CN103665866A - Preparation method for graphene-polyimide composite film - Google Patents

Preparation method for graphene-polyimide composite film Download PDF

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Publication number
CN103665866A
CN103665866A CN201310685647.8A CN201310685647A CN103665866A CN 103665866 A CN103665866 A CN 103665866A CN 201310685647 A CN201310685647 A CN 201310685647A CN 103665866 A CN103665866 A CN 103665866A
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graphene
acid anhydride
polyamic acid
preparation
composite film
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CN103665866B (en
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岑建军
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Ningbo Jinshan New Material Co ltd
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NINGBO JINSHAN ELECTRONIC MATERIALS CO Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003—Preparatory processes
    • C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1046—Polyimides containing oxygen in the form of ether bonds in the main chain
    • C08G73/105—Polyimides containing oxygen in the form of ether bonds in the main chain with oxygen only in the diamino moiety
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a preparation method for a graphene-polyimide composite film. The preparation method comprises the following steps: adopting graphene and polyamide acid prepared through enabling 4, 4-diaminodiphenyl ether and pyromellitic acid dianhydride to be subjected to polycondensation in a solvent; adding dispersed graphene suspension liquid into the polyamide acid prepared through polycondensation reaction, dispersing circularly for 10-16 hours, adjusting the molar ratio of amine to anhydride in the polyamide acid to (1:0.98)-(1:0.995), and enabling the viscosity to reach 60000 CP-90000 CP, wherein the graphene is 1-15% of the solid content of the polyamide acid; then, defoaming and casting for forming the film; finally, performing imidization, rolling and slitting. According to the graphene-polyimide composite film prepared by the preparation method, the tensile strength is not less than 100 Mpa, the heat-conducting property is not less than 5w/m.k, and the elongation at break is not less than 15%.

Description

The preparation method of Graphene polyimide composite film
Technical field
The present invention relates to a kind of preparation method of Graphene polyimide composite film.
Background technology
Kapton (PI film) is since dropping into application the sixties in last century, and with its excellent thermal characteristics, dielectric properties and mechanical property etc. become the preferred material of the industrial circles such as electronics and space flight.Along with the development of high and new technology, common polyimide material can not meet the requirement of the manufacture of high-new technology products to material property, therefore the polyimide modified focus that just becomes present research.Inorganic component is introduced in polyimide matrix and reached the compound of inorganic-organic performance, become in its modification work comparatively effective means.
There are some researches show, only add micro-Graphene and just can produce larger lifting to the capacity of heat transmission of resin matrix and linear expansivity, greatly strengthen and widened its Application Areas.Yet for the relevant research and development of Graphene/composite polyimide material but seldom, and its heat conductivility of the material of developing is at present poor, is generally less than 0.5w/m.k, cannot be satisfied with well the demand on market.
Summary of the invention
The object of the invention is to provide in order to solve above-mentioned the deficiencies in the prior art the preparation method of the better Graphene polyimide composite film of a kind of heat conductivility.
To achieve these goals, the preparation method of the Graphene polyimide composite film that the present invention is designed, comprise adopt Graphene and by diamine and binary acid anhydride in solvent polycondensation and polyamic acid, its concrete steps are as follows:
Step 1: first by 1 part of Graphene by milling, disperseing, disperse particle diameter to reach below 100nm, be distributed to equably in 9 parts of dimethylacetamide solvents, then in above-mentioned suspension, add again 1 part of polyamic acid, continue to disperse, finally obtain graphene suspension;
Step 2: using as 4 of diamine, 4-diaminodiphenyl oxide and be simultaneously dissolved in dimethylacetamide solvent as the pyromellitic acid anhydride of binary acid anhydride, wherein 4, it is 1:0.80 ~ 1:0.90 proportioning that part of 4-diaminodiphenyl oxide and pyromellitic acid anhydride take the mole number of amine and the mole number of acid anhydride, then above-mentioned scattered graphene suspension is joined in the above-mentioned polyamic acid obtaining through polycondensation, through circulation, disperse, continue 10 hours ~ 16 hours, again the mol ratio of amine in polyamic acid and acid anhydride is transferred to 1:0.98 ~ 1:0.995, viscosity reaches 60000 CP ~ 90000 CP, wherein Graphene ratio in the solid content of polyamic acid is 1% ~ 15%,
Step 3: by above-mentioned polymkeric substance deaeration casting film-forming, last imidization, rolling are cut.
The Graphene polyimide composite film that the present invention obtains, has the groups such as hydroxyl, carboxyl due to Graphene surface, can with polyimide on group form hydrogen bond, both consistencies are good, make being dispersed in polyimide matrix of graphene uniform; In addition polyimide matrix Stability Analysis of Structures, good heat conductivility and conductivity that Graphene has,, can improve heat conductivility and the specific inductivity of polyimide, tensile strength >=the 100Mpa of the laminated film obtaining, heat conductivility >=5w/m.k, elongation at break >=15%.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1:
The preparation method of Graphene polyimide composite film provided by the invention, comprises and adopts Graphene and polyamic acid, and its concrete steps are as follows:
Step 1: first 1 part of Graphene is distributed in 9 parts of dimethylacetamide solvents by milling, being uniformly dispersed, then adds again 1 part of polyamic acid in above-mentioned suspension, continue to disperse, finally obtain graphene suspension;
Step 2: by 4,4-diaminodiphenyl oxide and pyromellitic acid anhydride are dissolved in dimethylacetamide solvent simultaneously, wherein 4, it is 1:0.80 proportioning that 4-diaminodiphenyl oxide and pyromellitic acid anhydride be take the mole number of amine and the mole number of acid anhydride, then above-mentioned scattered graphene suspension is joined in polyamic acid, through circulation, disperse, continue 10 hours ~ 16 hours, again the mol ratio of amine in polyamic acid and acid anhydride is transferred to 1:0.98, viscosity reaches 60000 CP, and wherein Graphene ratio in the solid content of polyamic acid is 7%;
Step 3: by above-mentioned polymkeric substance deaeration casting film-forming, last imidization, rolling are cut.
The tensile strength 118Mpa of the Graphene polyimide composite film of the present embodiment gained, heat conductivility reaches 5.3w/m.k, elongation at break 18%.
Embodiment 2:
In the present embodiment, the preparation method's of Graphene polyimide composite film concrete steps are as follows:
Step 1: first 1 part of Graphene is distributed in 9 parts of dimethylacetamide solvents by milling, being uniformly dispersed, then adds again 1 part of polyamic acid in above-mentioned suspension, continue to disperse, finally obtain graphene suspension;
Step 2: by 4,4-diaminodiphenyl oxide and pyromellitic acid anhydride are dissolved in dimethylacetamide solvent simultaneously, wherein 4, it is 1:0.90 proportioning that 4-diaminodiphenyl oxide and pyromellitic acid anhydride be take the mole number of amine and the mole number of acid anhydride, then above-mentioned scattered graphene suspension is joined in polyamic acid, through circulation, disperse, continue 10 hours ~ 16 hours, again the mol ratio of amine in polyamic acid and acid anhydride is transferred to 1:0.99, viscosity reaches 90000 CP, and wherein Graphene ratio in the solid content of polyamic acid is 10%;
Step 3: by above-mentioned polymkeric substance deaeration casting film-forming, last imidization, rolling are cut.
The tensile strength 110Mpa of the Graphene polyimide composite film of the present embodiment gained, heat conductivility reaches 5.8w/m.k, elongation at break 15.1%.

Claims (1)

1. a preparation method for Graphene polyimide composite film, comprise adopt Graphene and by 4,4-diaminodiphenyl oxide and pyromellitic acid anhydride in solvent polycondensation and polyamic acid, it is characterized in that in accordance with the following steps:
Step 1: first by 1 part of Graphene by milling, disperseing, disperse particle diameter to reach below 100nm, be distributed to equably in 9 parts of dimethylacetamide solvents, then in above-mentioned suspension, add again 1 part of polyamic acid, continue to disperse, finally obtain graphene suspension;
Step 2: using as 4 of diamine, 4-diaminodiphenyl oxide and be simultaneously dissolved in dimethylacetamide solvent as the pyromellitic acid anhydride of binary acid anhydride, wherein 4, it is 1:0.80 ~ 1:0.90 proportioning that part of 4-diaminodiphenyl oxide and pyromellitic acid anhydride take the mole number of amine and the mole number of acid anhydride, then above-mentioned scattered graphene suspension is joined in the above-mentioned polyamic acid obtaining through polycondensation, through circulation, disperse, continue 10 hours ~ 16 hours, again the mol ratio of amine in polyamic acid and acid anhydride is transferred to 1:0.98 ~ 1:0.995, viscosity reaches 60000 CP ~ 90000 CP, wherein Graphene ratio in the solid content of polyamic acid is 1% ~ 15%,
Step 3: by above-mentioned polymkeric substance deaeration casting film-forming, last imidization, rolling are cut.
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104130576A (en) * 2014-07-03 2014-11-05 苏州世优佳电子科技有限公司 Graphene heat-conduction film
CN105061763A (en) * 2015-07-31 2015-11-18 苏州高通新材料科技有限公司 Sulfonated graphene-containing high heat conduction and high barrier polyimide film and production method thereof
CN106496615A (en) * 2016-11-08 2017-03-15 贵阳学院 A kind of preparation method of heat-pesistant thin film
CN106496611A (en) * 2016-09-26 2017-03-15 安徽国风塑业股份有限公司 A kind of preparation method of high heat conduction Kapton
CN106867256A (en) * 2017-02-27 2017-06-20 华烁科技股份有限公司 A kind of Graphene fabric-modifying anisotropic thermal Kapton, preparation method and application
CN107760028A (en) * 2017-11-16 2018-03-06 中国运载火箭技术研究院 A kind of light promotes graphene composite material film and its preparation method and application
CN109437905A (en) * 2018-11-27 2019-03-08 宁波今山新材料有限公司 A kind of preparation method of tear-resistant graphite film
CN110128654A (en) * 2019-06-11 2019-08-16 慧迈材料科技(广东)有限公司 A kind of Kapton of novel containing graphene
CN110191571A (en) * 2019-05-27 2019-08-30 维沃移动通信有限公司 Circuit board arrangement and terminal device
CN110396193A (en) * 2019-09-04 2019-11-01 江苏亚宝绝缘材料股份有限公司 A kind of preparation method and product of in-situ polymerization graphene hybrid modification polyamic acid resin
CN114854070A (en) * 2022-06-16 2022-08-05 启明新材料股份有限公司 Heat conduction BOPP film

Families Citing this family (1)

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CN107265451B (en) * 2017-07-17 2019-10-25 安徽国风塑业股份有限公司 A kind of preparation method of the polyimides graphite film of high conductive high strength

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104130576A (en) * 2014-07-03 2014-11-05 苏州世优佳电子科技有限公司 Graphene heat-conduction film
CN105061763A (en) * 2015-07-31 2015-11-18 苏州高通新材料科技有限公司 Sulfonated graphene-containing high heat conduction and high barrier polyimide film and production method thereof
CN106496611A (en) * 2016-09-26 2017-03-15 安徽国风塑业股份有限公司 A kind of preparation method of high heat conduction Kapton
CN106496615A (en) * 2016-11-08 2017-03-15 贵阳学院 A kind of preparation method of heat-pesistant thin film
CN106867256B (en) * 2017-02-27 2019-10-18 华烁科技股份有限公司 A kind of graphene fabric-modifying anisotropic thermal Kapton, preparation method and application
CN106867256A (en) * 2017-02-27 2017-06-20 华烁科技股份有限公司 A kind of Graphene fabric-modifying anisotropic thermal Kapton, preparation method and application
CN107760028A (en) * 2017-11-16 2018-03-06 中国运载火箭技术研究院 A kind of light promotes graphene composite material film and its preparation method and application
CN107760028B (en) * 2017-11-16 2020-06-09 中国运载火箭技术研究院 Light-propelled graphene composite material film and preparation method and application thereof
CN109437905A (en) * 2018-11-27 2019-03-08 宁波今山新材料有限公司 A kind of preparation method of tear-resistant graphite film
CN109437905B (en) * 2018-11-27 2021-08-17 宁波今山新材料有限公司 Preparation method of tear-resistant graphite film
CN110191571A (en) * 2019-05-27 2019-08-30 维沃移动通信有限公司 Circuit board arrangement and terminal device
CN110128654A (en) * 2019-06-11 2019-08-16 慧迈材料科技(广东)有限公司 A kind of Kapton of novel containing graphene
CN110396193A (en) * 2019-09-04 2019-11-01 江苏亚宝绝缘材料股份有限公司 A kind of preparation method and product of in-situ polymerization graphene hybrid modification polyamic acid resin
CN114854070A (en) * 2022-06-16 2022-08-05 启明新材料股份有限公司 Heat conduction BOPP film
CN114854070B (en) * 2022-06-16 2023-04-18 启明新材料股份有限公司 Heat conduction BOPP film

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