CN108047471B - Continuous preparation method of graphene film prepreg - Google Patents
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- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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Abstract
The invention relates to a continuous preparation method of a graphene film prepreg, and belongs to the technical field of functional materials. The graphene film prepreg is prepared by taking a resin adhesive film and a graphene film as raw materials through a hot melting process, wherein the resin adhesive film is formed by coating resin with the width of 100-1400mm and the surface density of 10-100g/m2 on release paper, and the resin is one of epoxy resin, phenolic resin, unsaturated polyester, polyurethane, bismaleimide resin and polyimide resin; the graphene film is a film with a three-dimensional network structure or a porous structure and prepared by taking graphene as a main raw material, and the raw material composition of the graphene film is determined according to the use function of the graphene film prepreg. The method can be used for continuously preparing the graphene film prepreg, so that the graphene film prepreg has the advantage of high yield, and can well meet a large number of requirements of practical application. One of the most critical aspects of the present invention is the continuous preparation of graphene films.
Description
Technical Field
The invention relates to a continuous preparation method of a graphene film prepreg, and belongs to the technical field of functional materials.
Background
With the rapid development of science and technology, the fields of aerospace and the like put forward higher requirements on used materials, such as lighter weight, more excellent performance, simpler and more convenient manufacturing process and lower cost. Resin-based composite materials have attracted attention because of their advantages of light weight, low expansion, and excellent properties. Since the end of the last century, resin-based composite materials gradually replace traditional metal materials to meet the urgent requirements of the fields of aerospace and the like. However, the existing resin-based composite materials filled with carbon fibers, aramid fibers and the like cannot meet actual use requirements in some aspects, and a novel resin-based composite material needs to be developed or an original resin-based composite material needs to be modified so as to meet urgent needs in the fields of aerospace and the like, and the application range of the composite material is further expanded.
In the fields of aerospace and the like, resin-based composite materials are mainly prepared by paving and pasting prepreg or resin adhesive films and then forming by an autoclave. Therefore, the development of a novel prepreg is one of the main approaches to solve the above problems. Graphene with a two-dimensional plane structure has many incomparable performances, such as excellent electrical conductivity and thermal conductivity, low weight and density, and the like. Since 2010, two scientists have won the reward of nobel physics for graphene, and have made a great deal of research on its application in various fields. Graphene has become one of the hottest materials today. The preparation of the prepreg into a corresponding prepreg can have advantages which are not compared with other prepregs (such as carbon fiber prepregs). The resin-based composite material prepared by the method or the resin-based composite material modified by the resin-based composite material has outstanding performance and advantages in certain aspects, meets the urgent needs of the fields of aerospace and the like, and further expands the application range of the composite material.
At present, there are some patents related to graphene prepregs, for example, patent with application number CN201410459232 reports a preparation method of a graphene prepreg, which is to prepare graphene paper by a press-coating method of a flat vulcanizing machine, and then compound the graphene paper with a semi-cured epoxy resin adhesive film to obtain the graphene prepreg. However, the preparation method cannot realize continuous preparation of the graphene prepreg, and the resin adhesive film used is limited to the semi-cured epoxy resin adhesive film.
Disclosure of Invention
The invention provides a continuous preparation method of a graphene film prepreg aiming at the problems in the prior art.
The purpose of the invention is realized by the following technical scheme:
the graphene film prepreg is prepared by taking a resin adhesive film and a graphene film as raw materials through a hot melting process,
the resin adhesive film refers to that resin with the width of 100-1400mm and the surface density of 10-100g/m2 is coated on release paper, and the used resin is one of epoxy resin, phenolic resin, unsaturated polyester, polyurethane, bismaleimide resin and polyimide resin;
the graphene film is a film with a three-dimensional network structure or a porous structure, which is prepared by taking graphene as a main raw material, the raw material composition of the graphene film is determined according to the use function of the graphene film prepreg, and the used raw material is one or a combination of more of a conductive raw material, a non-conductive raw material, a heat-conducting raw material and an auxiliary raw material: the conductive raw material comprises reduced graphene oxide, graphene nanosheets, expanded graphene or graphene powder; the non-conductive raw materials comprise epoxy resin, phenolic resin, unsaturated polyester, polyurethane, bismaleimide resin, polyimide resin or graphene oxide; the heat-conducting raw material comprises boron nitride, aluminum oxide, aluminum nitride, magnesium oxide, silicon oxide or zinc oxide; the auxiliary raw materials comprise sodium hydroxide, hydroiodic acid, ammonia water, p-phenylenediamine or ethylenediamine, and the used solvent is one or more of deionized water, ethanol, acetone, dichloromethane, trichloromethane and tetrahydrofuran;
the preparation steps are as follows:
step one, continuously preparing a graphene film:
preparing slurry: formulating a raw material formula according to the use function of the graphene film prepreg, weighing corresponding raw materials and a solvent, and uniformly mixing to prepare graphene slurry with the concentration of 5-200 mg/ml;
coating: storing the uniformly mixed slurry in a storage tank, placing the storage tank above a conveying carrier of a conductive film machine, adjusting a discharging switch to enable the slurry to flow onto the conveying carrier, starting the conveying switch, wherein the conveying speed is 0.1-1m/min, scraping the graphene slurry on the conveying carrier into a film with the thickness of 0.3-3mm and the width of 100 plus 1400mm by using a scraper and a baffle plate, wherein the conductive film machine comprises an unreeling device, a scraper device and a heating device, the unreeling device is arranged at the foremost end of the conductive film machine, the conveying carrier is arranged on the unreeling device, the conveying carrier is pulled to pass through the scraper device and the heating device, and then the conveying carrier enters a pre-dipping machine, and conveying power is provided by a pre-dipping machine;
film forming: the scraped graphene slurry film is conveyed forwards to a heating area of a conductive film machine through a conveying carrier, and is treated at the temperature of 30-120 ℃ to obtain a graphene film;
step two, continuously preparing a graphene film prepreg:
conveying the prepared graphene film to the front end of a compression roller platform of a pre-dipping machine through a conveying carrier, realizing primary compounding of the graphene film and a resin adhesive film through a conveying device of the pre-dipping machine, conveying the compound of the graphene film and the resin adhesive film to an area, provided with a temperature system and a compression roller system, of the pre-dipping machine, and performing compression roller treatment under the pressure of 0.1-20kg at the temperature of 30-200 ℃ to obtain the graphene film prepreg.
The invention has the advantages and beneficial effects that,
the graphene film prepreg provided by the invention has the following advantages and excellent effects: firstly, continuous preparation determines that the graphene film prepreg has the advantage of high yield, and can well meet a large amount of requirements of practical application. One of the most critical aspects of the present invention is the continuous preparation of graphene films. The method ensures that the graphene film prepreg can be continuously prepared and produced on a prepreg machine by a hot-melt compounding method like the traditional prepreg (such as carbon fiber prepreg and the like). The length of the graphene film prepreg obtained by continuous preparation is not limited by equipment, can be 10m, 50m or even longer, and the final delivery product can be obtained by cooling, cutting and rolling. The graphene film prepreg has the characteristic of continuous preparation, so that the yield of the graphene film prepreg is high, and the requirements of various purposes can be well met. Secondly, the adjustable electric conductivity and heat conductivity enable the graphene film prepreg to have the characteristic of wide application. The graphene film used by the graphene film prepreg is single-component or multi-component composite, and the components have different functions in the graphene film. The adjustability of the conductivity and the thermal conductivity of the graphene film and the prepreg of the graphene film is realized by adjusting the raw material type, the raw material proportion and the solvent amount of the graphene film, so that the performance of the prepared graphene film prepreg meets the actual application requirement, and the application is wide. Thirdly, various choices of resin adhesive films add a plurality of beneficial effects to the graphene film prepreg: for example, the prepreg can meet the requirements of different use environments and can be co-cured with other prepregs. There may be multiple use environment requirements, such as temperature requirements, for the same application. Due to the various choices of the resin adhesive films, the application limit of the use environment requirement on the graphene film prepreg can be greatly reduced. If the graphene film prepreg is required to be used for a long time at the temperature of 200 ℃, the bismaleimide resin adhesive film and the graphene film can be selected for hot-melt compounding to prepare the graphene film prepreg; if the graphene film prepreg is required to be used at room temperature for a long time, the epoxy resin adhesive film and the graphene film can be selected for hot-melt compounding to prepare the graphene film prepreg. In addition, when the graphene thin film prepreg is used together with other prepregs, the same resin as the other prepregs may be selected as the adhesive film to prepare the graphene thin film prepreg. The prepared graphene film prepreg and other prepregs can be co-cured by an autoclave to prepare a composite material. This makes the composite material simple in process, high in efficiency and low in manufacturing cost.
Drawings
FIG. 1 is a prepared graphene thin film prepreg;
FIG. 2 is a composite material prepared by molding a graphene film prepreg and a carbon fiber prepreg through an autoclave;
fig. 3 is a schematic structural diagram of the conductive film machine of the present invention.
Detailed Description
The graphene film prepreg is prepared by taking a resin adhesive film and a graphene film as raw materials through a hot melting process,
the resin adhesive film refers to that the release paper is coated with resin with the width of 100-1400mm and the surface density of 10-100g/m2, and the used resin is one of epoxy resin, phenolic resin, unsaturated polyester, polyurethane, bismaleimide resin and polyimide resin. The appropriate resin adhesive film is selected according to the specific use condition of the graphene film prepreg (such as use environment requirements and other prepreg components).
The graphene film is a film with a three-dimensional network structure or a porous structure, which is prepared by taking graphene as a main raw material, the raw material composition of the graphene film is determined according to the use function of the graphene film prepreg, and the used raw material is one or a combination of more of a conductive raw material, a non-conductive raw material, a heat-conducting raw material and an auxiliary raw material: the conductive raw material comprises reduced graphene oxide, graphene nanosheets, expanded graphene or graphene powder; the non-conductive raw materials comprise epoxy resin, phenolic resin, unsaturated polyester, polyurethane, bismaleimide resin, polyimide resin or graphene oxide; the heat-conducting raw material comprises boron nitride, aluminum oxide, aluminum nitride, magnesium oxide, silicon oxide or zinc oxide; the auxiliary raw materials comprise sodium hydroxide, hydroiodic acid, ammonia water, p-phenylenediamine or ethylenediamine. The solvent is one or more of deionized water, ethanol, acetone, dichloromethane, chloroform and tetrahydrofuran. The types of the raw materials, the proportion of the raw materials and the dosage of the solvent are adjusted according to specific requirements and purposes. For example, the adjustability of the electrical conductivity and the thermal conductivity of the graphene film and the prepreg thereof is realized by adjusting the types and the proportions of the conductive raw material, the non-conductive raw material and the thermal conductive raw material, so that the performance of the prepared graphene film prepreg meets the actual application requirements.
The preparation steps are as follows:
step one, continuously preparing a graphene film:
preparing slurry: formulating a raw material formula according to the use function of the graphene film prepreg, weighing corresponding raw materials and a solvent, and uniformly mixing to prepare graphene slurry with the concentration of 5-200 mg/ml;
coating: and storing the uniformly mixed slurry in a storage tank, placing the storage tank above a conveying carrier of a conductive film machine, adjusting a discharging switch to enable the slurry to flow onto the conveying carrier, starting the conveying switch, wherein the conveying speed is 0.1-1m/min, and scraping the graphene slurry on the conveying carrier into a film with the thickness of 0.3-3mm and the width of 100-1400mm by using a scraper and a baffle plate. Electrically conductive membrane machine includes unwinding device 1, scraper device 2 and heating device 3. The unwinding device 1 and the heating device 3 of the conductive film machine are the same as those of a pre-dipping machine in specific composition; the scraper device 2 of the conductive film machine is similar to that of the pre-dipping machine, except that the scraper is not necessarily perpendicular to the platform, but the angle is adjustable from 0 to 90 degrees. The unwinding device 1 is arranged on the unwinding device 1 at the foremost end of the conductive film machine, the conveying carrier is pulled to pass through the scraper device 2 and the heating device 3 and then enters the pre-dipping machine, and conveying power is provided by the pre-dipping machine.
Film forming: the scraped graphene slurry film is conveyed forwards to a heating area through a conveying carrier and is treated at the temperature of 30-120 ℃ to obtain a graphene film;
step two, continuously preparing a graphene film prepreg:
the prepared graphene film is conveyed to the front end of a compression roller platform of the pre-dipping machine through a conveying carrier, and preliminary compounding of the graphene film and a resin adhesive film is realized through a conveying device of the pre-dipping machine. And conveying the composite to a region with a temperature system and a compression roller system, and performing compression roller treatment under the pressure of 0.1-20kg at the temperature of 30-200 ℃ to obtain the graphene film prepreg. And cooling, cutting and rolling the graphene film prepreg to obtain the final delivery product. The graphene film prepreg can be formed by compounding a single-layer resin adhesive film or compounding a double-layer resin adhesive film.
The following is described in further detail with reference to the following examples:
example one (conductive):
step one, continuously preparing a graphene film:
preparing slurry: weighing 22.5g of graphene nanosheet, 2.5g of epoxy resin and 500ml of ethanol, performing ultrasonic treatment for 20min, stirring for 20min, and uniformly mixing to prepare graphene slurry with the concentration of 50 mg/ml;
coating: the graphene slurry mixed uniformly is stored in the storage tank, the storage tank is arranged above the release paper of the conductive film machine, and the discharge switch is adjusted to enable the graphene slurry mixed uniformly to flow onto the release paper. And starting a transmission switch, wherein the transmission speed is 0.1m/min, and scraping the graphene slurry on the release paper into a film with the thickness of 1mm and the width of 300mm by using a scraper and a baffle. The scraper is inclined, and the angle between the scraper and the platform is 30 degrees;
film forming: the scraped graphene slurry film is conveyed forwards to a heating area through release paper, and is treated at the temperature of 60 ℃ to obtain a graphene film;
step two, continuously preparing a graphene film prepreg:
the prepared graphene film is conveyed to the front end of a compression roller platform of a pre-dipping machine through release paper, and the graphene film and the medium-temperature curing epoxy resin adhesive film are preliminarily compounded through a conveying device of the pre-dipping machine to form a medium-temperature curing epoxy resin adhesive film-graphene film structure. Conveying the composite of the graphene film and the medium-temperature cured epoxy resin adhesive film to an area with a temperature system and a compression roller system, and performing compression roller treatment under the pressure of 0.1kg-5kg at the temperature of 80 ℃ (the number of the compression rollers is 2, and the pressure is 0.1kg and 5kg respectively) to obtain the single-layer resin adhesive film composite graphene film prepreg. And cooling, cutting and rolling the graphene film prepreg to obtain the final delivery product. The graphene film prepreg prepared in the figure 1 can be prepared into a composite material together with a carbon fiber prepreg by paving and autoclave molding. (FIG. 2) the conductivity of the graphene thin film prepreg was tested to be about 5000S/m. The electrical conductivity of the corresponding composite material on one side of the graphene film prepreg is 100S/m.
Example two (thermal conductivity):
step one, continuously preparing a graphene film:
preparing slurry: weighing 18g of graphene nanosheet, 4.5g of tetrapod-like zinc oxide whisker, 2g of graphene oxide, 0.5g of sodium hydroxide and 500ml of deionized water, carrying out ultrasonic treatment for 20min and stirring for 20min, and then uniformly mixing to prepare graphene slurry with the concentration of 50 mg/ml;
coating: the graphene slurry mixed uniformly is stored in the storage tank, the storage tank is arranged above the release paper of the conductive film machine, and the discharge switch is adjusted to enable the graphene slurry mixed uniformly to flow onto the release paper. And starting a transmission switch, wherein the transmission speed is 0.1m/min, and scraping the graphene slurry on the release paper into a film with the thickness of 1mm and the width of 300mm by using a scraper and a baffle. The scraper is inclined, and the angle between the scraper and the platform is 30 degrees;
film forming: the scraped graphene slurry film is conveyed forwards to a heating area through release paper, and is treated at the temperature of 120 ℃ to obtain a graphene film;
step two, continuously preparing a graphene film prepreg:
the prepared graphene film is conveyed to the front end of a compression roller platform of a pre-dipping machine through release paper, and the graphene film and the medium-temperature curing epoxy resin adhesive film are preliminarily compounded through a conveying device of the pre-dipping machine to form a medium-temperature curing epoxy resin adhesive film-graphene film structure. Conveying the composite of the graphene film and the medium-temperature cured epoxy resin adhesive film to an area with a temperature system and a compression roller system, and performing compression roller treatment under the pressure of 1kg-8kg at the temperature of 80 ℃ (the number of the compression rollers is 3, and the pressure is 1kg, 4kg and 8kg respectively) to obtain the single-layer resin adhesive film composite graphene film prepreg. And cooling, cutting and rolling the graphene film prepreg to obtain the final delivery product. Through testing, the electric conductivity of the graphene film prepreg is about 1000S/m, the horizontal thermal conductivity is 20W/m.k, and the vertical thermal conductivity is 8W/m.k.
Claims (1)
1. A continuous preparation method of a graphene film prepreg is characterized by comprising the following steps: the graphene film prepreg is prepared by taking a resin adhesive film and a graphene film as raw materials through a hot melting process, wherein the resin adhesive film is formed by coating 100-1400mm width and 10-100g/m on release paper2The resin with the surface density is one of epoxy resin, phenolic resin, unsaturated polyester, polyurethane, bismaleimide resin and polyimide resin; the graphene film is a film with a three-dimensional network structure or a porous structure prepared by taking graphene as a main raw material, the raw material composition of the graphene film is determined according to the use function of the graphene film prepreg, and the used raw material consists of one or more of a conductive raw material and a non-conductive raw material, a heat-conducting raw material or an auxiliary raw material; the conductive raw material comprises reduced graphene oxide, graphene nanosheets, expanded graphene or graphene powder; the non-conductive raw materials comprise epoxy resin, phenolic resin, unsaturated polyester, polyurethane, bismaleimide resin, polyimide resin or graphene oxide; the heat-conducting raw material comprises boron nitride, aluminum oxide, aluminum nitride, magnesium oxide, silicon oxide or zinc oxide; the auxiliary raw materials comprise sodium hydroxide, hydroiodic acid, ammonia water, p-phenylenediamine or ethylenediamine, and the used solvent is one or more of deionized water, ethanol, acetone, dichloromethane, chloroform and tetrahydrofuranSeveral kinds of the raw materials; the preparation steps are as follows:
step one, continuously preparing a graphene film:
preparing slurry: formulating a raw material formula according to the use function of the graphene film prepreg, weighing corresponding raw materials and a solvent, and uniformly mixing to prepare graphene slurry with the concentration of 5-200 mg/ml;
(1) coating: storing the uniformly mixed slurry in a storage tank, placing the storage tank above a conveying carrier of a conductive film machine, adjusting a discharging switch to enable the slurry to flow onto the conveying carrier, starting the conveying switch, wherein the conveying speed is 0.1-1m/min, scraping the graphene slurry on the conveying carrier into a film with the thickness of 0.3-3mm and the width of 100 plus 1400mm by using a scraper and a baffle plate, wherein the conductive film machine comprises an unreeling device, a scraper device and a heating device, the unreeling device is arranged at the foremost end of the conductive film machine, the conveying carrier is arranged on the unreeling device, the conveying carrier is pulled to pass through the scraper device and the heating device, and then the conveying carrier enters a pre-dipping machine, and conveying power is provided by a pre-dipping machine;
(2) film forming: the scraped graphene slurry film is conveyed forwards to a heating area of a conductive film machine through a conveying carrier and passes through a conveying carrier 30oC-120 oC, performing temperature treatment to obtain a graphene film;
step two, continuously preparing a graphene film prepreg:
conveying the prepared graphene film to the front end of a compression roller platform of a pre-dipping machine through a conveying carrier, realizing preliminary compounding of the graphene film and a resin adhesive film through a conveying device of the pre-dipping machine, conveying the compound of the graphene film and the resin adhesive film to an area, provided with a temperature system and a compression roller system, of the pre-dipping machine at 30oC-200 oAnd C, treating the graphene film by a compression roller with the pressure of 0.1-20kg to obtain the graphene film prepreg.
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| 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 |
| CN115464941A (en) * | 2022-09-15 | 2022-12-13 | 上海伽材新材料科技有限公司 | Preparation method of carbon fiber/graphene composite electromagnetic shielding prepreg |
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