CN1323940C - 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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- CN1323940C CN1323940C CNB2004100026281A CN200410002628A CN1323940C CN 1323940 C CN1323940 C CN 1323940C CN B2004100026281 A CNB2004100026281 A CN B2004100026281A CN 200410002628 A CN200410002628 A CN 200410002628A CN 1323940 C CN1323940 C CN 1323940C
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Abstract
The present invention provides preparation of nanometer graphite carbon sol by using an anode graphite electrode oxidation method, which comprises: an anode graphite electrode and a stainless steel plate are respectively arranged in a positive pole and negative pole mode and put in an oxidation tank, the positive electrode and the negative electrode are separated by a plastic mesh, the electrodes are connected with a power supply in a parallel-serial mode, an electrolytic solution is poured in the oxidation tank, the added total quantity of the electrolyte is less than 0.1% of the weight of the electrolytic solution, the electrolyte is added to the electrolytic solution for one time, the power supply is on so as to carry out the oxidation treatment, the current is controlled at 5 to 150 mA/cm<2>, each tank voltage is controlled at 10 (+/-)3V, the temperature is controlled at below 60DEG C, and the electrolytic solution is stirred every 4 to 12 hours; the concentration of the graphite carbon in the detection tank, the oxidation is finished when the concentration of the sol reaches 0.1 to 5%, and the solution in the tank is the nanometer graphite carbon sol. The present invention has the advantages of low production cost, stable product quality, no pollution, etc., is suitable for the requirement of industrialized large-scale production, has the characteristic of adaptability to high temperature and low temperature, and has wide application fields.
Description
Technical field
The present invention relates to a kind of preparation method of 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, the preparation method of the nano graphite carbon sol that suitability for industrialized is produced.
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 preparation method of nano graphite carbon sol, the anode graphite and the negative electrode that adopt plastic wire will be arranged in the oxidation trough separate, sun, negative 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, making the interior collosol concentration of groove reach oxidation in 0.1～5% o'clock finishes, it is characterized in that negative electrode adopts stainless steel plate, when the connection power supply carried out oxide treatment, current control was at 5～150mA/cm
2, ionogen is in disposable adding electrolytic solution.
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 |
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| CNB2004100026281A CN1323940C (en) | 2004-01-21 | 2004-01-21 | Preparation of nano-graphite carbon sol by anode graphite electrode oxidation method |
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| Publication Number | Publication Date |
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| CN1557700A CN1557700A (en) | 2004-12-29 |
| CN1323940C true 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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Families Citing this family (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 |
| 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 |
| 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 |
| 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 |
| CN109231185A (en) * | 2018-10-24 | 2019-01-18 | 深圳大学 | A kind of preparation method of nano-sized carbon onion |
Citations (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 |
| CN1146642A (en) * | 1995-09-29 | 1997-04-02 | 藤田贤一 | Electrolyte and lead accumulator using the same |
| JP2000086220A (en) * | 1998-09-14 | 2000-03-28 | Kenichi Fujita | Ultrafine carbon particle |
| CN1378976A (en) * | 2002-05-17 | 2002-11-13 | 贵州航天纳米科技有限责任公司 | Process for preparing nano graphite carbon powder from nano graphite sol |
| CN1378975A (en) * | 2002-05-17 | 2002-11-13 | 贵州航天纳米科技有限责任公司 | 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
Patent Citations (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 |
| CN1146642A (en) * | 1995-09-29 | 1997-04-02 | 藤田贤一 | Electrolyte and lead accumulator using the same |
| JP2000086220A (en) * | 1998-09-14 | 2000-03-28 | Kenichi Fujita | Ultrafine carbon particle |
| CN1378976A (en) * | 2002-05-17 | 2002-11-13 | 贵州航天纳米科技有限责任公司 | Process for preparing nano graphite carbon powder from nano graphite sol |
| CN1378975A (en) * | 2002-05-17 | 2002-11-13 | 贵州航天纳米科技有限责任公司 | Process for preparing nano graphite carbon sol with dual graphite electrodes |
Non-Patent Citations (1)
| Title |
|---|
| 石墨电化学氧化剂制备纳米粒子及表征 翁文桂等，华侨大学学报（自然科学版），第23卷第4期 2002 * |
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| CN1557700A (en) | 2004-12-29 |
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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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