CN109817385A - A kind of preparation method that environment-friendly type graphene conductive carbon is starched and its application on flexible heating film - Google Patents
A kind of preparation method that environment-friendly type graphene conductive carbon is starched and its application on flexible heating film Download PDFInfo
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Abstract
The present invention relates to graphene conductive technical field of material, the preparation method of specifically a kind of environment-friendly type graphene conductive carbon slurry and its application on flexible heating film, comprising the following steps: stir conductive carbon black, graphene powder, dispersing agent, adhesion promoter, defoaming agent and the first solvent to obtain inorganic filler in dispersion machine；It weighs polyester resin and acrylic resin is added to stirring in the second solvent and forms mixture；Inorganic filler and said mixture are added to stirring evenly in blender, the conductive carbon paste slurry to get environment-friendly type is then ground, which is coated on substrate, and depends on substrate and is wrapped in the outer surface of heat pipeline to be added and play the role of heating and thermal insulation.Resistance value is highly stable after heating by the present invention, and surface heat temperature is uniform, used solvent and all environmentally friendly solvents of auxiliary agent, lays a good foundation for environment-friendly type graphene conductive carbon slurry.
Description
Technical field
The present invention relates to graphene conductive technical field of material, specifically a kind of environment-friendly type graphene conductive carbon slurry
Preparation method and its application on flexible heating film.
Background technique
Electrocondution slurry is to be distributed evenly in thermoplasticity or thermosetting resin with the carbon system particle of nonmetal conductor material
The thick electrically conductive ink of middle formation.After being heating and curing, ink film layer is not oxidizable, and performance is stablized；Acid and alkali resistance and solvent corrosion,
Protection and conductive effect can be played.The adhesive force of ink is strong, antistripping, with metal, glass-cloth board and Vc, PET and PC piece
Material is well combined.With having in the fields such as solar battery, supercapacitor, energy catalysis to electrode for electrocondution slurry production
Actual application.Electrocondution slurry is a kind of composite material being made of binder, conductive filler, solvent and auxiliary agent.Wherein, it bonds
Agent is the film forming matter of electrocondution slurry, and in a binder, formed has the suitable of certain viscosity and rheological behavior to dispersing conductive fine particles
Close the suspended substance of silk-screen printing or coating.Electrocondution slurry is as a kind of intermediate products, after silk-screen printing or thin film cladding
It needs to finally obtain conductive film layer through completion of cure at a certain temperature after a period of time.
Currently, the report about conductive carbon paste is also relatively more, such as: application No. is 201010297360.4 patents to disclose
A kind of High-conductivity carbon slurry and preparation method thereof, but the conductive film obtained using the conductive carbon paste, film layer are easy to appear stomata；Shen
Number it please disclose for 201110180193.X a patent and a kind of heat is distributed evenly in the carbon system particle of nonmetal conductor material
Electrically conductive ink obtained from plastic resin, but the electrically conductive ink dissolvent residual that the method obtains is higher, and then influences its electric conductivity
Energy；Application No. is the conductive carbon pastes of 201310108657.5 patent disclosure, using ethyl acetate as solvent, conductive carbon powder and change
Property nano-sized carbon as conductive material, still, the conductive film thicknesses of layers that is prepared of conductive carbon paste of this method preparation is easy not
?.Application No. is: 201711324606.0 patent disclose a kind of environment-friendly type low resistance graphene carbon fiber conductive carbon paste and
Preparation method has obtained the carbon fiber guiding electrical carbon slurry that a kind of good conductivity, internal resistance is small, carbon material is evenly distributed, is easy to coat,
But it applies a large amount of organic solvent, hence it is evident that not environmentally friendly enough.
Summary of the invention
In order to solve the above technical problems, The present invention provides a kind of environment-friendly type graphene conductive carbon slurry preparation method,
The graphene conductive carbon slurry solvent of this method preparation uses environmentally friendly solvent, and product dissolvent residual is less, and electric conductivity is excellent,
Conductive film thicknesses of layers is uniform.
The technical solution for solving above-mentioned technical problem is as follows:
A kind of preparation method of environment-friendly type graphene conductive carbon slurry, comprising the following steps:
(1) preparation of inorganic filler:
By weight percentage, according to following component ingredient: 5~15% conductive carbon black, 20~40% Graphene powder
Body, 1~2% BYK Series Dispersant, 1~2% adhesion promoter, 1~2% defoaming agent and the first of 40~60%
Solvent；Then these substances are sufficiently stirred in dispersion machine until being uniformly dispersed；
(2) preparation of organic carrier:
According to quality meter, 1 part of polyester resin is weighed respectively and 1 part of acrylic resin is added in 3 part of second solvent, is placed in
It heats and is sufficiently stirred in electric heating reacting kettle, be dissolved completely in polyester resin and acrylic resin in solvent and formed uniformly
Mixture；
(3) preparation of conductive carbon paste:
It will be stirred in the inorganic filler that step (1) obtains and the organic carrier that step (2) obtains all addition to blender
Then 30~35min weighs 1-1.2 kilograms of mixture until being uniformly mixed, be placed in sand mill and grind 1h, so repeats,
Pack the conductive carbon paste slurry up to environment-friendly type.
It further says, the production method of the graphene powder are as follows: graphene oxide filter cake is dispersed in water, is added
Entering dispersing agent is sufficiently mixed it with graphene oxide, is then centrifuged mixture, dry, obtained after reduction partial size be 10~
The graphene powder of 100nm；
The dispersing agent is sodium citrate or neopelex；
The mass ratio of the graphene oxide and dispersing agent is 50-90:1.
It further says, the adhesion promoter is BNK-NSF364 environment-friendly type adhesion promoter.
It further says, it according to mass ratio is 1:1- that the defoaming agent, which is nano-titanium dioxide and nano silica,
1.2 mixture.
It further says, the first solvent described in step (1) is liquid carbon dioxide.
Furthermore, the second solvent described in step (2) is ethyl alcohol, n-butanol, any one in isopropanol.
It is a further object to provide a kind of environmental protection of the preparation method preparation of environment-friendly type graphene conductive carbon slurry
Environment-friendly type graphene conductive carbon slurry slurry is coated on substrate surface and flexible heating film is made by the application of type graphene conductive carbon slurry
Heating and thermal insulation is carried out to pipeline；The following steps are included:
Environment-friendly type graphene conductive carbon slurry slurry is coated on the substrate of PET/PI by gravure techniques, the substrate
Surface is circumferentially bonded with metal current-carrying conductive layer, and the width of the metal current-carrying item is 0.5-1.5cm, environment-friendly type graphene
Conductive carbon paste coating is wound after 120 DEG C of drying, is then covered one layer of PI film again in coating surface, is obtained flexible heating film, this is soft
Heat pyrexia film is wrapped in the outer surface of heat pipeline to be added, so that the outer surface of environment-friendly type graphene conductive carbon slurry and heat pipeline to be added
It directly contacts, plays the role of to pipe tracing.
The beneficial effects of the present invention are:
Conductive carbon paste performance prepared by the present invention is using its square resistance as evaluation index.Square resistance is a pros
Resistance between shape thin film of conductive material edge to edge, specific test method are as follows: conductive carbon paste is through being screen-printed to PET base material
On, drying machine after dry half an hour, carries out sheet resistance test, the partial size of carbon slurry to it with four-point probe at 120 DEG C
At 8-9 μm, the sheet resistance of product of the present invention is 5-10 Ω/sq, lower than conductive carbon paste product at present on the market.And in heating
Resistance value is highly stable afterwards, and surface heat temperature is uniform, by the electrocondution slurry be coated on substrate on, and depend on substrate be wrapped in
Play the role of heating and thermal insulation in the outer surface of heating pipe.Resistance value is highly stable after heating by the present invention, surface heat temperature
Degree uniformly, lay a good foundation for environment-friendly type graphene conductive carbon slurry by used solvent and all environmentally friendly solvents of auxiliary agent.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the grain size distribution of product of the present invention；
Specific embodiment
Embodiment 1:
A kind of preparation method of environment-friendly type graphene conductive carbon slurry, comprising the following steps:
(1) preparation of inorganic filler:
By weight percentage, according to following component ingredient: 5% conductive carbon black, 30% graphene powder, 2%
BYK Series Dispersant, 1% adhesion promoter, 2% defoaming agent and 60% liquid carbon dioxide；Then by these objects
Matter is sufficiently stirred until being uniformly dispersed in dispersion machine；
(2) preparation of organic carrier:
According to quality meter, 1 part of polyester resin is weighed respectively and 1 part of acrylic resin is added in 3 parts of ethyl alcohol, be placed in electricity and add
It heats and is sufficiently stirred in thermal response kettle, be dissolved completely in polyester resin and acrylic resin in solvent and form uniform mixing
Object；
(3) preparation of conductive carbon paste:
It will be stirred in the inorganic filler that step (1) obtains and the organic carrier that step (2) obtains all addition to blender
Then 30min weighs 1 kilogram of mixture until being uniformly mixed, be placed in sand mill and grind 1h, so repeats, packs to obtain the final product
The conductive carbon paste slurry of environment-friendly type.
The production method of graphene powder are as follows: be dispersed in water graphene oxide filter cake, dispersing agent, which is added, makes itself and oxygen
Graphite alkene is sufficiently mixed, and is then centrifuged mixture, dry, and the graphene powder that partial size is 10nm is obtained after reduction；Dispersion
Agent is sodium citrate；The mass ratio of graphene oxide and dispersing agent is 50:1.
Adhesion promoter is BNK-NSF364 environment-friendly type adhesion promoter.
Defoaming agent is the mixture that nano-titanium dioxide and nano silica are 1:1 according to mass ratio.
Flexible heating film is made coated on substrate surface in environment-friendly type graphene conductive carbon slurry slurry to heat pipeline
Heat preservation, comprising the following steps:
By environment-friendly type graphene conductive carbon slurry slurry by gravure techniques coated on the substrate of PET, the surface of substrate is all
To metal current-carrying conductive layer is bonded with, the width of metal current-carrying item is 0.5cm, and environment-friendly type graphene conductive carbon starches coating warp
It is wound after 120 DEG C of drying, then covers one layer of PI film again in coating surface, obtain flexible heating film, which is wrapped in
It is played so that environment-friendly type graphene conductive carbon slurry is directly contacted with the outer surface of heat pipeline to be added the outer surface of heat pipeline to be added
Effect to pipe tracing.
Embodiment 2:
A kind of preparation method of environment-friendly type graphene conductive carbon slurry, comprising the following steps:
(1) preparation of inorganic filler:
By weight percentage, according to following component ingredient: 15% conductive carbon black, 40% graphene powder, 2%
BYK Series Dispersant, 2% adhesion promoter, 1% defoaming agent and 40% liquid carbon dioxide；Then by these objects
Matter is sufficiently stirred until being uniformly dispersed in dispersion machine；
(2) preparation of organic carrier:
According to quality meter, 1 part of polyester resin is weighed respectively and 1 part of acrylic resin is added in 3 parts of n-butanols, is placed in electricity
It heats and is sufficiently stirred in heating reaction kettle, so that polyester resin and acrylic resin is dissolved completely in formation in solvent uniform mixed
Close object；
(3) preparation of conductive carbon paste:
It will be stirred in the inorganic filler that step (1) obtains and the organic carrier that step (2) obtains all addition to blender
Then 35min weighs 1.2 kilograms of mixture until being uniformly mixed, be placed in sand mill and grind 1h, so repeats, and packaging is
Obtain the conductive carbon paste slurry of environment-friendly type.
The production method of graphene powder are as follows: be dispersed in water graphene oxide filter cake, dispersing agent, which is added, makes itself and oxygen
Graphite alkene is sufficiently mixed, and is then centrifuged mixture, dry, and the graphene powder that partial size is 100nm is obtained after reduction；Dispersion
Agent is neopelex；The mass ratio of graphene oxide and dispersing agent is 90:1.
Adhesion promoter is BNK-NSF364 environment-friendly type adhesion promoter.
Defoaming agent is the mixture that nano-titanium dioxide and nano silica are 1:1.2 according to mass ratio.
Flexible heating film is made coated on substrate surface in environment-friendly type graphene conductive carbon slurry slurry to heat pipeline
Heat preservation, comprising the following steps:
By environment-friendly type graphene conductive carbon slurry slurry by gravure techniques coated on the substrate of PI, the surface of substrate is circumferential
It is bonded with metal current-carrying conductive layer, the width of metal current-carrying item is 1.5cm, and environment-friendly type graphene conductive carbon starches coating through 120
DEG C drying after wind, then cover one layer of PI film again in coating surface, obtain flexible heating film, which is wrapped in be added
It plays so that environment-friendly type graphene conductive carbon slurry is directly contacted with the outer surface of heat pipeline to be added to pipe the outer surface of heat pipeline
The effect of road heating and thermal insulation.
Embodiment 3:
A kind of preparation method of environment-friendly type graphene conductive carbon slurry, comprising the following steps:
(1) preparation of inorganic filler:
By weight percentage, according to following component ingredient: 10% conductive carbon black, 25% graphene powder, 1%
BYK Series Dispersant, 2% adhesion promoter, 2% defoaming agent and 60% liquid carbon dioxide；Then by these objects
Matter is sufficiently stirred until being uniformly dispersed in dispersion machine；
(2) preparation of organic carrier:
According to quality meter, 1 part of polyester resin is weighed respectively and 1 part of acrylic resin is added in 3 parts of isopropanols, is placed in electricity
It heats and is sufficiently stirred in heating reaction kettle, so that polyester resin and acrylic resin is dissolved completely in formation in solvent uniform mixed
Close object；
(3) preparation of conductive carbon paste:
It will be stirred in the inorganic filler that step (1) obtains and the organic carrier that step (2) obtains all addition to blender
Then 35min weighs 1 kilogram of mixture until being uniformly mixed, be placed in sand mill and grind 1h, so repeats, packs to obtain the final product
The conductive carbon paste slurry of environment-friendly type.
The production method of graphene powder are as follows: be dispersed in water graphene oxide filter cake, dispersing agent, which is added, makes itself and oxygen
Graphite alkene is sufficiently mixed, and is then centrifuged mixture, dry, and the graphene powder that partial size is 50nm is obtained after reduction；Dispersion
Agent is sodium citrate；The mass ratio of graphene oxide and dispersing agent is 80:1.
Adhesion promoter is BNK-NSF364 environment-friendly type adhesion promoter.
Defoaming agent is the mixture that nano-titanium dioxide and nano silica are 1:1.2 according to mass ratio.
Flexible heating film is made coated on substrate surface in environment-friendly type graphene conductive carbon slurry slurry to heat pipeline
Heat preservation, comprising the following steps:
By environment-friendly type graphene conductive carbon slurry slurry by gravure techniques coated on the substrate of PET, the surface of substrate is all
To metal current-carrying conductive layer is bonded with, the width of metal current-carrying item is 1cm, and environment-friendly type graphene conductive carbon starches coating through 120
DEG C drying after wind, then cover one layer of PI film again in coating surface, obtain flexible heating film, which is wrapped in be added
It plays so that environment-friendly type graphene conductive carbon slurry is directly contacted with the outer surface of heat pipeline to be added to pipe the outer surface of heat pipeline
The effect of road heating and thermal insulation.
The above is only presently preferred embodiments of the present invention, not does limitation in any form to the present invention, it is all according to
According to any simple modification to the above embodiments in technical spirit of the invention, equivalent variations, guarantor of the invention is each fallen within
Within the scope of shield.
Claims (8)
1. a kind of preparation method of environment-friendly type graphene conductive carbon slurry, which comprises the following steps:
(1) preparation of inorganic filler:
By weight percentage, according to following component ingredient: 5~15% conductive carbon black, 20~40% graphene powder, 1
~2% BYK Series Dispersant, 1~2% adhesion promoter, 1~2% defoaming agent and 40~60% the first solvent；
Then these substances are sufficiently stirred in dispersion machine until being uniformly dispersed；
(2) preparation of organic carrier:
According to quality meter, 1 part of polyester resin is weighed respectively and 1 part of acrylic resin is added in 3 part of second solvent, be placed in electricity and add
It heats and is sufficiently stirred in thermal response kettle, be dissolved completely in polyester resin and acrylic resin in solvent and form uniform mixing
Object；
(3) preparation of conductive carbon paste:
Will inorganic filler that step (1) obtains and organic carrier that step (2) obtains all be added to stirring 30 in blenders~
Then 35min weighs 1-1.2 kilograms of mixture until being uniformly mixed, be placed in sand mill and grind 1h, so repeats, packaging
Slurry is starched up to environment-friendly type graphene conductive carbon.
2. the preparation method of environment-friendly type graphene conductive carbon slurry according to claim 1, which is characterized in that the graphite
The production method of alkene powder are as follows: be dispersed in water graphene oxide filter cake, dispersing agent, which is added, keeps it abundant with graphene oxide
Mixture, is then centrifuged by mixing, dry, and the graphene powder that partial size is 10~100nm is obtained after reduction；
The dispersing agent is sodium citrate or neopelex；
The mass ratio of the graphene oxide and dispersing agent is 50-90:1.
3. the preparation method of environment-friendly type graphene conductive carbon slurry according to claim 1, which is characterized in that the attachment
Power promotor is BNK-NSF364 environment-friendly type adhesion promoter.
4. the preparation method of environment-friendly type graphene conductive carbon slurry according to claim 1, which is characterized in that the defoaming
Agent is the mixture that nano-titanium dioxide and nano silica are 1:1-1.2 according to mass ratio.
5. the preparation method of environment-friendly type graphene conductive carbon slurry according to claim 1, which is characterized in that in step (1)
First solvent is liquid carbon dioxide.
6. the preparation method of environment-friendly type graphene conductive carbon slurry according to claim 1, which is characterized in that in step (2)
Second solvent is ethyl alcohol, n-butanol, any one in isopropanol.
7. a kind of environment-friendly type of the preparation method preparation of environment-friendly type graphene conductive carbon slurry as claimed in any one of claims 1 to 6
The application of graphene conductive carbon slurry, which is characterized in that environment-friendly type graphene conductive carbon slurry slurry is made coated on substrate surface
Flexible heating film carries out heating and thermal insulation to pipeline.
8. application according to claim 7, which comprises the following steps:
Environment-friendly type graphene conductive carbon slurry slurry is coated on the substrate of PET/PI by gravure techniques, the surface of the substrate
It is circumferentially bonded with metal current-carrying conductive layer, the width of the metal current-carrying item is 0.5-1.5cm, environment-friendly type graphene conductive
Carbon is starched coating and is wound after 120 DEG C of drying, then covers one layer of PI film again in coating surface, obtains flexible heating film, flexibility hair
Hotting mask is wrapped in the outer surface of heat pipeline to be added, so that environment-friendly type graphene conductive carbon slurry is direct with the outer surface of heat pipeline to be added
Contact, plays the role of to pipe tracing.
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| CN110911031A (en) * | 2019-10-21 | 2020-03-24 | 珠海烯蟀科技有限公司 | Device with conducting strip as graphene layer power supply electrode |
| CN110944416A (en) * | 2019-10-29 | 2020-03-31 | 珠海烯蟀科技有限公司 | Graphene composite slurry, heating coating and preparation method thereof |
| CN111447699A (en) * | 2020-04-15 | 2020-07-24 | 广东康烯科技有限公司 | Flexible graphene heating film and preparation method thereof |
| CN112164489A (en) * | 2020-09-04 | 2021-01-01 | 苏州烯时代材料科技有限公司 | Conductive carbon paddle for blood glucose test paper, preparation method of conductive carbon paddle and blood glucose test paper |
| CN112543518A (en) * | 2020-12-03 | 2021-03-23 | 元普(苏州)新材料科技有限公司 | Graphene flexible heating material and preparation method thereof |
| CN112694774A (en) * | 2021-01-21 | 2021-04-23 | 湖南翰坤实业有限公司 | Environment-friendly energy-saving nano graphene heating coating and preparation method thereof |
| CN113871094A (en) * | 2020-06-30 | 2021-12-31 | 三元科技（深圳）有限公司 | Coating method of conductive coating of circuit and cable with conductive coating |
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| CN112164489B (en) * | 2020-09-04 | 2022-04-19 | 苏州烯时代材料科技有限公司 | Conductive carbon paste for blood glucose test paper, preparation method thereof and blood glucose test paper |
| WO2022061997A1 (en) * | 2020-09-25 | 2022-03-31 | 欧菲光集团股份有限公司 | Conductive ink, ultrasonic fingerprint module, and electronic device |
| CN112543518B (en) * | 2020-12-03 | 2021-06-25 | 元普(苏州)新材料科技有限公司 | Graphene flexible heating material and preparation method thereof |
| CN112543518A (en) * | 2020-12-03 | 2021-03-23 | 元普(苏州)新材料科技有限公司 | Graphene flexible heating material and preparation method thereof |
| CN112694774A (en) * | 2021-01-21 | 2021-04-23 | 湖南翰坤实业有限公司 | Environment-friendly energy-saving nano graphene heating coating and preparation method thereof |
| CN114205937A (en) * | 2022-01-17 | 2022-03-18 | 归壹生命科技(东莞)有限公司 | Manufacturing process of graphene electric heating PI (polyimide) membrane |
| CN116376341A (en) * | 2023-03-08 | 2023-07-04 | 安徽宇航派蒙健康科技股份有限公司 | Conductive filler, conductive film, electrothermal film and preparation method |
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