CN108047471A - A kind of continuous preparation method of graphene film prepreg - Google Patents
A kind of continuous preparation method of graphene film prepreg Download PDFInfo
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- CN108047471A CN108047471A CN201810024685.1A CN201810024685A CN108047471A CN 108047471 A CN108047471 A CN 108047471A CN 201810024685 A CN201810024685 A CN 201810024685A CN 108047471 A CN108047471 A CN 108047471A
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- 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
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- 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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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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
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Abstract
The present invention relates to a kind of continuous preparation methods of graphene film prepreg, belong to technical field of function materials.Graphene film prepreg is using resin glued membrane and graphene film as raw material, it is prepared by hot melting process, resin glued membrane refers to scribbling the resin of 100 1400mm breadth and 10 100g/m2 surface densities in release paper, and resin used is epoxy resin, one kind in phenolic resin, unsaturated polyester (UP), polyurethane, bismaleimide resin, polyimide resin；Graphene film is the film with three-dimensional net structure or porous structure being prepared using graphene as primary raw material, determines that the raw material of graphene film forms using function according to graphene film prepreg.The present invention, which can be prepared continuously, determines that graphene film prepreg has the advantages that yield is high, can meet the wilderness demand of practical application well.One of the most key place of the present invention is can continuously preparing for graphene film.
Description
Technical field
The present invention relates to a kind of continuous preparation methods of graphene film prepreg, belong to technical field of function materials.
Background technology
As the fields such as the fast development of science and technology, aerospace put forward higher requirements used material, than
Such as, quality is lighter, performance is more excellent, manufacturing process is easier, and cost is lower.Since polymer matrix composites have weight
Gently, low bulk and many advantages, such as have excellent performance, gradually attracts attention.Since the end of last century, resin base
Composite material is just gradually instead of traditional metal material, to meet an urgent demand in the fields such as aerospace.It is but existing
The polymer matrix composites of the fillings such as carbon fiber, aramid fiber can not also meet actual requirement in some aspects, it is necessary to
The polymer matrix composites of development of new are modified original polymer matrix composites, to meet the necks such as aerospace
The active demand in domain further expands the application range of composite material.
In fields such as aerospaces, polymer matrix composites are mainly by prepreg or resin glued membrane paving, then pass through
The method for crossing autoclave molding is prepared.Therefore, the prepreg of development of new is one of main path to solve the above problems.
The graphene of two-dimension plane structure has many incomparable performances, such as excellent electric conductivity and heat conductivility, light weight
Density is low etc..Since 2010, after two scientists obtain Nobel Prize in physics because of graphene, people were to it each
Substantial amounts of research has been done in the application in field.Graphene already becomes one of now most popular material.It is prepared into corresponding
Prepreg, can have other prepregs (for example, carbon fiber prepreg) institute it is incomparable the advantages of.Resin base prepared therefrom
Composite material or the polymer matrix composites by its modification, can have the advantages that in some aspects prominent performance and, satisfaction
The active demand in the fields such as aerospace further expands the application range of composite material.
At present, there are some and the relevant patent of graphene prepreg, such as the patent report of Application No. CN201410459232
A kind of preparation method of graphene prepreg in road, it is that the method covered using vulcanizing press prepares graphene paper, then
Graphene paper and semi-solid preparation epoxy resin glued membrane is compound, obtain graphene prepreg.But its preparation method can not achieve stone
The continuous preparation of black alkene prepreg, resin glued membrane used are also limited to the epoxy resin glued membrane of semi-solid preparation.
The content of the invention
The present invention exactly for the above-mentioned prior art there are the problem of and design and provide a kind of graphene film prepreg
Continuous preparation method.
The purpose of the present invention is what is be achieved through the following technical solutions：
Graphene film prepreg is using resin glued membrane and graphene film as raw material, is prepared by hot melting process,
Resin glued membrane refers to scribbling the resin of 100-1400mm breadth and 10-100g/m2 surface densities, institute in release paper
It is one kind in epoxy resin, phenolic resin, unsaturated polyester (UP), polyurethane, bismaleimide resin, polyimide resin with resin；
Graphene film is that have three-dimensional net structure or porous structure using graphene as what primary raw material was prepared
Film, determine that the raw material of graphene film forms using function according to graphene film prepreg, raw material used is leads
The combination of one or more of electric raw material, non-conductive raw material, four parts of heat conduction raw material and auxiliary material：Conductive material includes
Redox graphene, graphene nanometer sheet, expanded graphite alkene or graphene powder；Non-conductive raw material includes epoxy resin, phenol
Urea formaldehyde, unsaturated polyester (UP), polyurethane, bismaleimide resin, polyimide resin or graphene oxide；Heat conduction raw material includes nitridation
Boron, aluminium oxide, aluminium nitride, magnesia, silica or zinc oxide；Auxiliary material include sodium hydroxide, hydroiodic acid, ammonium hydroxide, to benzene
Diamines or ethylenediamine, solvent used are one in deionized water, ethyl alcohol, acetone, dichloromethane, chloroform and tetrahydrofuran
Kind is several；
Preparation process is：
Step 1: the continuous preparation of graphene film：
With slurries：According to the use function of graphene film prepreg, composition of raw materials is formulated, weighs corresponding raw material and molten
Agent is uniformly mixed, and the graphene slurries that concentration is 5-200mg/ml are made；
Film：Uniformly mixed slurries are stored in storage tank, and storage tank is placed in the transmission carrier of conductive film machine
Top adjusts discharging switch, it is made to flow on transmission carrier, opens transmission switch, transfer rate 0.1-1m/min, using scraping
The graphene slurries transmitted on carrier are spread to the film that thickness is 0.3-3mm, breadth is 100-1400mm by knife and baffle, conductive
Film machine includes unwinding device, doctor blade device and heating unit, and unwinding device is placed in the front end of conductive film machine, and transmission carrier is placed in
On unwinding device, traction transmission carrier is by doctor blade device and heating unit, and subsequently into pre- dipping machine, transmission power is by presoaking
Machine provides；
Film forming：The heating zone of conductive film machine, warp are forwarded to by transmitting carrier by the graphene slurries film scraped
30 DEG C -120 DEG C of Temperature Treatment, obtains graphene film；
Step 2: the continuous preparation of graphene film prepreg：
Graphene film obtained is sent on the pressure roller platform front end of pre- dipping machine by transmitting carrier, passes through pre- dipping machine
Transmission device, the preliminary compound of graphene film and resin glued membrane is realized, by graphene film and the compound of resin glued membrane
The region with temperature system and pressing roll system of pre- dipping machine is sent to, at a temperature of 30 DEG C -200 DEG C, by 0.1-20kg
The roll process of pressure obtains graphene film prepreg.
The present invention has the advantage that and advantageous effect,
Graphene film prepreg of the present invention, has the advantages that the following aspects and excellent effect：Firstth, can connect
Continuous preparation determines that graphene film prepreg has the advantages that yield is high, can meet a large amount of need of practical application well
It asks.One of the most key place of the present invention is can continuously preparing for graphene film.It ensure that graphene film prepreg
Can be as traditional prepeg (for example, carbon fiber prepreg etc.), it can be on pre- dipping machine by heating compound method, even
Continuous preparation is produced.The continuous graphene film prepreg length that is prepared from equipment limit, can be 10m, 50m even
It is longer, by cooling down, cutting and wind to get to final delivered product.The characteristics of can continuously preparing so that graphene film
The yield of prepreg is high, can meet wilderness demand for various purposes well.Secondth, adjustable electric conductivity and thermal conductivity
It can so that graphene film prepreg has the characteristics that widely used.Graphene film used in graphene film prepreg is
One pack system is multi-component compound, and effect of each component played in graphene film is also different.By adjusting graphene
Raw material type, material rate and the solvent dosage of film realize graphene film and its prepreg electric conductivity and heat conductivility
Controllability so that the performance of the graphene film prepreg of preparation meets actual application requirement, widely used.3rd,
Various selection of resin glued membrane adds many beneficial effects to graphene film prepreg：For example, it disclosure satisfy that difference makes
With the requirement of environment, can realize and other prepreg co-curings.Same purposes can there are a variety of use environments to require, than
Such as temperature requirement.Various selection of resin glued membrane can greatly reduce application of the use environment requirement to graphene film prepreg
Limitation.If the it is required that long-time service at 200 DEG C, it is possible to bismaleimide resin glued membrane and graphene film be selected to heat compound, system
Standby graphene film prepreg；If it is required that long-time service at room temperature, it is possible to select epoxy resin glued membrane and graphene thin
Film hot melt is compound, prepares graphene film prepreg.In addition, when graphene film prepreg is used in conjunction with other prepregs
When, the resin identical with other prepregs can be selected as glued membrane to prepare graphene film prepreg.The graphene of preparation
Film prepreg can prepare composite material with other prepregs by autoclave co-curing.This causes the technique letter of composite material
Single, more efficient, manufacture cost is substantially reduced.
Description of the drawings
Fig. 1 is the graphene film prepreg prepared；
Fig. 2 is the composite material that graphene film prepreg is prepared with carbon fiber prepreg by autoclave molding；
Fig. 3 is the structure diagram of conductive film machine of the present invention.
Specific embodiment
Graphene film prepreg of the present invention is using resin glued membrane and graphene film as raw material, is prepared by hot melting process
It forms,
Resin glued membrane refers to scribbling the resin of 100-1400mm breadth and 10-100g/m2 surface densities, institute in release paper
It is one kind in epoxy resin, phenolic resin, unsaturated polyester (UP), polyurethane, bismaleimide resin, polyimide resin with resin.Root
It selects to close according to the particular condition in use (for example, use environment requirement, component of other prepregs) of graphene film prepreg
Suitable resin glued membrane.
Graphene film is that have three-dimensional net structure or porous structure using graphene as what primary raw material was prepared
Film, determine that the raw material of graphene film forms using function according to graphene film prepreg, raw material used is leads
The combination of one or more of electric raw material, non-conductive raw material, four parts of heat conduction raw material and auxiliary material：Conductive material includes
Redox graphene, graphene nanometer sheet, expanded graphite alkene or graphene powder；Non-conductive raw material includes epoxy resin, phenol
Urea formaldehyde, unsaturated polyester (UP), polyurethane, bismaleimide resin, polyimide resin or graphene oxide；Heat conduction raw material includes nitridation
Boron, aluminium oxide, aluminium nitride, magnesia, silica or zinc oxide；Auxiliary material include sodium hydroxide, hydroiodic acid, ammonium hydroxide, to benzene
Diamines or ethylenediamine.Solvent used is one in deionized water, ethyl alcohol, acetone, dichloromethane, chloroform and tetrahydrofuran
Kind is several.According to specific requirement and purposes, the dosage of the species of raw material, the ratio of raw material and solvent is adjusted.It is for example, logical
The species and ratio of conductive material, non-conductive raw material and heat conduction raw material are overregulated, realizes that graphene film and its prepreg are conductive
The controllability of performance and heat conductivility so that the performance of the graphene film prepreg of preparation meets actual application requirement.
Preparation process is：
Step 1: the continuous preparation of graphene film：
With slurries：According to the use function of graphene film prepreg, composition of raw materials is formulated, weighs corresponding raw material and molten
Agent is uniformly mixed, and the graphene slurries that concentration is 5-200mg/ml are made；
Film：Uniformly mixed slurries are stored in storage tank, and storage tank is placed in the transmission carrier of conductive film machine
Top adjusts discharging switch, it is made to flow on transmission carrier, opens transmission switch, transfer rate 0.1-1m/min, using scraping
The graphene slurries transmitted on carrier are spread to the film that thickness is 0.3-3mm, breadth is 100-1400mm by knife and baffle.It is conductive
Film machine includes unwinding device 1, doctor blade device 2 and heating unit 3.Wherein, the unwinding device 1 of conductive film machine and heating unit 3 have
Body is formed such as pre- dipping machine；The doctor blade device 2 of conductive film machine is similar to pre- dipping machine, the difference is that, scraper is not
Centainly perpendicular to platform, but angle is adjustable from 0o-90o.Unwinding device 1 is put transmission carrier in the front end of conductive film machine
In on unwinding device 1, traction transmission carrier, subsequently into pre- dipping machine, transmits power by doctor blade device 2 and heating unit 3
It is provided by pre- dipping machine.
Film forming：The graphene slurries film scraped is forwarded to heating zone by transmitting carrier, through 30 DEG C -120 DEG C
Temperature Treatment, obtain graphene film；
Step 2: the continuous preparation of graphene film prepreg：
Graphene film obtained is sent on the pressure roller platform front end of pre- dipping machine by transmitting carrier, passes through pre- dipping machine
Transmission device, realize the preliminary compound of graphene film and resin glued membrane.Compound is sent to temperature system and pressure
At a temperature of 30 DEG C -200 DEG C, by the roll process of 0.1-20kg pressure, it is pre- to obtain graphene film for the region of roller system
Leaching material.Graphene film prepreg is cooled down, cut and wound to get to final delivered product.Graphene film is pre-
Leaching material can be that single-layer resin glued membrane is compound or double-layer resin glued membrane is compound.
It is described in further detail below in conjunction with embodiment：
Embodiment one (conduction)：
Step 1: the continuous preparation of graphene film：
With slurries：Weigh 22.5g graphene nanometer sheets, 2.5g epoxy resin and 500ml ethyl alcohol, by ultrasonic 20min and
It after stirring 20min, is uniformly mixed, the graphene slurries that concentration is 50mg/ml is made；
Film：Uniformly mixed graphene slurries are stored in storage tank, and by storage tank be placed in conductive film machine from
Above type paper, discharging switch is adjusted, uniformly mixed graphene slurries is made to flow in release paper.Open transmission switch, transmission speed
It spends for 0.1m/min, the graphene slurries in release paper spreads to thickness is 1mm, breadth is 300mm's using scraper and baffle
Film.Scraper tilts, and the angle with platform is 30o；
Film forming：The graphene slurries film scraped is forwarded to by heating zone by release paper, at 60 DEG C of temperature
Reason, obtains graphene film；
Step 2: the continuous preparation of graphene film prepreg：
Graphene film obtained is sent on the pressure roller platform front end of pre- dipping machine by release paper, passes through pre- dipping machine
Transmission device makes graphene film and intermediate temperature setting epoxy resin glued membrane tentatively compound, and formation intermediate temperature setting epoxy resin glued membrane-
The structure of graphene film.The compound of graphene film and intermediate temperature setting epoxy resin glued membrane is sent to temperature system
With the region of pressing roll system, at a temperature of 80 DEG C, (pressure roller quantity is 2 to the roll process by 0.1kg-5kg pressure, pressure
Power is respectively 0.1kg and 5kg), obtain the compound graphene film prepreg of single-layer resin glued membrane.By graphene film prepreg
Processing is cooled down, cut and wound to get to final delivered product.Graphene film prepreg prepared by (Fig. 1) can be with
With carbon fiber prepreg together, by paving and the method for autoclave molding, it is prepared into composite material.(Fig. 2) after tested, the stone
The electrical conductivity of black alkene film prepreg is about 5000S/m.Corresponding composite material, the conductance in graphene film prepreg one side
Rate is 100S/m.
Embodiment two (heat conduction)：
Step 1: the continuous preparation of graphene film：
With slurries：Weigh 18g graphene nanometer sheets, 4.5g four acicular type zinc oxide crystal whiskers, 2g graphene oxides, 0.5g hydrogen-oxygens
Change sodium and 500ml deionized waters, after ultrasonic 20min and stirring 20min, be uniformly mixed, the stone that concentration is 50mg/ml is made
Black alkene slurries；
Film：Uniformly mixed graphene slurries are stored in storage tank, and by storage tank be placed in conductive film machine from
Above type paper, discharging switch is adjusted, uniformly mixed graphene slurries is made to flow in release paper.Open transmission switch, transmission speed
It spends for 0.1m/min, the graphene slurries in release paper spreads to thickness is 1mm, breadth is 300mm's using scraper and baffle
Film.Scraper tilts, and the angle with platform is 30o；
Film forming：The graphene slurries film scraped is forwarded to by heating zone by release paper, at 120 DEG C of temperature
Reason, obtains graphene film；
Step 2: the continuous preparation of graphene film prepreg：
Graphene film obtained is sent on the pressure roller platform front end of pre- dipping machine by release paper, passes through pre- dipping machine
Transmission device makes graphene film and intermediate temperature setting epoxy resin glued membrane tentatively compound, and formation intermediate temperature setting epoxy resin glued membrane-
The structure of graphene film.The compound of graphene film and intermediate temperature setting epoxy resin glued membrane is sent to temperature system
With the region of pressing roll system, at a temperature of 80 DEG C, (pressure roller quantity is 3 to the roll process by 1kg-8kg pressure, pressure
Respectively 1kg, 4kg and 8kg), obtain the compound graphene film prepreg of single-layer resin glued membrane.By graphene film prepreg
Processing is cooled down, cut and wound to get to final delivered product.After tested, the conductance of the graphene film prepreg
Rate is about 1000S/m, and horizontal thermal conductivity is 20W/mk, and vertical thermal conductivity is 8W/mk.
Claims (1)
1. a kind of continuous preparation method of graphene film prepreg, it is characterised in that：Graphene film prepreg is with resin
Glued membrane and graphene film are raw material, are prepared by hot melting process, resin glued membrane refers to scribbling 100- in release paper
1400mm breadth and 10-100g/m2The resin of surface density, resin used is epoxy resin, phenolic resin, unsaturated polyester (UP), poly-
One kind in urethane, bismaleimide resin, polyimide resin；Graphene film is the tool being prepared using graphene as primary raw material
There is the film of three-dimensional net structure or porous structure, graphene film is determined according to the use function of graphene film prepreg
Raw material composition, raw material used is conductive material, non-conductive raw material, one kind in four parts of heat conduction raw material and auxiliary material
Or several combination：Conductive material includes redox graphene, graphene nanometer sheet, expanded graphite alkene or graphene powder；
Non-conductive raw material includes epoxy resin, phenolic resin, unsaturated polyester (UP), polyurethane, bismaleimide resin, polyimide resin or oxidation
Graphene；Heat conduction raw material includes boron nitride, aluminium oxide, aluminium nitride, magnesia, silica or zinc oxide；Auxiliary material includes hydrogen
Sodium oxide molybdena, hydroiodic acid, ammonium hydroxide, p-phenylenediamine or ethylenediamine, solvent used for deionized water, ethyl alcohol, acetone, dichloromethane,
One or several kinds in chloroform and tetrahydrofuran；Preparation process is：
Step 1: the continuous preparation of graphene film：
With slurries：According to the use function of graphene film prepreg, composition of raw materials is formulated, weighs corresponding raw material and solvent,
It is uniformly mixed, the graphene slurries that concentration is 5-200mg/ml is made；
(1) film：Uniformly mixed slurries are stored in storage tank, and storage tank is placed on the transmission carrier of conductive film machine
Side adjusts discharging switch, it is made to flow on transmission carrier, opens transmission switch, and transfer rate 0.1-1m/min utilizes scraper
The graphene slurries transmitted on carrier are spread into the film that thickness is 0.3-3mm, breadth is 100-1400mm, conductive film with baffle
Machine includes unwinding device, doctor blade device and heating unit, and unwinding device is placed in the front end of conductive film machine, and transmission carrier, which is placed in, to be put
On winding apparatus, traction transmission carrier is by doctor blade device and heating unit, and subsequently into pre- dipping machine, transmission power is by pre- dipping machine
It provides；
(2) form a film：The heating zone of conductive film machine is forwarded to by transmitting carrier by the graphene slurries film scraped, through 30
DEG C -120 DEG C of Temperature Treatment, obtains graphene film；
Step 2: the continuous preparation of graphene film prepreg：
Graphene film obtained is sent on the pressure roller platform front end of pre- dipping machine by transmitting carrier, passes through the biography of pre- dipping machine
Device is sent, realization graphene film is preliminary compound with resin glued membrane, and the compound of graphene film and resin glued membrane is transmitted
To the region with temperature system and pressing roll system of pre- dipping machine, at a temperature of 30 DEG C -200 DEG C, by 0.1-20kg pressure
Roll process, obtain graphene film prepreg.
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Cited By (3)
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| CN108790372A (en) * | 2018-06-12 | 2018-11-13 | 合肥科塑信息科技有限公司 | A kind of producing equipment of graphene prepreg |
| CN109651636A (en) * | 2018-12-24 | 2019-04-19 | 王新民 | A kind of preparation method of prepreg |
| CN113402750A (en) * | 2021-06-04 | 2021-09-17 | 中国航发北京航空材料研究院 | Preparation method of graphene prepreg with three-dimensional network structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108790372A (en) * | 2018-06-12 | 2018-11-13 | 合肥科塑信息科技有限公司 | A kind of producing equipment of graphene prepreg |
| CN108790372B (en) * | 2018-06-12 | 2020-09-18 | 绍兴纤逸纺织科技有限公司 | Preparation equipment of graphite alkene preimpregnation material |
| CN109651636A (en) * | 2018-12-24 | 2019-04-19 | 王新民 | A kind of preparation method of prepreg |
| CN113402750A (en) * | 2021-06-04 | 2021-09-17 | 中国航发北京航空材料研究院 | Preparation method of graphene prepreg with three-dimensional network structure |
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| CN108047471B (en) | 2020-12-29 |
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