application, have only a few countries to produce at present, its complex manufacturing, cost is high, easily produce dust pollution, be unfavorable for large-scale industrial production.
Summary of the invention
The object of the present invention is to provide a kind of technology simple, production cost is low, and result of use is good, and the anode graphite anodizing legal system that suitability for industrialized is produced is equipped with nano graphite carbon sol.
The present invention adopts the anode graphite electrode for anodal, and stainless steel plate is a negative pole, and puts into oxidation trough by the positive and negative electrode arrangement, separates with plastic wire between the positive and negative electrode, and electrode adopts the parallel-series mode to be connected with power supply.Electrolytic solution is poured in the oxidation trough, and ionogen adopts sulfuric acid or potassium hydroxide to add in the electrolytic solution, and it adds total amount by below 0.1% of electrolyte weight, and limit once adds in the electrolytic solution.Connect power supply, carry out oxide treatment, current control is at 5～150mA/cm
2, every bath voltage is controlled at 10 ± 3V, and temperature is controlled at below 60 ℃, stirs once every 4～12 hours.Detect graphite carbon concentration in the groove, collosol concentration reaches at 0.1～5% o'clock in the groove, and oxidation finishes, and solution is nano graphite carbon sol in the groove.
Routine techniques shows, after forming, carbon particulate is easy to reunite again, prevent the generation of this phenomenon, have only two kinds of basic skills at present: the first forms electrostatic double layer on the surface of nano particle, make that like charges repels each other between the nano particle, it two is to wrap up with another kind of material at nano grain surface, and it can not be contacted with each other.
It is that positive and negative electrode inserts in the electrolyte solution that the present invention adopts anode graphite electrode and stainless steel plate, after the energising, carbon atom obtains energy at positive pole under the effect of electric current, when energy surpasses valence bond power between carbon atom, and when obtaining to have the nano-scale range of formation carbon microparticle surface energy simultaneously, this part carbon atom will break away from anode plate, form the carbon granule of nano-scale range and be free in the electrolytic solution.Because it has extremely strong selection adsorptivity, nano carbon particle can be selected electricity layer negative ion, mutually exclusive formation double electrical layers between them, thus make nano carbon sol liquid be stablized formation.
Production cost of the present invention is low, and constant product quality is pollution-free, has the advantages such as requirement of suitability for industrialized scale operation, also has the characteristics that adapt to the high and low temperature ability.Be applicable to industries such as battery manufacturing, colour TV, oil, agricultural, electrically heated components and parts, electro-conductive material, health care, Application Areas is extremely extensive.
Embodiment
Oxidation trough of the present invention adopts the non-metallic material of insulativity to make, the anode graphite electrode adopts purity to make greater than 90% graphite, negative pole adopts the stainless steel plate of 1～1.5mm thickness, use stainless steel plate not only can improve the thickness and the tankage sheet number of the anode graphite plate in the oxidation trough, and can reduce production costs significantly.According to the watt level of DC power supply device, multi-disc anode graphite electrode and stainless steel plate can be put into two or more oxidation troughs respectively by the positive and negative electrode arrangement.Negative pole has more a slice than positive pole.Separate with the polyethylene plastic wire between the positive and negative electrode, electrode and power supply adopt the parallel-series mode to be connected, and positive pole and negative pole in every groove are connected in parallel respectively, between groove and the groove for connecting.
Electrolytic solution (deionized water) is poured in the oxidation trough, and electrolytic solution can be done suitably to adjust according to the character of required nano-graphite colloidal sol, and acidic sol can add the sulfuric acid of proportion 1.28, and alkaline colloidal sol can add the potassium hydroxide of proportion 1.30.Electrolytical adding total amount is by below 0.1% of electrolyte weight, and limit once adds in the electrolytic solution, thereby helps improving the preparation purity of Nano sol.When continuing to produce, get final product with remaining nanometer carbon liquid in the groove, the colloidal sol of producing like this is high purity.
Connect power supply, carry out oxide treatment, current control is at 5～150mA/cm
2, every bath voltage is controlled at 10 ± 3V, and temperature is controlled at below 60 ℃, stirs once every 4～12 hours, and churning time is 5～10 minutes.In the production process,, positive source can be changed when anode thickness during less than 10mm, detect graphite carbon concentration in the groove, collosol concentration is 0.1～5% o'clock, and oxidation finishes, solution is nano graphite carbon sol in the groove, and less than 10nm, all the other are 20% also in nano-scale range more than 80% for granularity.
Claims (1)
1, a kind of in oxidation trough by just, negative potential is arranged, just, separate with plastic wire between the negative potential, electrode adopts the parallel-series mode to be connected with power supply, electrolytic solution is poured in the oxidation trough, ionogen adopts sulfuric acid or potassium hydroxide to add in the electrolytic solution, it adds 0.1% below the adding of total amount by electrolyte weight, connect power supply and carry out oxide treatment, every bath voltage is controlled at 10 ± 3V, temperature is controlled at below 60 ℃, stirred once every 4～12 hours, make collosol concentration in the groove reach 0.1～5% anode graphite anodizing legal system and be equipped with nano graphite carbon sol, just it is characterized in that, negative potential adopts anode graphite and stainless steel plate respectively, and current control is at 5～150mA/cm
2, ionogen is limit once according to quantity and is added in the electrolytic solution during preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100026281A CN1323940C (en) | 2004-01-21 | 2004-01-21 | Preparation of nano-graphite carbon sol by anode graphite electrode oxidation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100026281A CN1323940C (en) | 2004-01-21 | 2004-01-21 | Preparation of nano-graphite carbon sol by anode graphite electrode oxidation method |
Publications (2)
| Publication Number | Publication Date |
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| CN1557700A true CN1557700A (en) | 2004-12-29 |
| CN1323940C CN1323940C (en) | 2007-07-04 |
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| CNB2004100026281A Expired - Fee Related CN1323940C (en) | 2004-01-21 | 2004-01-21 | Preparation of nano-graphite carbon sol by anode graphite electrode oxidation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408152C (en) * | 2005-04-20 | 2008-08-06 | 北京天中树科技发展有限公司 | Production and producer for nanometer carbon liquid |
| CN100427193C (en) * | 2006-06-13 | 2008-10-22 | 中国江南航天工业集团江南工业贸易公司 | Device for producing nano carbon sol by oxidation process |
| CN101469431B (en) * | 2007-12-24 | 2011-01-19 | 清华大学 | Method for preparing nano oxidized graphite particle or flake graphite and benzene hexacarbonic acid simultaneously |
| CN103373722A (en) * | 2012-04-17 | 2013-10-30 | 夏华松 | Preparation of nano-graphite carbon sol |
| CN104451757A (en) * | 2014-10-20 | 2015-03-25 | 风禾尽起科技(北京)有限公司 | Preparation method of carbon and silicon powder |
| CN106337192A (en) * | 2016-10-03 | 2017-01-18 | 上海库儿科技有限公司 | Method for preparing nanocarbon solution with conductive carbon fibers as electrode |
| 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 |
| CN109231185A (en) * | 2018-10-24 | 2019-01-18 | 深圳大学 | A kind of preparation method of nano-sized carbon onion |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH078790A (en) * | 1993-06-24 | 1995-01-13 | Kenichi Fujita | Preparation of colloidal solution of carbon |
| CN1078753C (en) * | 1995-09-29 | 2002-01-30 | 藤田贤一 | Electrolyte and lead accumulator using the same |
| JP2000086220A (en) * | 1998-09-14 | 2000-03-28 | Kenichi Fujita | Ultrafine carbon particle |
| CN1166558C (en) * | 2002-05-17 | 2004-09-15 | 陈万哲 | Process for preparing nano graphite carbon powder from nano graphite sol |
| CN1151061C (en) * | 2002-05-17 | 2004-05-26 | 陈万哲 | Process for preparing nano graphite carbon sol with dual graphite electrodes |
-
2004
- 2004-01-21 CN CNB2004100026281A patent/CN1323940C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408152C (en) * | 2005-04-20 | 2008-08-06 | 北京天中树科技发展有限公司 | Production and producer for nanometer carbon liquid |
| CN100427193C (en) * | 2006-06-13 | 2008-10-22 | 中国江南航天工业集团江南工业贸易公司 | Device for producing nano carbon sol by oxidation process |
| CN101469431B (en) * | 2007-12-24 | 2011-01-19 | 清华大学 | Method for preparing nano oxidized graphite particle or flake graphite and benzene hexacarbonic acid simultaneously |
| CN103373722A (en) * | 2012-04-17 | 2013-10-30 | 夏华松 | Preparation of nano-graphite carbon sol |
| CN104451757A (en) * | 2014-10-20 | 2015-03-25 | 风禾尽起科技(北京)有限公司 | Preparation method of carbon and silicon powder |
| CN104451757B (en) * | 2014-10-20 | 2017-07-14 | 风禾尽起科技(北京)有限公司 | A kind of preparation method of carbon silica flour |
| CN106337192A (en) * | 2016-10-03 | 2017-01-18 | 上海库儿科技有限公司 | Method for preparing nanocarbon solution with conductive carbon fibers as electrode |
| 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 |
| CN109231185A (en) * | 2018-10-24 | 2019-01-18 | 深圳大学 | A kind of preparation method of nano-sized carbon onion |
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| Publication number | Publication date |
|---|---|
| CN1323940C (en) | 2007-07-04 |
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Effective date of registration: 20060526 Address after: 563000 Guizhou Aerospace nanometer science and technology company, No. 26 rain water channel, Guizhou, Zunyi Applicant after: Liu Fangde Co-applicant after: Li Shengnan Co-applicant after: Fu Yuanchao Address before: 563000 Guizhou Aerospace nanometer science and technology company, No. 26 rain water channel, Guizhou, Zunyi Applicant before: Liu Fangde Co-applicant before: Li Shengnan Co-applicant before: Fu Yuanchao Co-applicant before: Chen Wanzhe Co-applicant before: Zhu Guanghua Co-applicant before: Xie Longmeng |
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