CN108530892A - A kind of graphene doping polybenzimidazoles-polyimide composite film and preparation method thereof - Google Patents
A kind of graphene doping polybenzimidazoles-polyimide composite film and preparation method thereof Download PDFInfo
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- C08L79/00—Compositions 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 C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
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- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
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- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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Abstract
The invention discloses a kind of graphenes to adulterate polybenzimidazoles polyimide composite film and preparation method thereof, include successively from top to bottom graphene composite film layer, graphene layer, graphene composite film layer, the graphene composite film layer and graphene layer are bonded by pressure-sensitive adhesive；The preparation method of the graphene composite film includes the preparation process of the preparation of epoxy group POSS, composite material；The composite material is 1 by the mass ratio of epoxy group POSS, graphene oxide, polybenzimidazoles, polyimides, catalyst by component：(2‑3)：(5‑7)：(5‑7)：1 is made；Graphene doping polybenzimidazoles polyimide composite film prepared by the present invention good, excellent in mechanical performance with thermal conductivity, it is good with other materials adhesiveness, it is easily worked the advantageous feature of molding.
Description
Technical field
The invention belongs to technical field of composite materials, are related to a kind of composite membrane more particularly to a kind of graphene doping polyphenyl
And imidazoles-polyimides composite heat conduction film.
Background technology
With the development of the social economy, electronic product and device have progressed into huge numbers of families, ceased with people’s lives
Correlation, these electronic products and device, will produce certain heat at work, and the temperature of device work is made to increase, and be formed
Hot localised points seriously affect service efficiency and the service life of device.Currently, Heat Conduction Material has widely in various industrial circles
Using, but due to the limitation of thermal conductivity, the effect is unsatisfactory for heat conduction soaking, limits the design of device or system.Especially
In microelectronic industry, integrated, the trend toward miniaturization of design of electronic circuits are more and more obvious, the equal hot material of high-performance heat conduction
It is required that also higher and higher, demand is also increasing.
It is that basic material is manufactured that the equal hot material of traditional heat conduction, which is mostly with metal or graphite, using aluminum bronze as representative
Metal class Heat Conduction Material weight is big and oxidizable, limits its application, cannot be satisfied need of the existing electronic product to heat conduction and heat radiation
It asks, graphite-like Heat Conduction Material is mainly by the charing of method and macromolecule, the graphitization etc. directly rolled after graphite treatment
Made of method, surface is that the heat sink material of graphite its tensile strength is not high, and frangible and granule dust is more and is inconvenient to install
With use, it is seen then that the equal hot material of conventional thermal conductive cannot meet electronic industry development for heat conduction soaking the needs of.
In order to improve the mechanical property of material, workability can in the prior art occur with the adhesion property of other materials
Using polyimides as polymer bond's material of representative, there is excellent mechanical property, electrical property, chemical stability, anti-spoke
Penetrating property, high temperature resistant and resistance to low temperature.But the thermal coefficient of Kapton is only 0.16W/ (MK), is limited in electricity
Application in sub- field of material technology.Graphene is as a kind of emerging material, with preferable thermal conductivity, but its it is frangible and
Granule dust is more and be inconvenient to install and use, be doped in polymer be difficult to again it is evenly dispersed, so as to cause membrane material
It can be unstable.
Therefore, seek more efficient way, prepare thermal conductivity and the more excellent heat conducting film gesture of mechanical property must
Row.
Invention content
The main purpose of the present invention is to provide a kind of graphenes to adulterate polybenzimidazoles-polyimide composite film, this is multiple
Film preparation raw material is closed to be easy to get, it is cheap；In addition, the composite membrane combine graphene and polyimides, polybenzimidazoles it is excellent
Point, with thermal conductivity, good, excellent in mechanical performance, good with other materials adhesiveness, is easily worked the advantageous feature of molding.
To achieve the above objectives, the technical solution adopted by the present invention is：A kind of graphene doping polybenzimidazoles-polyamides is sub-
Amine composite membrane, includes graphene composite film layer, graphene layer, graphene composite film layer successively from top to bottom, and the graphene is multiple
It closes film layer and graphene layer is bonded by pressure-sensitive adhesive.
The preparation method of the graphene composite film, includes the following steps：
1) preparation of epoxy group POSS：Isopropyl is added into the three-necked flask equipped with blender, dropping funel and thermometer
Alcohol, the tetramethylammonium hydroxide aqueous solution that mass fraction is 1-3%, are added dropwise dimethylbenzene in 2 hours with constant pressure funnel under stiring
With the mixed solution of KH560, after completion of dropwise addition, it is continuously stirred at room temperature 2 hours and hydrolyzes, then be condensed at 90-110 DEG C
Reaction 5-8 hour, after with saturated salt solution adjust solution PH to neutrality, be stirred at room temperature 2-3 hour, be evaporated under reduced pressure removing solvent,
It is used in combination acetone to wash 5-8 times, vacuum distillation removes acetone；
2) preparation of composite material：It will be through epoxy group POSS, graphene oxide, polyphenyl that step 1) is prepared and miaow
Azoles, polyimides, catalyst be added in double screw extruder melted, extrusion molding；The extrusion temperature of double screw extruder
Degree is：One 180-190 DEG C of area, two 190-200 DEG C of areas, three 200-210 DEG C of areas, four 210-220 DEG C of areas, five 220-230 DEG C of areas, machine
230-240 DEG C of head；Screw speed 250-300r/min.
Wherein, isopropanol described in step 1), tetramethylammonium hydroxide aqueous solution, dimethylbenzene, KH560 mass ratio be
(30-40):100：(30-40)：(150-200)；
The mass ratio of epoxy group POSS described in step 2), graphene oxide, polybenzimidazoles, polyimides, catalyst
It is 1：(2-3)：(5-7)：(5-7)：1；
One kind in sodium hydroxide, potassium hydroxide, triphenylphosphine, sodium hydride, tertiary butyl potassium alcoholate of the catalyst or
It is several；
Preferentially, the pressure-sensitive adhesive agent is that pressure-sensitive acrylate sticks agent.
Compared with prior art, the present invention having the following advantages and beneficial effect：
(1) graphene doping polybenzimidazoles-polyimide compound film structure that the present invention designs is simple, easily manufactured,
Raw material is easy to get, cheap；
(2) graphene doping polybenzimidazoles-polyimide composite film that the present invention designs, combines graphene, polyphenyl
And the excellent characteristics of imidazoles, polyimides, epoxy group POSS, good, excellent in mechanical performance the feature with thermal conductivity.
(3) graphene doping polybenzimidazoles-polyimide composite film that the present invention designs, passes through surface of graphene oxide
Epoxy group and epoxy group POSS crosslinked action so that two different kinds of polymer links together, and forms three-dimensional
Network structure so that polymer has excellent mechanical property and its chemical stability and ageing resistance.
(4) graphene doping polybenzimidazoles-polyimide composite film that the present invention designs, graphene and epoxy group POSS
Codope can also play heat transfer conductive force, cage type knot special POSS other than playing the role of enhancing mechanical property
Structure, when being mixed with graphene oxide, graphene oxide can be interspersed in cage structure, form passage of heat.
(5) graphene doping polybenzimidazoles-polyimide composite film that the present invention designs, is compounded to form by several tunics,
Centre is graphene layer, is conducive to support graphene in this way, improves its mechanical property, and outer layer is graphene composition polymer
Film is conducive to adhere to other substances, installation and use.
Description of the drawings
Fig. 1 be according to a preferred embodiment of the present invention a kind of graphene doping polybenzimidazoles-polyimides it is multiple
Close membrane structure diagram；
Drawing reference numeral explanation：1- graphene composite film layers；2- pressure-sensitive adhesives；3- graphene layers.
Specific implementation mode
It is described below for disclosing the present invention so that those skilled in the art can realize the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Embodiment 1
A kind of graphene doping polybenzimidazoles-polyimide composite film includes graphene composite film successively from top to bottom
Layer, graphene layer, graphene composite film layer, the graphene composite film layer and graphene layer are bonded by pressure-sensitive adhesive.
The preparation method of the graphene composite film, includes the following steps：
1) preparation of epoxy group POSS：Isopropyl is added into the three-necked flask equipped with blender, dropping funel and thermometer
Alcohol 30g, the tetramethylammonium hydroxide aqueous solution 100g that mass fraction is 1%, are added dropwise two in 2 hours with constant pressure funnel under stiring
The mixed solution of toluene 30g and KH560 150g after completion of dropwise addition, are continuously stirred at room temperature 2 hours and hydrolyze, then at 90 DEG C
Carry out condensation reaction 5 hours, after with saturated salt solution adjust solution PH to neutrality, be stirred at room temperature 2 hours, vacuum distillation removes molten
Agent is used in combination acetone to wash 5 times, and vacuum distillation removes acetone；
2) preparation of composite material：It will be through epoxy group POSS 50g that step 1) is prepared, graphene oxide 100g, poly-
Benzimidazole 250g, polyimides 250g, sodium hydroxide 50g be added in double screw extruder melted, extrusion molding；It is double
The extrusion temperature of screw extruder is：One 180 DEG C of area, two 190 DEG C of areas, three 200 DEG C of areas, four 210 DEG C of areas, five 220 DEG C of areas, head
230℃；Screw speed 250r/min.
The pressure-sensitive adhesive agent is that pressure-sensitive acrylate sticks agent.
Embodiment 2
A kind of graphene doping polybenzimidazoles-polyimide composite film includes graphene composite film successively from top to bottom
Layer, graphene layer, graphene composite film layer, the graphene composite film layer and graphene layer are bonded by pressure-sensitive adhesive.
The preparation method of the graphene composite film, includes the following steps：
1) preparation of epoxy group POSS：Isopropyl is added into the three-necked flask equipped with blender, dropping funel and thermometer
Alcohol 33g, the tetramethylammonium hydroxide aqueous solution 100g that mass fraction is 2%, are added dropwise two in 2 hours with constant pressure funnel under stiring
The mixed solution of toluene 34g and KH560 170g after completion of dropwise addition, are continuously stirred at room temperature 2 hours and hydrolyze, then at 95 DEG C
Carry out condensation reaction 6 hours, after with saturated salt solution adjust solution PH to neutrality, be stirred at room temperature 2.3 hours, vacuum distillation removes
Solvent is used in combination acetone to wash 6 times, and vacuum distillation removes acetone；
2) preparation of composite material：It will be through epoxy group POSS 50g that step 1) is prepared, graphene oxide 120g, poly-
Benzimidazole 280g, polyimides 300g, potassium hydroxide 50g be added in double screw extruder melted, extrusion molding；It is double
The extrusion temperature of screw extruder is：One 185 DEG C of area, two 195 DEG C of areas, three 205 DEG C of areas, four 215 DEG C of areas, five 225 DEG C of areas, head
235℃；Screw speed 260r/min.
The pressure-sensitive adhesive agent is that pressure-sensitive acrylate sticks agent.
Embodiment 3
A kind of graphene doping polybenzimidazoles-polyimide composite film includes graphene composite film successively from top to bottom
Layer, graphene layer, graphene composite film layer, the graphene composite film layer and graphene layer are bonded by pressure-sensitive adhesive.
The preparation method of the graphene composite film, includes the following steps：
1) preparation of epoxy group POSS：Isopropyl is added into the three-necked flask equipped with blender, dropping funel and thermometer
Alcohol 36g, the tetramethylammonium hydroxide aqueous solution 100g that mass fraction is 2.5%, are added dropwise in 2 hours with constant pressure funnel under stiring
The mixed solution of dimethylbenzene 35g and KH560 180g after completion of dropwise addition, are continuously stirred at room temperature 2 hours and hydrolyze, then 100
Condensation reaction 7 hours is carried out at DEG C, after with saturated salt solution adjust solution PH to neutrality, be stirred at room temperature 2.5 hours, be evaporated under reduced pressure
Solvent is removed, acetone is used in combination to wash 7 times, vacuum distillation removes acetone；
2) preparation of composite material：It will be through epoxy group POSS 50g that step 1) is prepared, graphene oxide 135g, poly-
Benzimidazole 320g, polyimides 330g, triphenylphosphine 50g be added in double screw extruder melted, extrusion molding；It is double
The extrusion temperature of screw extruder is：One 188 DEG C of area, two 197 DEG C of areas, three 207 DEG C of areas, four 218 DEG C of areas, five 225 DEG C of areas, head
235℃；Screw speed 270r/min.
The pressure-sensitive adhesive agent is that pressure-sensitive acrylate sticks agent.
Embodiment 4
A kind of graphene doping polybenzimidazoles-polyimide composite film includes graphene composite film successively from top to bottom
Layer, graphene layer, graphene composite film layer, the graphene composite film layer and graphene layer are bonded by pressure-sensitive adhesive.
The preparation method of the graphene composite film, includes the following steps：
1) preparation of epoxy group POSS：Isopropyl is added into the three-necked flask equipped with blender, dropping funel and thermometer
Alcohol 38g, the tetramethylammonium hydroxide aqueous solution 100g that mass fraction is 3%, are added dropwise two in 2 hours with constant pressure funnel under stiring
The mixed solution of toluene 40g and KH560 190g after completion of dropwise addition, are continuously stirred at room temperature 2 hours and hydrolyze, then at 105 DEG C
Lower progress condensation reaction 7.5 hours, after with saturated salt solution adjust solution PH to neutrality, be stirred at room temperature 2.8 hours, be evaporated under reduced pressure
Solvent is removed, acetone is used in combination to wash 8 times, vacuum distillation removes acetone；
2) preparation of composite material：It will be through epoxy group POSS50g that step 1) is prepared, graphene oxide 150g, poly-
Benzimidazole 330g, polyimides 350g, sodium hydride 50g be added in double screw extruder melted, extrusion molding；Double spiral shells
The extrusion temperature of bar extruder is：One 190 DEG C of area, two 195 DEG C of areas, three 210 DEG C of areas, four 218 DEG C of areas, five 228 DEG C of areas, head
240℃；Screw speed 290r/min.
The pressure-sensitive adhesive agent is that pressure-sensitive acrylate sticks agent.
Embodiment 5
A kind of graphene doping polybenzimidazoles-polyimide composite film includes graphene composite film successively from top to bottom
Layer, graphene layer, graphene composite film layer, the graphene composite film layer and graphene layer are bonded by pressure-sensitive adhesive.
The preparation method of the graphene composite film, includes the following steps：
1) preparation of epoxy group POSS：Isopropyl is added into the three-necked flask equipped with blender, dropping funel and thermometer
Alcohol 40g, the tetramethylammonium hydroxide aqueous solution 100g that mass fraction is 3%, are added dropwise two in 2 hours with constant pressure funnel under stiring
The mixed solution of toluene 40g and KH560 200g after completion of dropwise addition, are continuously stirred at room temperature 2 hours and hydrolyze, then at 110 DEG C
Lower progress condensation reaction 8 hours, after with saturated salt solution adjust solution PH to neutrality, be stirred at room temperature 3 hours, vacuum distillation remove
Solvent is used in combination acetone to wash 8 times, and vacuum distillation removes acetone；
2) preparation of composite material：It will be through epoxy group POSS 50g that step 1) is prepared, graphene oxide 150g, poly-
Benzimidazole 350g, polyimides 350g, tertiary butyl potassium alcoholate 50g be added in double screw extruder melted, extrusion molding；
The extrusion temperature of double screw extruder is：One 190 DEG C of area, two 200 DEG C of areas, three 210 DEG C of areas, four 220 DEG C of areas, five 230 DEG C of areas, machine
First 240 DEG C；Screw speed 300r/min.
The pressure-sensitive adhesive agent is that pressure-sensitive acrylate sticks agent.
Comparative example
Commercially available heat conduction film is purchased from Shanghai great Chu Electron Material Co., Ltd, model GS Kaptons.
Performance test：
(1) thermal coefficient：According to the measurement heat-pole method standard of GB/T10297-1998 non-metallic solid material heat-conducting coefficients
It is tested；
(2) tensile strength is tested：According to GB/T 1040-2006《Plastic tensile method for testing performance》It is tested；
(3) heat resistance (Martin) is tested：It is tested according to GB1035-1979；
(4) shore hardness：According to GB/T531-1992 standard testings；Test result is shown in Table 1.
1 embodiment of table and comparative example the performance test results
| Project | Thermal coefficient, W/m.k | Tensile strength, MPa | Heat resistance (Martin), DEG C | Shore hardness, A |
| Embodiment 1 | 73 | 103 | 220 | 86 |
| Embodiment 2 | 77 | 105 | 230 | 88 |
| Embodiment 3 | 85 | 110 | 243 | 94 |
| Embodiment 4 | 92 | 115 | 254 | 96 |
| Embodiment 5 | 103 | 120 | 265 | 99 |
| Comparative example | 16 | 26 | 180 | 63 |
As can be seen from the above table, graphene of the invention adulterates polybenzimidazoles-polyimide composite film thermal coefficient 73-
103W/m.k, tensile strength 103-120MPa, 220-265 DEG C of heat resistance (Martin), shore hardness 86-99A；And conventional commercial
Heat conduction film coefficient of heat transfer 16W/m.k, tensile strength 26MPa, 180 DEG C of heat resistance (Martin), shore hardness 63A, it is seen that this hair
Graphene doping polybenzimidazoles-polyimide composite film disclosed in bright embodiment has preferable thermal conductivity, tensile strength, resistance to
Hot and hardness.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection domain by appended claims and its
Equivalent defines.
Claims (6)
1. a kind of graphene adulterates polybenzimidazoles-polyimide composite film, which is characterized in that include graphite successively from top to bottom
Alkene composite film, graphene layer, graphene composite film layer, the graphene composite film layer and graphene layer pass through pressure-sensitive adhesive
It bonds.
2. a kind of graphene according to claim 1 adulterates polybenzimidazoles-polyimide composite film, which is characterized in that
The preparation method of the graphene composite film, includes the following steps：
1) preparation of epoxy group POSS：Isopropanol, matter are added into the three-necked flask equipped with blender, dropping funel and thermometer
Measure score be 1-3% tetramethylammonium hydroxide aqueous solution, under stiring in 2 hours with constant pressure funnel be added dropwise dimethylbenzene and
The mixed solution of KH560 after completion of dropwise addition, is continuously stirred at room temperature 2 hours and hydrolyzes, then at 90-110 DEG C be condensed instead
Answer 5-8 hours, after with saturated salt solution adjust solution PH to neutrality, be stirred at room temperature 2-3 hour, vacuum distillation removing solvent, and
It is washed 5-8 times with acetone, vacuum distillation removes acetone；
2) preparation of composite material：It will be through epoxy group POSS that step 1) is prepared, graphene oxide, polybenzimidazoles, poly-
Acid imide, catalyst be added in double screw extruder melted, extrusion molding；The extrusion temperature of double screw extruder is：
One 180-190 DEG C of area, two 190-200 DEG C of areas, three 200-210 DEG C of areas, four 210-220 DEG C of areas, five 220-230 DEG C of areas, head
230-240℃；Screw speed 250-300r/min.
3. a kind of graphene according to claim 2 adulterates polybenzimidazoles-polyimide composite film, which is characterized in that
Isopropanol described in step 1), tetramethylammonium hydroxide aqueous solution, dimethylbenzene, KH560 mass ratio be (30-40):100：
(30-40)：(150-200).
4. a kind of graphene according to claim 2 adulterates polybenzimidazoles-polyimide composite film, which is characterized in that
Epoxy group POSS described in step 2), graphene oxide, polybenzimidazoles, polyimides, catalyst mass ratio be 1：(2-
3)：(5-7)：(5-7)：1.
5. a kind of graphene according to claim 2 adulterates polybenzimidazoles-polyimide composite film, which is characterized in that
The catalyst is selected from one or more of sodium hydroxide, potassium hydroxide, triphenylphosphine, sodium hydride, tertiary butyl potassium alcoholate.
6. a kind of graphene according to claim 1 adulterates polybenzimidazoles-polyimide composite film, which is characterized in that
The pressure-sensitive adhesive agent is that pressure-sensitive acrylate sticks agent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111319319A (en) * | 2020-03-20 | 2020-06-23 | 中国地质大学（北京） | rGO-PEI/PVDF pyroelectric film and preparation method thereof |
| CN114232345A (en) * | 2021-12-20 | 2022-03-25 | 河南蓝翎环科防水材料有限公司 | Ultraviolet radiation resistant waterproof protective material and production process thereof |
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| US20160059444A1 (en) * | 2014-08-29 | 2016-03-03 | Yanbo Wang | Production of highly conductive graphitic films from polymer films |
| CN104464955A (en) * | 2014-11-28 | 2015-03-25 | 中国科学院金属研究所 | Method for manufacturing large-area high-performance graphene composite transparent conductive films on large scale |
| CN106113731A (en) * | 2016-06-23 | 2016-11-16 | 深圳市莱必德电子材料有限公司 | Graphene heat conduction and heat radiation film |
| CN107215023A (en) * | 2017-05-24 | 2017-09-29 | 深圳市莱必德电子材料有限公司 | Graphene heat conduction and heat radiation reflectance coating and preparation method thereof |
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| CN111319319A (en) * | 2020-03-20 | 2020-06-23 | 中国地质大学（北京） | rGO-PEI/PVDF pyroelectric film and preparation method thereof |
| CN111319319B (en) * | 2020-03-20 | 2021-03-02 | 中国地质大学（北京） | rGO-PEI/PVDF pyroelectric film and preparation method thereof |
| CN114232345A (en) * | 2021-12-20 | 2022-03-25 | 河南蓝翎环科防水材料有限公司 | Ultraviolet radiation resistant waterproof protective material and production process thereof |
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