CN103915134A - Method for preparing environment-friendly graphene-based conductive carbon paste - Google Patents
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Abstract
The invention relates to a method for preparing environment-friendly graphene-based conductive carbon paste. The method includes the following steps that firstly, inorganic filler is prepared, wherein conductive carbon black, graphene, graphite, a dispersing agent, an adhesion promoter and an antifoaming agent are dispersed uniformly in a dispersion machine; secondly, an organic carrier is prepared, wherein solvent type resin A, solvent type resin B, solvent type resin C and a mixed solvent are weighed and placed in an electrical heating reaction vessel to be heated and fully and uniformly stirred and mixed; thirdly, the inorganic carrier and the organic carrier are mixed together and ground in a sand mill to form an even mixed phase, a base material is coated with paste and dried to prepare a film, and then the resistance of the film is measured. The method for preparing the environment-friendly graphene-based conductive carbon paste is simple, convenient to operate and reasonable in formula, the traditional conductive carbon black is used as raw materials, and a proper amount of the graphene is added, so that conductivity of the carbon paste is improved; the prepared carbon paste is small in internal resistance, uniform in size distribution, and capable of achieving coating easily and being widely applied to a heating panel, a warmer, a wall warmer, a ground warmer and other products.
Description
Technical field
The present invention relates to graphene-based high conductive carbon paste of a kind of environment-friendly type and preparation method thereof.Graphene-based high heating carbon slurry can be widely used in the aspects such as the warm floor heating of wall, Electrically heated blanket, Saunas heating board, CPU heat-generating mouse mat, Far infrared carbon crystal picture, far-infrared warming sole, far infrared health care cushion.
Background technology
Along with economic fast development, modern society is more and more higher to the quality of heating, and the just research and development to electrocondution slurry of a step of most critical in the middle of the technique of heating.On market, electrocondution slurry is divided into two classes, one class is the inorganic filler take argent as representative, an other class is exactly the inorganic filler take material with carbon element as representative, but just practical situations in the market, conductive carbon paste is compared with conductive silver paste, sheet resistance value is larger, but with low cost, cost performance is high, stable performance, becomes the main direction of current research and development so improve the conductivity of conductive carbon paste.Graphene is a kind of new carbon, and it is the hexagonal lattice structure being formed by monolayer carbon atom close-packed arrays, and because it has excellent conductivity, (horizontal conductivity is up to 10
6s/m), can be used as a kind of well conductive filler and be applied to conductive carbon paste market.The graphene-based electrocondution slurry of this patent research and development is carbon slurry products with conducting function that a class is made up of graphene powder, resin, auxiliary agent and solvent etc., compared with existing metal species electrocondution slurry, graphene-based electrocondution slurry has huge cost advantage, and conduct electricity very well, internal resistance is little, even particle size distribution, is easy to the advantages such as coating.Compared with traditional carbon back conductive carbon paste product, graphene-based electrocondution slurry has again significant advantage aspect electric conductivity.Graphene-based electrocondution slurry is applicable to the modes such as wire mark, gravure, flexo, offset printing and ink jet printing, can be applied to the aspects such as printed substrate (PCB), radio-frequency (RF) identification (RFID), display screen (as OLED), electrode sensor.Therefore graphene-based electrocondution slurry is expected to be used widely in, flexible electronic product frivolous radio-frequency (RF) tag, intelligent packaging, thin film switch, conducting wire and the sensor next generation, and market prospects are huge.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, provide one effectively to improve the quality of products, technique is simple, and the preparation method of the graphene-based high conductive carbon paste of the significant environment-friendly type of effect can be useful in the warm floor heating of wall etc. above product.In order to achieve the above object, the concrete technical scheme that the present invention implements is:
(1) preparation of inorganic filler: 5% ~ 15% conductive carbon black, 5% ~ 15% graphene powder, 15% ~ 25% graphite, dispersant B YK, adhesion promoter and the defoamer of 5% left and right and 40% ~ 60% solvent fully stir until be uniformly dispersed in dispersion machine.
(2) preparation of organic carrier: according to mass percent metering, take respectively 20% polyurethane resin and 20% acrylic resin, and 60% solvent, be placed in electric heating reacting kettle heating and fully stir, make resin dissolve completely and mix.
(3) prepare carbon slurry: above-mentioned inorganic carrier and organic carrier are mixed, in mixer, stir, mixing time is 30 min, and being then placed in per kilogram milling time in sand mill is 1 h, make it to form uniform mixing phase, can obtain the conductive carbon paste slurry of environment-friendly type.
Final products Performance Evaluating Indexes prepared by this programme is to measure its sheet resistance.Concrete method of testing is: drying machine is tested product after dry 30 min at 120 ℃, and the grain fineness of slurry is less than below 10 μ m, and wherein the low energy of the sample resistance value of 6*6 cm reaches 90 Ω/cm
2, heating after resistance value highly stable, surface heat temperature is even, and slurry PET, glass fabric and epoxy resin board etc. above base material adhesive force fine, acid and alkali-resistance, solvent corrosion performance is good, meets national standard.The topmost technical characterstic of this electrocondution slurry is environmental protection, electric conductivity excellence, and printing adaptability is extremely strong, and the mar proof that adhesive force is excellent, good and chemical resistance, anti-aging, long service life, heating efficiency be high, have the features such as far infrared heating function.
Because technique scheme is used, the present invention compared with prior art has following advantages: Graphene prepares by physics stripping method, surface is zero defect almost, add the electric conductivity that has strengthened slurry in organic carrier to as inorganic filler, and the preparation method of graphene powder is easy, and cost is low.Organic solvent used is the absolute ethyl alcohol of environment-friendly type, greatly reduces production cost, highly-conductive hot carbon prepared by the present invention starch not only environmental protection and also cost lower, key is to conduct electricity very well, be applicable to large-scale industrial production.
Embodiment
Below by concrete enforcement, the present invention is described in further detail.It should be noted that, following example only limits to the present invention, but is not limited to practical range of the present invention.
Embodiment 1: the preparation of the heating carbon slurry that graphene powder addition is 5%
(1) preparation of inorganic carrier: 10% conductive carbon black, 5% graphene powder, 20% graphite, dispersant B YK, adhesion promoter, defoamer and 40% ~ 60% solvent are uniformly dispersed in dispersion machine.
(2) preparation of organic carrier: according to mass percent metering, take respectively 20% polyurethane resin and 20% acrylic resin, 60% solvent, is placed in electric heating reacting kettle heating and fully stirs, and makes resin dissolve completely and mix.
(3) preparation of carbon slurry: above-mentioned inorganic carrier and organic carrier are mixed, be fully uniformly dispersed in dispersion machine, the time of dispersion is 30min, being then placed in per kilogram milling time in sand mill is 1h, makes it to form uniform mixing phase.After grinding, obtain the conductive carbon paste of environment-friendly type.
Embodiment 2: the preparation of the heating carbon slurry that graphene powder addition is 7%:
(1) preparation of inorganic carrier: 10% conductive carbon black, 7% graphene powder, 20% graphite, dispersant B YK, adhesion promoter, defoamer and 40% ~ 60% solvent are uniformly dispersed in dispersion machine.
(2) preparation of organic carrier: according to mass percent metering, take respectively 20% polyurethane resin and 20% acrylic resin, 60% solvent, is placed in electric heating reacting kettle heating and fully stirs, and makes resin dissolve completely and mix.
(3) preparation of carbon slurry: above-mentioned inorganic carrier and organic carrier are mixed, be fully uniformly dispersed in dispersion machine, the time of dispersion is 30min, being then placed in per kilogram milling time in sand mill is 1h, makes it to form uniform mixing phase.After grinding, obtain the conductive carbon paste of environment-friendly type.
Embodiment 3: the preparation of the heating carbon slurry that graphene powder addition is 9%:
(1) preparation of inorganic carrier: 10% conductive carbon black, 9% graphene powder, 20% graphite, dispersant B YK, adhesion promoter, defoamer and 40% ~ 60% solvent are uniformly dispersed in dispersion machine.
(2) preparation of organic carrier: according to mass percent metering, take respectively 20% polyurethane resin and 20% acrylic resin, 60% solvent, is placed in electric heating reacting kettle heating and fully stirs, and makes resin dissolve completely and mix.
(3) preparation of carbon slurry: above-mentioned inorganic carrier and organic carrier are mixed, be fully uniformly dispersed in dispersion machine, the time of dispersion is 30min, being then placed in per kilogram milling time in sand mill is 1h, makes it to form uniform mixing phase.After grinding, obtain the conductive carbon paste of environment-friendly type.
Embodiment 4: the preparation of the heating carbon slurry that graphene powder addition is 11%:
(1) preparation of inorganic carrier: 10% conductive carbon black, 11% graphene powder, 20% graphite, dispersant B YK, adhesion promoter, defoamer and 40% ~ 60% solvent are uniformly dispersed in dispersion machine.
(2) preparation of organic carrier: according to mass percent metering, take respectively 20% polyurethane resin and 20% acrylic resin, 60% solvent, is placed in electric heating reacting kettle heating and fully stirs, and makes resin dissolve completely and mix.
(3) preparation of carbon slurry: above-mentioned inorganic carrier and organic carrier are mixed, be fully uniformly dispersed in dispersion machine, the time of dispersion is 30min, being then placed in per kilogram milling time in sand mill is 1h, makes it to form uniform mixing phase.After grinding, obtain the conductive carbon paste of environment-friendly type.
Embodiment 5: the preparation of the heating carbon slurry that graphene powder addition is 13%:
(1) preparation of inorganic carrier: 10% conductive carbon black, 13% graphene powder, 20% graphite, dispersant B YK, adhesion promoter, defoamer and 40% ~ 60% solvent are uniformly dispersed in dispersion machine.
(2) preparation of organic carrier: according to mass percent metering, take respectively 20% polyurethane resin and 20% acrylic resin, 60% solvent, is placed in electric heating reacting kettle heating and fully stirs, and makes resin dissolve completely and mix.
(3) preparation of carbon slurry: above-mentioned inorganic carrier and organic carrier are mixed, be fully uniformly dispersed in dispersion machine, the time of dispersion is 30min, being then placed in per kilogram milling time in sand mill is 1h, makes it to form uniform mixing phase.After grinding, obtain the conductive carbon paste of environment-friendly type.
Embodiment 6: the preparation of the heating carbon slurry that graphene powder addition is 15%:
(1) preparation of inorganic carrier: 10% conductive carbon black, 15% graphene powder, 20% graphite, dispersant B YK, adhesion promoter, defoamer and 40% ~ 60% solvent are uniformly dispersed in dispersion machine.
(2) preparation of organic carrier: according to mass percent metering, take respectively 20% polyurethane resin and 20% acrylic resin, 60% solvent, is placed in electric heating reacting kettle heating and fully stirs, and makes resin dissolve completely and mix.
(3) preparation of carbon slurry: above-mentioned inorganic carrier and organic carrier are mixed, be fully uniformly dispersed in dispersion machine, the time of dispersion is 30min, being then placed in per kilogram milling time in sand mill is 1h, makes it to form uniform mixing phase.After grinding, obtain the conductive carbon paste of environment-friendly type.
Take above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, relevant staff can, not departing from the scope of this invention technological thought, carry out various change and modification completely.The technical scope of this invention is not limited to the content on specification, must determine its technical scope according to claim scope.
Claims (10)
1. a conductive carbon paste, is characterized in that, comprises the raw material of following mass fraction: inorganic filler components 30% ~ 60%, resin carrier 30% ~ 40%, solvent 2% ~ 10%.
2. inorganic filler according to claim 1, it is characterized in that, comprise the raw material of following parts by weight: conductive carbon black 5% ~ 15%, graphene powder 5% ~ 15%, graphite 15% ~ 25%, wherein dispersant B YK, adhesion promoter, defoamer add total amount to be no more than 5%.
3. organic carrier according to claim 1, is characterized in that, described resin carrier is that following raw material forms: polyurethane resin, mylar, acrylic resin etc.
4. organic carrier according to claim 1, is characterized in that, described resin carrier is to form according to following mass fraction: polyurethane resin 5 ~ 15%, mylar 5 ~ 15%, acrylic resin 5 ~ 15%, solvent 45 ~ 65%.
5. solvent according to claim 1, its feature with, described solvent is absolute ethyl alcohol, diethylene adipate, ethyl acetate, one or both in 2-Butoxyethyl acetate.
6. conductive carbon paste according to claim 2, is characterized in that, described dispersant is BYK series.
7. conductive carbon paste according to claim 2, is characterized in that, described adhesion promoter is titanate coupling agent.
8. conductive carbon paste according to claim 2, is characterized in that, described defoamer is silicone defoaming agent.
9. claim 1 is stated a preparation method for heating carbon slurry, it is characterized in that, comprises the following steps:
1) prepare inorganic filler: 5% ~ 15% conductive carbon black, 5% ~ 15% graphene powder, 15% ~ 25% graphite, dispersant B YK, adhesion promoter and the defoamer of 5% left and right and 40% ~ 60% solvent fully stir until be uniformly dispersed in dispersion machine;
2) prepare organic carrier: according to mass percent metering, take respectively 20% mylar and 20% acrylic resin, and 60% solvent, be placed in electric heating reacting kettle heating and fully stir, make resin dissolve completely and mix;
3) prepare conductive carbon paste: above-mentioned inorganic carrier and organic carrier are mixed, in mixer, stir, mixing time is 30 min, and being then placed in per kilogram milling time in sand mill is 1 h, make it to form uniform mixing phase, can obtain the conductive carbon paste slurry of environment-friendly type.
10. conductive carbon paste is applicable to PET, glass fabric, the base materials such as epoxy resin board.
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| CN104153470A (en) * | 2014-08-18 | 2014-11-19 | 太仓派欧技术咨询服务有限公司 | Heating wall body and manufacturing method thereof |
| CN105244117A (en) * | 2015-09-29 | 2016-01-13 | 无锡同创石墨烯应用科技有限公司 | Preparation method of graphene-modified reinforced far infrared conductive paste |
| CN105352008A (en) * | 2015-12-04 | 2016-02-24 | 江苏洛基木业有限公司 | Graphene self-heating floor and low-voltage self-heating floor system |
| CN105621404A (en) * | 2016-02-19 | 2016-06-01 | 成都新柯力化工科技有限公司 | Method for preparing graphene nanoplatelets by viscously mechanical shearing and stripping |
| CN105702384A (en) * | 2016-03-24 | 2016-06-22 | 广州市尤特新材料有限公司 | Sintered high-heating paste and preparation method thereof |
| CN106084989A (en) * | 2016-06-20 | 2016-11-09 | 陈勇 | Low Temperature Far Infrared electric heating carbon is starched |
| CN106255239A (en) * | 2016-08-29 | 2016-12-21 | 江苏科暖热能科技有限公司 | A kind of floor heating Graphene electric hot plate and production method thereof |
| CN106243836A (en) * | 2016-08-15 | 2016-12-21 | 青岛德通纳米技术有限公司 | A kind of graphene conductive carbon slurry and preparation method thereof |
| CN106390295A (en) * | 2016-02-15 | 2017-02-15 | 青岛南墅泰星石墨制品有限公司 | Graphene electrothermal film health-care mat production method |
| CN106433319A (en) * | 2016-10-14 | 2017-02-22 | 中国科学院山西煤炭化学研究所 | Waterborne environment-friendly conducive carbon paste based on graphene-carbon black composite filler and preparation method |
| CN106848630A (en) * | 2017-03-08 | 2017-06-13 | 宁波高新区远创科技有限公司 | A kind of transmission line tower grounding network preparation method for being combined earthing material |
| CN108039225A (en) * | 2017-12-13 | 2018-05-15 | 常州烯材碳材料科技有限公司 | Environment-friendly type low resistance graphene carbon fiber conductive carbon paste and preparation method thereof |
| CN108260233A (en) * | 2018-01-24 | 2018-07-06 | 黄冈科瑞恩信息科技有限公司 | A kind of graphene superconductive far infrared heat generating pastes |
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| CN111393867A (en) * | 2020-04-15 | 2020-07-10 | 安徽扬子地板股份有限公司 | Special composite floor for geothermal and preparation method thereof |
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| CN109741855A (en) * | 2018-12-29 | 2019-05-10 | 长江润发中科(张家港)纳米科技有限公司 | A kind of graphene conductive slurry and preparation method thereof applied to Electric radiant Heating Film |
| CN109640410A (en) * | 2019-01-24 | 2019-04-16 | 杭州中暖科技有限公司 | A kind of preparation method of high efficiency graphene fever carbon slurry |
| CN110606968A (en) * | 2019-10-23 | 2019-12-24 | 陕西科技大学 | Preparation method of titanium dioxide/graphene flexible electrothermal film |
| CN111334026A (en) * | 2020-03-12 | 2020-06-26 | 周洪光 | PU conductive and heating carbon film and preparation method thereof |
| CN111393867A (en) * | 2020-04-15 | 2020-07-10 | 安徽扬子地板股份有限公司 | Special composite floor for geothermal and preparation method thereof |
| CN112908514A (en) * | 2021-02-22 | 2021-06-04 | 苏州英纳电子材料有限公司 | Easy-to-wipe black carbon slurry and preparation method thereof |
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