CN103151112A - Super conductive agent preparation method - Google Patents
Super conductive agent preparation method Download PDFInfo
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- CN103151112A CN103151112A CN2013100315774A CN201310031577A CN103151112A CN 103151112 A CN103151112 A CN 103151112A CN 2013100315774 A CN2013100315774 A CN 2013100315774A CN 201310031577 A CN201310031577 A CN 201310031577A CN 103151112 A CN103151112 A CN 103151112A
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Abstract
The invention discloses a super conductive agent preparation method. The super conductive agent preparation method includes a first step of mixing phenolic resin, or high-softening-point pitch or mixture of the mixing phenolic resin and the high-softening-point pitch with additives, inputting the mixture to an atomizing nozzle on the top of an atomizing tower through a high-pressure pump, mixing the mixture with high-pressure airflow, and spraying out atomized fine powder through the atomizing nozzle, a second step of enabling the atomized fine powder in the atomizing tower to be condensed into solidified fine powder through thermal shrinkage in the dropping process, a third step of inputting the solidified fine powder into a tempering convertor and then carrying out staging carbonization treatment on the solidified fine powder, and a fourth step of cooling the carbonized powder to the normal temperature under the protection of nitrogen and then discharging to obtain super conductive agents. The electrical conductivity of the super conductive agents prepared through the method is smaller than 10-4 s/cm, the purity of the super conductive agents is bigger than 99.95%, and the density of the super conductive agents is 0.4-0.6 g/ml. The super conductive agents prepared through the method have the advantages of being large in specific gravity, good in conductivity, and suitable for popularization and application.
Description
Technical field
The present invention relates to a kind of than preparation method great, the super conductive agent that conducts electricity very well.
Background technology
Conductive agent is in order to guarantee that electrode has good charge-discharge performance, when making, pole piece usually adds a certain amount of conductive materials, between active material, play the effect of collecting little electric current between active material and collector, accelerate the rate travel of electronics with the contact resistance that reduces electrode, simultaneously also can effectively improve the migration rate of lithium ion in electrode material, thereby improve the efficiency for charge-discharge of electrode.Along with people constantly propose Secretary to the speed that discharges and recharges, the service efficiency of for example lithium ion battery, existing conductive agent electric conductivity can't practical requirement.
Summary of the invention
The objective of the invention is the deficiency for existing conductive agent, provide a kind of than preparation method great, the super conductive agent that conducts electricity very well.
The objective of the invention is to solve by the following technical programs:
A kind of preparation method of super conductive agent is characterized in that described preparation method carries out in the steps below:
(1) phenolic resins, high softening point bitumen or both mixtures are mixed the atomizer that inputs to the atomizing tower top by high-pressure pump with auxiliary agent, and high pressure draught mixes by atomizer ejection atomizing fine powder material;
(2) the atomizing fine powder material from atomizing tower top free fall to atomisation tower at the bottom of, fine powder material thermal polycondensation in the high-temperature atomizing tower becomes the curing fine powder material in dropping process;
(3) in the modified converter of curing fine powder material input that collection is obtained, then with the heating rate of 2-5 ℃/min, furnace temperature is risen to 500 ℃-700 ℃ and keep constant temperature to carry out carbonization treatment to solidifying fine powder material in 1-2 hour, then keep constant temperature 0.5-1 hour to solidifying the further carbonization treatment of fine powder material after with the heating rate of 2-5 ℃/min, furnace temperature being risen to 1000 ℃-1200 ℃;
(4) powder after carbonization is cooled to the normal temperature discharging and namely gets super conductive agent under nitrogen protection.
The softening point of the high softening point bitumen in described step (1) is 200-300 ℃.
Auxiliary agent in described step (1) is the mixture of curing agent and plasticizer.
Auxiliary agent weight in described step (1) is the 2-8% of phenolic resins, high softening point bitumen or both mixture weight.
Pressure in high-pressure pump in described step (1) is 5-10 MPa.
The particle diameter of the atomizing fine powder material in described step (1) is the 100-300 nanometer.
Atomisation tower height in described step (2) is 20-30 rice.
In atomisation tower in described step (2), temperature is 300-400 ℃.
After reaching 500 ℃, the furnace temperature of the modified converter in described step (3) passes into nitrogen protection.
Super conductive agent particle diameter in described step (4) is the 80-300 nanometer.
The present invention has the following advantages compared to existing technology:
At first the present invention is atomized into fine powder material with raw material, and be the curing fine powder material by the process polycondensation of free fall, part volatile matter in atomization process is discharged from the atomizing tower top and is entered the condensate recovery system recycling, then make super conductive agent, these super conductive agent conductance＜10 by carbonization stage by stage
-4S/cm, purity＞99.95%, density 0.4-0.6g/ml have than characteristics great, that conduct electricity very well, suitable promoting the use of.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
At first the high-pressure pump that it is 6 MPa that the auxiliary agent that phenolic resins and curing agent, plasticizer is consisted of mixes by pressure inputs to the atomizer of atomizing tower top, it is the atomizing fine powder material of 100-300 nanometer that abundant and high pressure draught mixes by atomizer ejection particle diameter, and wherein the weight of auxiliary agent is 5% of phenolic resins weight; The atomizing fine powder material from 20 meters eminence free falls to atomisation tower at the bottom of, fine powder material thermal polycondensation in temperature is the high-temperature atomizing tower of 300 ℃ becomes the curing fine powder material in dropping process, the part volatile matter is discharged from the atomizing tower top and is entered condensate recovery system and recycle simultaneously; The curing fine powder material that collection obtains is inputted in modified converter, then with the heating rate of 5 ℃/min, furnace temperature being risen to 700 ℃ keeps constant temperature to carry out carbonization treatment to solidifying fine powder material in 1 hour, and remove oil smoke, low boiling volatile matter, wherein after reaching 500 ℃, the furnace temperature of modified converter passes into nitrogen protection, keep constant temperature 1 hour to solidifying the further carbonization treatment of fine powder material after with the heating rate of 2 ℃/min, furnace temperature being risen to 1000 ℃ again, and further remove oil smoke; At last be cooled to the normal temperature discharging under nitrogen protection and namely get the super conductive agent that particle diameter is the 80-300 nanometer.The super conductive agent conductance that the present invention makes＜10
-4S/cm, purity＞99.95%, density 0.4-0.6g/ml have than characteristics great, that conduct electricity very well, suitable promoting the use of.
Embodiment 2
At first be the atomizer that high softening point bitumen and the curing agent of 200-300 ℃, auxiliary agent that plasticizer the consists of high-pressure pump that to mix by pressure be 5MPa inputs to the tower top that atomizes with softening point, it is the atomizing fine powder material of 100-300 nanometer that abundant and high pressure draught mixes by atomizer ejection particle diameter, and wherein the quality of auxiliary agent is 2% of phenolic resins or high softening point bitumen; The atomizing fine powder material from 25 meters eminence free falls to atomisation tower at the bottom of, fine powder material thermal polycondensation in temperature is the high-temperature atomizing tower of 380 ℃ becomes the curing fine powder material in dropping process, the part volatile matter is discharged from the atomizing tower top and is entered condensate recovery system and recycle simultaneously; The curing fine powder material that collection obtains is inputted in modified converter, then with the heating rate of 3 ℃/min, furnace temperature being risen to 600 ℃ keeps constant temperature to carry out carbonization treatment to solidifying fine powder material in 1.5 hours, and remove oil smoke, low boiling volatile matter, wherein after reaching 500 ℃, the furnace temperature of modified converter passes into nitrogen protection, keep constant temperature 0.6 hour to solidifying the further carbonization treatment of fine powder material after with the heating rate of 4 ℃/min, furnace temperature being risen to 1150 ℃ again, and further remove oil smoke; At last be cooled to the normal temperature discharging under nitrogen protection and namely get the super conductive agent that particle diameter is the 80-300 nanometer.The super conductive agent conductance that the present invention makes＜10
-4S/cm, purity＞99.95%, density 0.4-0.6g/ml have than characteristics great, that conduct electricity very well, suitable promoting the use of.
Embodiment 3
At first be the atomizer that mixture and the auxiliary agent that curing agent, plasticizer consist of of the high softening point bitumen of 200-300 ℃ and the phenolic resins high-pressure pump that to mix by pressure be 8 MPa inputs to the tower top that atomizes with softening point, it is the atomizing fine powder material of 100-300 nanometer that abundant and high pressure draught mixes by atomizer ejection particle diameter, and wherein the quality of auxiliary agent is 8% of phenolic resins or high softening point bitumen; The atomizing fine powder material from 25 meters eminence free falls to atomisation tower at the bottom of, fine powder material thermal polycondensation in temperature is the high-temperature atomizing tower of 350 ℃ becomes the curing fine powder material in dropping process, the part volatile matter is discharged from the atomizing tower top and is entered condensate recovery system and recycle simultaneously; The curing fine powder material that collection obtains is inputted in modified converter, then with the heating rate of 2 ℃/min, furnace temperature being risen to 500 ℃ keeps constant temperature to carry out carbonization treatment to solidifying fine powder material in 2 hours, and remove oil smoke, low boiling volatile matter, wherein after reaching 500 ℃, the furnace temperature of modified converter passes into nitrogen protection, keep constant temperature 0.5 hour to solidifying the further carbonization treatment of fine powder material after with the heating rate of 5 ℃/min, furnace temperature being risen to 1200 ℃ again, and further remove oil smoke; At last be cooled to the normal temperature discharging under nitrogen protection and namely get the super conductive agent that particle diameter is the 80-300 nanometer.The super conductive agent conductance that the present invention makes＜10
-4S/cm, purity＞99.95%, density 0.4-0.6g/ml have than characteristics great, that conduct electricity very well, suitable promoting the use of.
Embodiment 4
At first the high-pressure pump that it is 10 MPa that the auxiliary agent that phenolic resins and curing agent, plasticizer is consisted of mixes by pressure inputs to the atomizer of atomizing tower top, it is the atomizing fine powder material of 100-300 nanometer that abundant and high pressure draught mixes by atomizer ejection particle diameter, and wherein the quality of auxiliary agent is 6% of phenolic resins or high softening point bitumen; The atomizing fine powder material from 30 meters eminence free falls to atomisation tower at the bottom of, fine powder material thermal polycondensation in temperature is the high-temperature atomizing tower of 300 ℃ becomes the curing fine powder material in dropping process, the part volatile matter is discharged from the atomizing tower top and is entered condensate recovery system and recycle simultaneously; The curing fine powder material that collection obtains is inputted in modified converter, then with the heating rate of 4 ℃/min, furnace temperature being risen to 650 ℃ keeps constant temperature to carry out carbonization treatment to solidifying fine powder material in 1.2 hours, and remove oil smoke, low boiling volatile matter, wherein after reaching 500 ℃, the furnace temperature of modified converter passes into nitrogen protection, keep constant temperature 0.7 hour to solidifying the further carbonization treatment of fine powder material after with the heating rate of 3 ℃/min, furnace temperature being risen to 1100 ℃ again, and further remove oil smoke; At last be cooled to the normal temperature discharging under nitrogen protection and namely get the super conductive agent that particle diameter is the 80-300 nanometer.The super conductive agent conductance that the present invention makes＜10
-4S/cm, purity＞99.95%, density 0.4-0.6g/ml have than characteristics great, that conduct electricity very well, suitable promoting the use of.
Above embodiment only for explanation technological thought of the present invention, can not limit protection scope of the present invention with this, every technological thought that proposes according to the present invention, and any change of doing on the technical scheme basis is within all falling into protection range of the present invention; The technology that the present invention does not relate to all can be realized by prior art.
Claims (10)
1. the preparation method of a super conductive agent is characterized in that described preparation method carries out in the steps below:
(1) phenolic resins, high softening point bitumen or both mixtures are mixed the atomizer that inputs to the atomizing tower top by high-pressure pump with auxiliary agent, and high pressure draught mixes by atomizer ejection atomizing fine powder material;
(2) the atomizing fine powder material from atomizing tower top free fall to atomisation tower at the bottom of, fine powder material thermal polycondensation in the high-temperature atomizing tower becomes the curing fine powder material in dropping process;
(3) in the modified converter of curing fine powder material input that collection is obtained, then with the heating rate of 2-5 ℃/min, furnace temperature is risen to 500 ℃-700 ℃ and keep constant temperature to carry out carbonization treatment to solidifying fine powder material in 1-2 hour, then keep constant temperature 0.5-1 hour to solidifying the further carbonization treatment of fine powder material after with the heating rate of 2-5 ℃/min, furnace temperature being risen to 1000 ℃-1200 ℃;
(4) powder after carbonization is cooled to the normal temperature discharging and namely gets super conductive agent under nitrogen protection.
2. the preparation method of super conductive agent according to claim 1, the softening point that it is characterized in that the high softening point bitumen in described step (1) is 200-300 ℃.
3. the preparation method of super conductive agent according to claim 1, is characterized in that the auxiliary agent in described step (1) is the mixture of curing agent and plasticizer.
4. the preparation method of according to claim 1 or 3 described super conductive agents, is characterized in that the auxiliary agent weight in described step (1) is the 2-8% of phenolic resins, high softening point bitumen or both mixture weight.
5. the preparation method of super conductive agent according to claim 1, is characterized in that the pressure in the high-pressure pump in described step (1) is 5-10 MPa.
6. the preparation method of super conductive agent according to claim 1, the particle diameter that it is characterized in that the atomizing fine powder material in described step (1) is the 100-300 nanometer.
7. the preparation method of super conductive agent according to claim 1, is characterized in that the atomisation tower height in described step (2) is 20-30 rice.
8. the preparation method of super conductive agent according to claim 1, is characterized in that in the atomisation tower in described step (2), temperature is 300-400 ℃.
9. the preparation method of super conductive agent according to claim 1 is characterized in that passing into nitrogen protection after modified converter furnace temperature in described step (3) reaches 500 ℃.
10. the preparation method of super conductive agent according to claim 1, is characterized in that the super conductive agent particle diameter in described step (4) is the 80-300 nanometer.
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| CN2013100315774A CN103151112A (en) | 2013-01-28 | 2013-01-28 | Super conductive agent preparation method |
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| CN2013100315774A CN103151112A (en) | 2013-01-28 | 2013-01-28 | Super conductive agent preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799775A (en) * | 2016-08-30 | 2018-03-13 | 宁德新能源科技有限公司 | Water system battery and its anode pole piece |
| CN107814373A (en) * | 2017-11-01 | 2018-03-20 | 江苏省宜兴中等专业学校 | A kind of preparation method of conductive agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020027066A1 (en) * | 2000-09-06 | 2002-03-07 | Koichi Kanno | Processes for producing coke, artificial graphite and carbon material for negative electrode of non-aqueous solvent type secondary battery and pitch composition used therefor |
| CN102179217A (en) * | 2011-03-10 | 2011-09-14 | 江苏国正新材料科技有限公司 | Preparation method of hyper-energy active electrical carbon hollow micro ball |
| CN102363524A (en) * | 2011-06-30 | 2012-02-29 | 江苏国正新材料科技有限公司 | Preparation method of high-efficiency carbon material hollow spheres |
-
2013
- 2013-01-28 CN CN2013100315774A patent/CN103151112A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020027066A1 (en) * | 2000-09-06 | 2002-03-07 | Koichi Kanno | Processes for producing coke, artificial graphite and carbon material for negative electrode of non-aqueous solvent type secondary battery and pitch composition used therefor |
| CN102179217A (en) * | 2011-03-10 | 2011-09-14 | 江苏国正新材料科技有限公司 | Preparation method of hyper-energy active electrical carbon hollow micro ball |
| CN102363524A (en) * | 2011-06-30 | 2012-02-29 | 江苏国正新材料科技有限公司 | Preparation method of high-efficiency carbon material hollow spheres |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799775A (en) * | 2016-08-30 | 2018-03-13 | 宁德新能源科技有限公司 | Water system battery and its anode pole piece |
| CN107814373A (en) * | 2017-11-01 | 2018-03-20 | 江苏省宜兴中等专业学校 | A kind of preparation method of conductive agent |
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Owner name: BEIJING ZHONGSHIHONG INSTALLATION ENGINEERING CO., Free format text: FORMER OWNER: JIANGSU GUOZHENG NEW MATERIAL TECHNOLOGY CO., LTD. Effective date: 20141118 |
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Effective date of registration: 20141118 Address after: 100020, Beijing, Chaoyang District, 16 Wai Street, China Life Building, 5 floor, South District Applicant after: BEIJING ZHONGSHIHONG INSTALLATION ENGINEERING CO., LTD. Address before: Xinjiezhen Zhenxin West Road Yixing Jiangsu province 214204 city of Wuxi City, No. 6-8 Applicant before: Jiangsu Guozheng New Material Technology Co., Ltd. |
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Application publication date: 20130612 |