CN109741855A - A kind of graphene conductive slurry and preparation method thereof applied to Electric radiant Heating Film - Google Patents

A kind of graphene conductive slurry and preparation method thereof applied to Electric radiant Heating Film Download PDF

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Publication number
CN109741855A
CN109741855A CN201811632861.6A CN201811632861A CN109741855A CN 109741855 A CN109741855 A CN 109741855A CN 201811632861 A CN201811632861 A CN 201811632861A CN 109741855 A CN109741855 A CN 109741855A
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China
Prior art keywords
graphene conductive
parts
conductive slurry
heating film
radiant heating
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CN201811632861.6A
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刘元哲
韩文利
刘佳林
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Changjiang Runfa Zhongke (zhangjiagang) Nanotechnology Co Ltd
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Changjiang Runfa Zhongke (zhangjiagang) Nanotechnology Co Ltd
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Priority to CN201811632861.6A priority Critical patent/CN109741855A/en
Publication of CN109741855A publication Critical patent/CN109741855A/en
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Abstract

The graphene conductive slurry and preparation method thereof that the invention discloses a kind of applied to Electric radiant Heating Film, electrocondution slurry is formulated by weight, including 4-20 parts of matrix resin, 40-60 parts of esters solvent, 0.6-1.7 parts of adhesion promoter, 0.5-1.1 parts of rheological agent, auxiliary agent 1.5-2.8 parts anti-settling, 0.7-1.3 parts of powder directing agent, 0.5-1.8 parts of curing catalysts and 10-60 parts of conductive powder body.Electrocondution slurry prepared by the present invention has good antioxygenic property and acid-proof alkaline, and the 2000 hours attenuation rates that are powered are low, are applied in Electric radiant Heating Film, can significantly improve its stability in use and its service life.

Description

A kind of graphene conductive slurry and preparation method thereof applied to Electric radiant Heating Film
Technical field
The graphene conductive slurry and preparation method thereof that the present invention relates to a kind of applied to Electric radiant Heating Film, belongs to electrocondution slurry skill Art field.
Background technique
Studies have shown that Beijing PM2.5 has 6 important sources, is soil dirt, fire coal, biomass combustion, vehicle exhaust respectively With waste incineration, industrial pollution and secondary inorganic aerosol, wherein coal-fired accounting is about 18%.Pollution that caused by coal burning is to haze weather Formation produces tremendous influence.In order to reduce winter pollution that caused by coal burning, improve air quality, many cities of northern China start to push away Extensively " coal changes electricity ".It will in the past be the heating system of heating source by burning coal, be changed to be converted into the heating side of heat source by electric energy Formula.
Wherein, electric heat membrane heating is one of electrical power heat-supply mode, it is one kind using electric power as the energy, passes through infrared radiation The novel heating mode conducted heat.Electric radiant Heating Film is the conductive composite film that can be generated heat after a kind of energization.It has high pressure resistant, moisture resistance Wet, bearing temperature range is wide, high tenacity, low-shrinkage, operational safety, convenient for storage and transportation, there is far infrared human body heat efficiency Equal excellent performances.
The heating principle of Electric radiant Heating Film is one layer of carbon-based pulp layer of coating on insulating film, the left and right two on another insulating film End is fitted to together by electrocondution slurry face-to-face parallel over two copper foils, copper foil and carbon-based pulp layer, is powered at copper foil end In the case of, traditional carbon-based pulp layer is to generate heat by carbon-based pulp layer by electric current, makes to heat film temperature rising, plays confession Warm effect.
For traditional carbon-based slurry since long-time is in the condition of high temperature, heating film heat fade rate is high, uses a period of time Heating effect can sharply decline afterwards.And since heating film surface covering is PET material, and heating film long-time high temperature is easy The pyrolysis and warpage for causing covering, cause security risk.
And using heating film made of grapheme material after powered up, the carbon molecules group in graphite ene coatings generates " Blang Violent friction and shock occur between carbon molecules for movement ", and the thermal energy of generation is in the form of far infrared radiation and convection current to unofficial biography It passs, the conversion ratio of electric energy and thermal energy is up to 98% or more.And since the thermal energy overwhelming majority is transmitted in a manner of far infrared radiation To human body, heating film self-temperature can be at 50 DEG C once, and safety is high with stability.
Summary of the invention
Excellent, decaying that the technical problem to be solved by the invention is to provide a kind of antioxygenic properties and acid-proof alkaline The low graphene conductive slurry and preparation method thereof of rate.
In order to solve the above technical problems, the technical solution adopted by the present invention are as follows:
A kind of graphene conductive slurry applied to Electric radiant Heating Film, by weight, including 4-20 parts of matrix resin, esters solvent 40-60 parts, 0.6-1.7 parts of adhesion promoter, 0.5-1.1 parts of rheological agent, auxiliary agent 1.5-2.8 parts anti-settling, powder directing agent 0.7-1.3 parts, 0.5-1.8 parts of curing catalysts and 10-60 parts of conductive powder body.
Described matrix resin is selected from modified polyester resin, modified epoxy, polyurethane resin, EVA, polyester resin or has Machine silicone resin.
It is described to be selected from DBE, ethyl acetate, butyl acetate, diethylene glycol ether acetate, butyl glycol ether, glutaric acid two One of methyl esters, dimethyl adipate or dimethyl succinate are a variety of.
The adhesion promoter is selected from silane coupling agent, titanate coupling agent, aluminate coupling agent or rare-earth coupling agent.
The rheological agent is selected from palygorskite clay, bentonite, organic clay, cellulose, polyvinylpyrrolidone, dodecane Base sodium sulfonate, Span 80 or xanthan gum.
The anti-settling auxiliary agent is selected from polyethylene wax, nano-particle carbon or fumed silica.
The powder directing agent is selected from BYK410 or PN411.
The curing catalysts are selected from blocked isocyanate, dicyandiamide or platinum catalyst.
The conductive powder body is a kind of or more in multi-layer graphene micro mist, single-layer graphene micro mist, superconductive carbon black powder Kind.
A kind of preparation method of the graphene conductive slurry applied to Electric radiant Heating Film is based on above-mentioned electrocondution slurry formula, including Following steps:
(1) preparation of macromolecule resin carrier weighs matrix resin according to formula ratio and solvent is mixed, in 70- Be completely dissolved at 90 DEG C, by above-mentioned macromolecule resin carrier on 400-800 mesh screen filtering and impurity removing, obtain macromolecule resin load Body detects its viscosity number, it is desirable that is worth for 100-5000cps;
(2) preparation of graphene conductive slurry weighs conductive powder body according to formula ratio, adhesion promoter, rheological agent, prevents The macromolecule resin carrier of the step of heavy auxiliary agent, powder directing agent, curing catalysts and 20-50wt% (1) preparation, by above-mentioned original Material is sufficiently mixed in batch mixer, obtains premix, then premix is carried out to high speed shear grinding point in grinder It dissipates, obtains graphene conductive slurry;
(3) post-processing of graphene conductive slurry, the graphene conductive slurry that step (2) is obtained pass through 100-300 mesh The screen to filtrate removes impurity or the non-uniform larger particles of dispersion in slurry, is then placed in the conductive silver paste filtered In vacuum degasing machine, to get the graphene conductive slurry after vacuumizing, its viscosity number is detected, it is desirable that be worth for 300- 30000cps。
Advantageous effects of the invention:, volume electricity extremely low using graphene conductive slurry resistance prepared by the present invention Resistance rate minimum 0.1 Ω cm of < is stored 1500 hours under hot and humid environment and is not aoxidized, and appearance is good in salt spray test, electricity Resistive < 10%, adhesive force 4B, the 2000 hours resistance of being powered rise < 10%, illustrate it with extremely strong inoxidizability, resistance to Acid-alkali salt performance and extremely low energization attenuation rate can effectively improve the stability in use and service life of Electric radiant Heating Film, and And gravure printing technique coating can be used in graphene conductive slurry prepared by the present invention, compares silk-screen printing technique, can significantly mention It rises production efficiency and reduces production loss.
Specific embodiment
The invention will be further described below.Following embodiment is only used for clearly illustrating technical side of the invention Case, and not intended to limit the protection scope of the present invention.
Graphene conductive slurry preparation method is specific as follows in the present invention:
Step (1) weighs 6% matrix resin by mass percentage and 40% solvent is mixed, and at 85 DEG C Dissolution completely, obtain macromolecule resin carrier, then by above-mentioned macromolecule resin carrier on 800 mesh screens filtering and impurity removing, obtain To final macromolecule resin carrier, detector viscosity number, it is desirable that be worth for 100-5000cps, under off-limits product does not enter One process;
Step (2) weighs the final macromolecule resin of conductive powder body, each additive and step (1) preparation according to formula ratio Above-mentioned weighed raw material is sufficiently mixed in batch mixer first, obtains premix, then grinding premix by carrier High speed shear grinding distribution is carried out in machine, obtains graphene conductive slurry;
Obtained graphene conductive slurry by 100 mesh net filtrations, is removed the impurity in slurry or divided by step (3) Non-uniform larger particles are dissipated, then the graphene conductive slurry head filtered are placed in vacuum degasing machine, after vacuumizing, i.e., The graphene conductive slurry, detector viscosity number, it is desirable that be worth for 300-30000cps, under off-limits product does not enter One process;
Detection method:
(1) volume resistivity measures;Resistivity tester;
(2) high temperature and humidity is tested: being stored 1500 hours under 85 DEG C of temperature, 85% humidity;
(3) salt mist experiment: under 35 ± 2 DEG C of air-proof condition, ambient humidity is greater than 80%, and pH value is in 6.5-7.2 range It is interior, with 5% ± 1% NaCl brine spray 72h;
(4) attenuation rate test: 25 ± 2 DEG C of environment temperature, ambient humidity 40 ± 20% air-proof condition under, to graphene Conductive coating both ends apply the voltage of 5V, are powered 2000 hours.
Table 1 is each embodiment composition proportion
Electrocondution slurry prepared in the above embodiments is through detecting: volume resistivity < 1 × 10-5Ω cm, in high temperature and humidity ring It stores 1500 hours and does not aoxidize under border, appearance is good in salt mist experiment, resistance variations < 10%, 4B grades of adhesive force, is powered Resistance rises < 10% within 2000 hours.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations Also it should be regarded as protection scope of the present invention.

Claims (10)

1. a kind of graphene conductive slurry applied to Electric radiant Heating Film, characterized in that by weight, including 4-20 parts of matrix resin, 40-60 parts of esters solvent, 0.6-1.7 parts of adhesion promoter, 0.5-1.1 parts of rheological agent, auxiliary agent 1.5-2.8 parts anti-settling, powder 0.7-1.3 parts of directing agent, 0.5-1.8 parts of curing catalysts and 10-60 parts of conductive powder body.
2. a kind of graphene conductive slurry applied to Electric radiant Heating Film according to claim 1, characterized in that described matrix tree Rouge is selected from modified polyester resin, modified epoxy, polyurethane resin, EVA, polyester resin or organic siliconresin.
3. a kind of graphene conductive slurry applied to Electric radiant Heating Film according to claim 1, characterized in that described to be selected from DBE, ethyl acetate, butyl acetate, diethylene glycol ether acetate, butyl glycol ether, dimethyl glutarate, dimethyl adipate Or one of dimethyl succinate or a variety of.
4. a kind of graphene conductive slurry applied to Electric radiant Heating Film according to claim 1, characterized in that the adhesive force Promotor is selected from silane coupling agent, titanate coupling agent, aluminate coupling agent or rare-earth coupling agent.
5. a kind of graphene conductive slurry applied to Electric radiant Heating Film according to claim 1, characterized in that the rheological agent Selected from palygorskite clay, bentonite, organic clay, cellulose, polyvinylpyrrolidone, dodecyl sodium sulfate, Span 80 or Xanthan gum.
6. a kind of graphene conductive slurry applied to Electric radiant Heating Film according to claim 1, characterized in that described anti-settling to help Agent is selected from polyethylene wax, nano-particle carbon or fumed silica.
7. a kind of graphene conductive slurry applied to Electric radiant Heating Film according to claim 1, characterized in that the powder is fixed BYK410 or PN411 is selected to agent.
8. a kind of graphene conductive slurry applied to Electric radiant Heating Film according to claim 1, characterized in that the solidification is urged Agent is selected from blocked isocyanate, dicyandiamide or platinum catalyst.
9. a kind of graphene conductive slurry applied to Electric radiant Heating Film according to claim 1, characterized in that the conducting powder Body is one or more in multi-layer graphene micro mist, single-layer graphene micro mist, superconductive carbon black powder.
10. a kind of preparation method of the graphene conductive slurry applied to Electric radiant Heating Film, characterized in that appointed based on claim 1-9 Graphene conductive formula of size described in one, comprising the following steps:
(1) preparation of macromolecule resin carrier weighs matrix resin according to formula ratio and solvent is mixed, at 70-90 DEG C Under be completely dissolved, by above-mentioned macromolecule resin carrier on 400-800 mesh screen filtering and impurity removing, obtain macromolecule resin carrier, Detect its viscosity number, it is desirable that be worth for 100-5000cps;
(2) preparation of graphene conductive slurry weighs conductive powder body according to formula ratio, adhesion promoter, rheological agent, anti-settling helps The macromolecule resin carrier of the step of agent, powder directing agent, curing catalysts and 20-50wt% (1) preparation, above-mentioned raw materials are existed It is sufficiently mixed in batch mixer, obtains premix, then premix is carried out in grinder to high speed shear grinding distribution, obtained To electrocondution slurry;
(3) post-processing of graphene conductive slurry, the graphene conductive slurry that step (2) is obtained pass through 100-300 mesh screen Filtering removes impurity or the non-uniform larger particles of dispersion in slurry, then sets the graphene conductive slurry filtered In vacuum degasing machine, to get the graphene conductive slurry after vacuumizing, its viscosity number is detected, it is desirable that be worth for 300- 30000cps。
CN201811632861.6A 2018-12-29 2018-12-29 A kind of graphene conductive slurry and preparation method thereof applied to Electric radiant Heating Film Pending CN109741855A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110570972A (en) * 2019-08-28 2019-12-13 北京中科纳通电子技术有限公司 Conductive paste applied to metal grid transparent conductive film and preparation method thereof
CN111436168A (en) * 2020-01-14 2020-07-21 北京服装学院 Graphene electrical heating slurry, graphene electrical heating film and preparation method and application thereof
CN111520670A (en) * 2020-05-11 2020-08-11 常州大学 Fresnel lighting power generation ventilation heating system suitable for cave dwelling
CN111944419A (en) * 2020-07-20 2020-11-17 广州精卓化工有限公司 Low-temperature cured electrically-induced thermal conductive slurry and preparation method thereof
CN114316769A (en) * 2021-12-31 2022-04-12 烯泽韩力石墨烯应用科技(无锡)有限公司 Graphene PTC (Positive temperature coefficient) electrothermal film slurry, preparation method thereof and electrothermal film
CN114350000A (en) * 2022-01-17 2022-04-15 归壹生命科技(东莞)有限公司 Manufacturing process of graphene electric heating silica gel sheet
CN114582543A (en) * 2021-11-05 2022-06-03 北京中科纳通电子技术有限公司 Formula and preparation method of hole-filling conductive slurry

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CN103915134A (en) * 2014-04-17 2014-07-09 江南石墨烯研究院 Method for preparing environment-friendly graphene-based conductive carbon paste
CN105505161A (en) * 2015-09-30 2016-04-20 无锡同创石墨烯应用科技有限公司 Graphite-modified water-based conductive coating composition and preparation method thereof
CN108084823A (en) * 2017-12-18 2018-05-29 中南大学 A kind of electric-heating coatings and its preparation method and application
CN109102962A (en) * 2018-07-03 2018-12-28 北京中科纳通电子技术有限公司 The Preparation method and use of conductive rubber strip

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN103915134A (en) * 2014-04-17 2014-07-09 江南石墨烯研究院 Method for preparing environment-friendly graphene-based conductive carbon paste
CN105505161A (en) * 2015-09-30 2016-04-20 无锡同创石墨烯应用科技有限公司 Graphite-modified water-based conductive coating composition and preparation method thereof
CN108084823A (en) * 2017-12-18 2018-05-29 中南大学 A kind of electric-heating coatings and its preparation method and application
CN109102962A (en) * 2018-07-03 2018-12-28 北京中科纳通电子技术有限公司 The Preparation method and use of conductive rubber strip

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110570972A (en) * 2019-08-28 2019-12-13 北京中科纳通电子技术有限公司 Conductive paste applied to metal grid transparent conductive film and preparation method thereof
CN111436168A (en) * 2020-01-14 2020-07-21 北京服装学院 Graphene electrical heating slurry, graphene electrical heating film and preparation method and application thereof
CN111520670A (en) * 2020-05-11 2020-08-11 常州大学 Fresnel lighting power generation ventilation heating system suitable for cave dwelling
CN111944419A (en) * 2020-07-20 2020-11-17 广州精卓化工有限公司 Low-temperature cured electrically-induced thermal conductive slurry and preparation method thereof
CN114582543A (en) * 2021-11-05 2022-06-03 北京中科纳通电子技术有限公司 Formula and preparation method of hole-filling conductive slurry
CN114316769A (en) * 2021-12-31 2022-04-12 烯泽韩力石墨烯应用科技(无锡)有限公司 Graphene PTC (Positive temperature coefficient) electrothermal film slurry, preparation method thereof and electrothermal film
CN114350000A (en) * 2022-01-17 2022-04-15 归壹生命科技(东莞)有限公司 Manufacturing process of graphene electric heating silica gel sheet

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