CN114957914A - Carbon fiber composite material and preparation and recovery method thereof - Google Patents

Carbon fiber composite material and preparation and recovery method thereof Download PDF

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CN114957914A
CN114957914A CN202210313665.2A CN202210313665A CN114957914A CN 114957914 A CN114957914 A CN 114957914A CN 202210313665 A CN202210313665 A CN 202210313665A CN 114957914 A CN114957914 A CN 114957914A
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parts
carbon fiber
graphite powder
expanded graphite
composite material
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王博
唐亮
屈建
陈兴元
汪登
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China State Construction Engineering Corp Ltd CSCEC
China State Construction Engineering Industry Technology Research Institute
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China State Construction Engineering Corp Ltd CSCEC
China State Construction Engineering Industry Technology Research Institute
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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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • 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
    • C08J11/00—Recovery or working-up of waste materials
    • C08J11/04—Recovery or working-up of waste materials of polymers
    • C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
    • C08J11/12—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by dry-heat treatment only
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/62—Plastics recycling; Rubber recycling

Abstract

The application discloses a carbon fiber composite material and a preparation and recovery method of the carbon fiber composite material, wherein the carbon fiber composite material comprises the following components in parts by weight: 100 parts of epoxy resin, 7-15 parts of modified expanded graphite powder, 15-25 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive; the modified expanded graphite powder comprises the following components in parts by weight: 100 parts of expanded graphite powder, 0.5-1.5 parts of gamma-aminopropyl triethoxysilane, 90 parts of absolute ethyl alcohol and 510 parts of deionized water.

Description

Carbon fiber composite material and preparation and recovery method thereof
Technical Field
The application relates to the technical field of composite material preparation, in particular to a carbon fiber composite material and a preparation and recovery method of the carbon fiber composite material.
Background
The carbon fiber composite material has excellent performances of light weight, high strength, corrosion resistance and the like, and is widely applied to various industries such as wind power, ships, buildings, rail transit and the like. However, since the carbon fiber composite material has excellent properties such as high strength and good corrosion resistance, the disposal of the waste of the carbon fiber composite material is also very troublesome.
With the increasing of the awareness of people on protecting the environment, the pollution problem of the thermosetting composite material waste to the environment also draws the wide attention of people. The waste of thermosetting composite materials mainly comes from defective products, leftover materials and composite material products with lost functions in the production process. Obviously, the more varieties and yields of thermoset composite waste, the more waste. At present, the recycling method of the carbon fiber composite material mainly comprises a pyrolysis method, a mechanical crushing method, an incineration method, a chemical dissolution method and the like, but the methods have the problems of high energy consumption, large pollution and the like.
In addition, since the existing carbon fiber composite material has a high demand for a recycling method, it is important to research a carbon fiber composite material which has a low demand for a recycling method and can reduce energy consumption during recycling.
Aiming at the technical problem that the normal work of the carbon fiber composite material can be ensured and the carbon fiber composite material can be recycled at a lower temperature, an effective solution is not provided at present.
Disclosure of Invention
The disclosure provides a carbon fiber composite material and a preparation and recovery method of the carbon fiber composite material, which at least solve the technical problem that the normal work of the carbon fiber composite material can be ensured and the carbon fiber composite material can be recovered at a lower temperature in the prior art.
According to one aspect of the application, a carbon fiber composite material is provided, which comprises the following components in parts by weight: 100 parts of epoxy resin, 7-15 parts of modified expanded graphite powder, 15-25 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive; the modified expanded graphite powder comprises the following components in parts by weight:
100 parts of expanded graphite powder, 0.5-1.5 parts of gamma-aminopropyltriethoxysilane, 90 parts of absolute ethyl alcohol and 510 parts of deionized water.
According to another aspect of the present application, there is provided a method of preparing a carbon fiber composite material, including: preparing materials according to the following parts by weight: 100 parts of epoxy resin, 7-15 parts of modified expanded graphite powder, 15-25 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive; adding the modified expanded graphite powder, the carbon fibers, the curing agent and the additive into epoxy resin to obtain a mixture consisting of the modified expanded graphite powder, the carbon fibers, the curing agent, the additive and the epoxy resin; and filling the mixture into a mold for heating to prepare the carbon fiber composite material.
According to another aspect of the present application, there is provided a method for recycling the carbon fiber composite material according to any one of claims 1 to 2, the carbon fiber composite material produced by the method according to any one of claims 3 to 7, comprising: crushing the carbon fiber composite material into carbon fiber composite material blocks with the diameter less than 5 cm; heating the carbon fiber composite material block to obtain a spalled carbon fiber composite material block; crushing the carbon fiber composite material blocks subjected to spalling, and screening and collecting a mixture obtained by crushing to obtain a carbon fiber crude product; and extruding the carbon fiber crude product, and screening and collecting the extruded carbon fiber crude product to obtain the recycled carbon fiber.
The carbon fiber composite material mainly comprises 100 parts by weight of epoxy resin, 7-15 parts by weight of modified expanded graphite powder, 15-25 parts by weight of carbon fiber, 80 parts by weight of curing agent and 3 parts by weight of additive. The modified expanded graphite powder is added in the preparation of the carbon fiber composite material, and the modified expanded graphite powder can expand after being heated to a certain temperature, so that the carbon fiber composite material can be subjected to spalling after being heated to a certain temperature. And extruding and screening the carbon fiber composite material after the bursting, and collecting the carbon fiber capable of being recycled. In addition, the temperature of the carbon fiber composite material added with the modified expanded graphite powder during spalling is far lower than the temperature required by the pyrolysis method for recycling the carbon fiber composite material. Therefore, the carbon fiber composite material in the application can greatly reduce the requirement on recycling conditions, reduce the consumption of energy and avoid the pollution to the environment. In addition, the expansion temperature of the modified expanded graphite powder is 150-180 ℃, so that the carbon fiber composite material cannot be cracked when being normally used for construction, and the carbon fiber composite material cannot normally work. Therefore, the technical effects that normal work of the carbon fiber composite material can be guaranteed, the carbon fiber composite material can be recycled at a lower temperature, resources needed by the carbon fiber composite material are reduced, and cost needed by the carbon fiber composite material is reduced are achieved through the product structure. And the technical problem that the normal work of the carbon fiber composite material can be ensured and the carbon fiber composite material can be recycled at a lower temperature in the prior art is solved.
The above and other objects, advantages and features of the present application will become more apparent to those skilled in the art from the following detailed description of specific embodiments thereof, taken in conjunction with the accompanying drawings.
Drawings
Some specific embodiments of the present application will be described in detail hereinafter by way of illustration and not limitation with reference to the accompanying drawings. The same reference numbers in the drawings identify the same or similar elements or components. Those skilled in the art will appreciate that the drawings are not necessarily drawn to scale. In the drawings:
FIG. 1 is a schematic flow diagram of a method for preparing a carbon fiber composite according to one embodiment of the present application.
Detailed Description
It should be noted that, in the present disclosure, the embodiments and features of the embodiments may be combined with each other without conflict. The present disclosure will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
In order to make the technical solutions of the present disclosure better understood by those skilled in the art, the technical solutions of the embodiments of the present disclosure will be clearly and completely described below with reference to the drawings in the embodiments of the present disclosure, and it is obvious that the described embodiments are only some embodiments of the present disclosure, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments disclosed herein without making any creative effort, shall fall within the protection scope of the present disclosure.
It should be noted that the terms "first," "second," and the like in the description and claims of the present disclosure and in the above-described drawings are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances for describing the embodiments of the disclosure herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
The application provides a carbon fiber composite material, which comprises the following components in parts by weight: 100 parts of epoxy resin, 7-15 parts of modified expanded graphite powder, 15-25 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive; the modified expanded graphite powder comprises the following components in parts by weight: 100 parts of expanded graphite powder, 0.5-1.5 parts of gamma-aminopropyl triethoxysilane, 90 parts of absolute ethyl alcohol and 510 parts of deionized water.
As described in the background art, with the increasing awareness of environmental protection, the pollution problem of the thermosetting composite material waste to the environment has attracted people's attention. The waste of thermosetting composite materials mainly comes from defective products, leftover materials and composite material products with lost functions in the production process. Obviously, the more varieties and yields of thermoset composite waste, the more waste. At present, the recycling method of the carbon fiber composite material mainly comprises a pyrolysis method, a mechanical crushing method, an incineration method, a chemical dissolution method and the like, but the methods have the problems of high energy consumption, large pollution and the like. In addition, since the existing carbon fiber composite material has a high requirement for a recycling method, it is important to research a carbon fiber composite material which has a low requirement for a recycling method and reduces energy consumption during recycling.
In order to solve the technical problems, the application provides a carbon fiber composite material which mainly comprises 100 parts by weight of epoxy resin, 7-15 parts by weight of modified expanded graphite powder, 15-25 parts by weight of carbon fibers, 80 parts by weight of curing agent and 3 parts by weight of additive. The modified expanded graphite powder mainly comprises 100 parts of expanded graphite powder, 0.5-1.5 parts of gamma-aminopropyl triethoxysilane, 15-25 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive.
And because the carbon fiber composite material may reach a high temperature of 80 to 100 ℃ in hot summer. Therefore, if the low-temperature modified expanded graphite powder is added, the carbon fiber composite material may expand in daily use, so that the carbon fiber composite material cannot be normally used. When the carbon fiber composite material is recycled by a conventional method, high temperature of more than 300 ℃ is generally required. Therefore, the existing resources are wasted and the economic cost is high.
Therefore, the modified expanded graphite powder added into the carbon fiber composite material has the characteristic of being capable of expanding when the initial expansion temperature (150-180 ℃) is reached. Therefore, the carbon fiber composite material can not only meet the requirement of recycling at a lower temperature, but also meet the temperature condition of the carbon fiber composite material in normal use.
Therefore, when the carbon fiber composite material needs to be recycled, the carbon fiber composite material after spalling is crushed into a carbon fiber composite material block smaller than 5cm, and then the carbon fiber composite material is heated to 180 ℃ and maintained for 2 hours. And crushing the carbon fiber composite material by using a mechanical extrusion mode with the extrusion pressure of 6Mpa, screening the crushed mixture, and collecting to obtain a crude carbon fiber product. Then, the carbon fiber is extruded by a mechanical extrusion mode with the extrusion pressure of 1.2Mpa, and is screened and collected, so that the carbon fiber which can be recycled is finally obtained.
The carbon fiber composite material can use E51 epoxy resin as a preparation raw material, the curing agent is methyltetrahydrophthalic anhydride, and the additive is one or more of a UV-absorbent, an antioxidant, a flame retardant, a release agent, a defoaming agent, nanoparticles and a stabilizer.
Therefore, the technical effects that normal work of the carbon fiber composite material can be guaranteed, the carbon fiber composite material can be recycled at a lower temperature, resources needed by the carbon fiber composite material are reduced, and cost needed by the carbon fiber composite material is reduced are achieved through the product structure. And the technical problem that the normal work of the carbon fiber composite material can be ensured and the carbon fiber composite material can be recycled at a lower temperature in the prior art is solved.
In addition, table 1 shows data of parts by weight of expanded graphite powder, modified expanded graphite powder, carbon fiber, curing agent, and additives among the modified expanded graphite powder in 6 experiments.
TABLE 1
Figure BDA0003568085520000051
Table 2 shows the weight parts data of epoxy resin, modified expanded graphite powder, carbon fiber, curing agent and additives in the carbon fiber composite in 6 experiments. The method for preparing the modified graphite powder comprises the following steps:
TABLE 2
Figure BDA0003568085520000052
Example 1:
when the gamma-aminopropyltriethoxysilane content is 0.7 part, the modified expanded graphite powder content is 12 parts, and the carbon fiber content is 20 parts, the carbon fiber composite material is prepared.
The method comprises the following steps: the preparation method comprises the following steps of preparing materials according to the weight part data of an experimental group 1, wherein 100 parts of expanded graphite powder, 510 parts of deionized water, 90 parts of absolute ethyl alcohol and 0.7 part of gamma-aminopropyltriethoxysilane are used. Wherein the particle size of the used expanded graphite powder is 10-20 μm, the expansion volume is 400-500 mL/g, and the actual expansion temperature is 150-180 ℃.
Step two: 10 parts of deionized water and 90 parts of absolute ethyl alcohol are mixed to obtain a first mixed solution.
Step three: and (3) dissolving 0.7 part of gamma-aminopropyltriethoxysilane in the first mixed solution to obtain a gamma-aminopropyltriethoxysilane solution.
Step four: and (3) ultrasonically dispersing 100 parts of expanded graphite powder into 500 parts of deionized water to obtain an expanded graphite powder dispersion liquid.
Step five: and dripping the gamma-aminopropyltriethoxysilane solution into the expanded graphite powder dispersion liquid to obtain a second mixed liquid. And slowly stirring the second mixed solution by using magnetic force, and controlling the temperature of the system to be 60 ℃. And after stirring for 1h, filtering the mixed solution, collecting expanded graphite powder, and cleaning the expanded graphite powder with distilled water. And then placing the cleaned expanded graphite powder in a vacuum oven at 6 ℃ for drying for 24 hours to finally obtain the modified expanded graphite powder.
Step six: and dispersing 12 parts of modified expanded graphite powder, 20 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive which are obtained by preparation into 100 parts of epoxy resin, and uniformly mixing.
Step seven: and filling the mixture into a mold, wherein the mold closing pressure of the mold is 2-8 Mpa. Uniformly heating the mold to 85-95 ℃, and maintaining the temperature for 120 min. And then heating the mold to 110-120 ℃, keeping the temperature for 60min, and finally cooling the mold to room temperature to obtain the carbon fiber composite material.
Example 2
When the gamma-aminopropyltriethoxysilane is 0.5 part, the modified expanded graphite powder is 7 parts, and the carbon fiber is 25 parts, the carbon fiber composite material is prepared.
The method comprises the following steps: the materials are prepared according to the weight part data of the experimental group 1, wherein 100 parts of expanded graphite powder, 510 parts of deionized water, 90 parts of absolute ethyl alcohol and 0.5 part of gamma-aminopropyltriethoxysilane are used. Wherein the particle size of the used expanded graphite powder is 10-20 μm, the expansion volume is 400-500 mL/g, and the actual expansion temperature is 150-180 ℃.
Step two: 10 parts of deionized water and 90 parts of absolute ethyl alcohol are mixed to obtain a first mixed solution.
Step three: and (2) dissolving 0.5 part of gamma-aminopropyl triethoxysilane in the first mixed solution to obtain a gamma-aminopropyl triethoxysilane solution.
Step four: and (3) ultrasonically dispersing 100 parts of expanded graphite powder into 500 parts of deionized water to obtain an expanded graphite powder dispersion liquid.
Step five: and dripping the gamma-aminopropyltriethoxysilane solution into the expanded graphite powder dispersion liquid to obtain a second mixed liquid. And slowly stirring the second mixed solution by using magnetic force, and controlling the temperature of the system to be 60 ℃. And after stirring for 1h, filtering the mixed solution, collecting expanded graphite powder, and cleaning the expanded graphite powder with distilled water. And then placing the cleaned expanded graphite powder in a vacuum oven at 6 ℃ for drying for 24 hours to finally obtain the modified expanded graphite powder.
Step six: dispersing 7 parts of modified expanded graphite powder, 25 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive in 100 parts of epoxy resin, and uniformly mixing.
Step seven: and filling the mixture into a mold, wherein the mold closing pressure of the mold is 2-8 Mpa. Uniformly heating the mold to 85-95 ℃, and maintaining the temperature for 120 min. And then heating the mold to 110-120 ℃, keeping the temperature for 60min, and finally cooling the mold to room temperature to obtain the carbon fiber composite material.
Example 3:
when the gamma-aminopropyltriethoxysilane content is 1.5 parts, the modified expanded graphite powder content is 9 parts, and the carbon fiber content is 16 parts, the carbon fiber composite material is prepared.
The method comprises the following steps: the preparation method comprises the following steps of preparing materials according to the data of the experimental group 1 by weight, wherein 100 parts of expanded graphite powder, 510 parts of deionized water, 90 parts of absolute ethyl alcohol and 1.5 parts of gamma-aminopropyltriethoxysilane are used. Wherein the particle size of the used expanded graphite powder is 10-20 μm, the expansion volume is 400-500 mL/g, and the actual expansion temperature is 150-180 ℃.
Step two: 10 parts of deionized water and 90 parts of absolute ethyl alcohol are mixed to obtain a first mixed solution.
Step three: and (3) dissolving 1.5 parts of gamma-aminopropyltriethoxysilane in the first mixed solution to obtain a gamma-aminopropyltriethoxysilane solution.
Step four: and (3) ultrasonically dispersing 100 parts of expanded graphite powder into 500 parts of deionized water to obtain an expanded graphite powder dispersion liquid.
Step five: and dripping the gamma-aminopropyltriethoxysilane solution into the expanded graphite powder dispersion liquid to obtain a second mixed liquid. And slowly stirring the second mixed solution by using magnetic force, and controlling the temperature of the system to be 60 ℃. And after stirring for 1h, filtering the mixed solution, collecting expanded graphite powder, and cleaning the expanded graphite powder with distilled water. And then placing the cleaned expanded graphite powder in a vacuum oven at 6 ℃ for drying for 24 hours to finally obtain the modified expanded graphite powder.
Step six: 9 parts of modified expanded graphite powder, 16 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive are dispersed in 100 parts of epoxy resin and uniformly mixed.
Step seven: and filling the mixture into a mold, wherein the mold closing pressure of the mold is 2-8 Mpa. Uniformly heating the mold to 85-95 ℃, and maintaining the temperature for 120 min. And then heating the mold to 110-120 ℃, keeping the temperature for 60min, and finally cooling the mold to room temperature to obtain the carbon fiber composite material.
Example 4:
when the gamma-aminopropyltriethoxysilane content is 1.3 parts, the modified expanded graphite powder content is 13 parts, and the carbon fiber content is 18 parts, the carbon fiber composite material is prepared.
The method comprises the following steps: the preparation method comprises the following steps of preparing materials according to the data of the experimental group 1 by weight, wherein 100 parts of expanded graphite powder, 510 parts of deionized water, 90 parts of absolute ethyl alcohol and 1.3 parts of gamma-aminopropyltriethoxysilane are used. Wherein the particle size of the used expanded graphite powder is 10-20 μm, the expansion volume is 400-500 mL/g, and the actual expansion temperature is 150-180 ℃.
Step two: 10 parts of deionized water and 90 parts of absolute ethyl alcohol are mixed to obtain a first mixed solution.
Step three: and (3) dissolving 1.3 parts of gamma-aminopropyltriethoxysilane in the first mixed solution to obtain a gamma-aminopropyltriethoxysilane solution.
Step four: and (3) ultrasonically dispersing 100 parts of expanded graphite powder into 500 parts of deionized water to obtain an expanded graphite powder dispersion liquid.
Step five: and dripping the gamma-aminopropyltriethoxysilane solution into the expanded graphite powder dispersion liquid to obtain a second mixed liquid. And slowly stirring the second mixed solution by using magnetic force, and controlling the temperature of the system to be 60 ℃. And after stirring for 1h, filtering the mixed solution, collecting expanded graphite powder, and cleaning the expanded graphite powder with distilled water. And then placing the cleaned expanded graphite powder in a vacuum oven at 6 ℃ for drying for 24 hours to finally obtain the modified expanded graphite powder.
Step six: 13 parts of modified expanded graphite powder, 18 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive are dispersed in 100 parts of epoxy resin and uniformly mixed.
Step seven: and filling the mixture into a mold, wherein the mold closing pressure of the mold is 2-8 Mpa. Uniformly heating the mold to 85-95 ℃, and maintaining the temperature for 120 min. And then heating the mold to 110-120 ℃, keeping the temperature for 60min, and finally cooling the mold to room temperature to obtain the carbon fiber composite material.
Example 5:
when the gamma-aminopropyltriethoxysilane content is 0.9 part, the modified expanded graphite powder content is 15 parts, and the carbon fiber content is 22 parts, the carbon fiber composite material is prepared.
The method comprises the following steps: the preparation method comprises the following steps of preparing materials according to the weight part data of an experimental group 1, wherein 100 parts of expanded graphite powder, 510 parts of deionized water, 90 parts of absolute ethyl alcohol and 0.9 part of gamma-aminopropyltriethoxysilane are used. Wherein the particle size of the used expanded graphite powder is 10-20 μm, the expansion volume is 400-500 mL/g, and the actual expansion temperature is 150-180 ℃.
Step two: 10 parts of deionized water and 90 parts of absolute ethyl alcohol are mixed to obtain a first mixed solution.
Step three: and (3) dissolving 0.9 part of gamma-aminopropyltriethoxysilane in the first mixed solution to obtain a gamma-aminopropyltriethoxysilane solution.
Step four: and (3) ultrasonically dispersing 100 parts of expanded graphite powder into 500 parts of deionized water to obtain an expanded graphite powder dispersion liquid.
Step five: and dripping the gamma-aminopropyltriethoxysilane solution into the expanded graphite powder dispersion liquid to obtain a second mixed liquid. And slowly stirring the second mixed solution by using magnetic force, and controlling the temperature of the system to be 60 ℃. And after stirring for 1h, filtering the mixed solution, collecting expanded graphite powder, and cleaning the expanded graphite powder with distilled water. And then placing the cleaned expanded graphite powder in a vacuum oven at 6 ℃ for drying for 24 hours to finally obtain the modified expanded graphite powder.
Step six: 15 parts of modified expanded graphite powder, 22 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive are dispersed in 100 parts of epoxy resin and uniformly mixed.
Step seven: and filling the mixture into a mold, wherein the mold closing pressure of the mold is 2-8 Mpa. Uniformly heating the mold to 85-95 ℃, and maintaining the temperature for 120 min. And then heating the mold to 110-120 ℃, keeping the temperature for 60min, and finally cooling the mold to room temperature to obtain the carbon fiber composite material.
Example 6:
when the gamma-aminopropyltriethoxysilane is 1 part, the modified expanded graphite powder is 10 parts, and the carbon fiber is 15 parts, the carbon fiber composite material is prepared.
The method comprises the following steps: the preparation method comprises the following steps of preparing materials according to the data of the experimental group 1 by weight, wherein 100 parts of expanded graphite powder, 510 parts of deionized water, 90 parts of absolute ethyl alcohol and 1 part of gamma-aminopropyltriethoxysilane are used. Wherein the particle size of the used expanded graphite powder is 10-20 μm, the expansion volume is 400-500 mL/g, and the actual expansion temperature is 150-180 ℃.
Step two: 10 parts of deionized water and 90 parts of absolute ethyl alcohol are mixed to obtain a first mixed solution.
Step three: and (3) dissolving 1 part of gamma-aminopropyltriethoxysilane in the first mixed solution to obtain a gamma-aminopropyltriethoxysilane solution.
Step four: and (3) ultrasonically dispersing 100 parts of expanded graphite powder into 500 parts of deionized water to obtain an expanded graphite powder dispersion liquid.
Step five: and dripping the gamma-aminopropyltriethoxysilane solution into the expanded graphite powder dispersion liquid to obtain a second mixed liquid. And slowly stirring the second mixed solution by using magnetic force, and controlling the temperature of the system to be 60 ℃. And after stirring for 1h, filtering the mixed solution, collecting expanded graphite powder, and cleaning the expanded graphite powder with distilled water. And then placing the cleaned expanded graphite powder in a vacuum oven at 6 ℃ for drying for 24 hours to finally obtain the modified expanded graphite powder.
Step six: dispersing 10 parts of modified expanded graphite powder, 15 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive in 100 parts of epoxy resin, and uniformly mixing.
Step seven: and filling the mixture into a mold, wherein the mold closing pressure of the mold is 2-8 Mpa. Uniformly heating the mold to 85-95 ℃, and maintaining the temperature for 120 min. And then heating the mold to 110-120 ℃, keeping the temperature for 60min, and finally cooling the mold to room temperature to obtain the carbon fiber composite material.
The carbon fiber composite material prepared in the 6 groups of examples is recycled, and the recycling method comprises the following steps:
the method comprises the following steps: and crushing the carbon fiber composite material into carbon fiber composite material blocks by using a crusher. Wherein the diameter of the carbon fiber composite material block needs to be less than 5 cm.
Step two: and (3) placing the carbon fiber composite material block in a heating box, heating to 180 ℃, and maintaining the whole heating process for 2 hours to prepare the spalling carbon fiber composite material block.
Step three: and crushing the carbon fiber composite material blocks which are subjected to spalling in a mechanical extrusion mode, and collecting a mixture of crushed carbon fiber composite materials to obtain a carbon fiber crude product. Wherein the extrusion pressure is 6 MPa.
Step four: and extruding, screening and collecting the obtained carbon fiber crude product by adopting a mechanical extrusion mode to finally obtain the recycled carbon fiber, wherein the extrusion pressure is 1.2 Mpa.
After the carbon fibers that can be recycled are obtained, the recovery rate of the carbon fibers is further examined. The first group is example 1, the second group is example 2, the third group is example 3, the fourth group is example 4, the fifth group is example 5, and the sixth group is example 6.
The results obtained are shown in table 3:
TABLE 3
Figure BDA0003568085520000101
The carbon fiber recovery rate is the weight of the carbon fiber obtained by recovery/the weight of the carbon fiber contained in the carbon fiber composite material before recovery. The residual resin content was determined according to the method provided by the national standard GB/T3855-2005. Therefore, after the modified expanded graphite powder is added, the recovery rate of the carbon fiber can reach 88% at most, and the content of the residual resin can reach 3.8% at least. Therefore, the modified expanded graphite powder is added in the process of preparing the carbon fiber composite material, so that the effects of improving the recovery rate of the carbon fiber and reducing the content of residual resin on the carbon fiber can be achieved.
And (3) comparing the carbon fiber recovery rate and the residual resin content of the carbon fiber composite material without adding the modified expanded graphite powder by taking the embodiment 4 as a comparison group, wherein the first group is the carbon fiber composite material without adding the modified expanded graphite powder, and the second group is the carbon fiber composite material prepared in the embodiment 4. The comparison results are detailed in table 4:
TABLE 4
Figure BDA0003568085520000102
Figure BDA0003568085520000111
As can be seen from table 4, when the carbon fiber composite material to which the modified expanded graphite powder was not added was recovered by the above recovery method, recovery of the carbon fibers could not be achieved. When the carbon fiber composite material added with the modified expanded graphite powder is recovered by the recovery method, the recovery rate of the carbon fiber composite material is 85 percent, and the content of the residual resin is 4.7 percent. Therefore, the recovery rate of the carbon fiber composite material can be greatly improved by adding the modified expanded graphite powder, and the residual resin content of the carbon fiber is reduced.
Further, the bending strength of the carbon fiber composite material of the above 6 examples and the bending strength of the carbon fiber composite material to which the modified expanded graphite powder was not added are shown in table 5. The first group was example 1, the second group was example 2, the third group was example 3, the fourth group was example 4, the fifth group was example 5, the sixth group was example 6, and the seventh group was the flexural strength of the carbon fiber composite material to which the modified expanded graphite powder was not added. As shown in the table 5 below, the following examples,
TABLE 5
Figure BDA0003568085520000112
Wherein, the bending strength of the carbon fiber composite material is measured according to the method provided by the national standard GB/T2567-2008.
As is clear from Table 5, the carbon fiber composite materials of examples 1 to 6 all had high flexural strength. Compared with the carbon fiber composite material without the modified expanded graphite powder, the bending strength of the first group of carbon fiber composite material with the modified expanded graphite powder is reduced by 3.1%; the bending strength of the second group of carbon fiber composite materials added with the modified expanded graphite powder is reduced by 2.0 percent compared with the carbon fiber composite materials not added with the modified expanded graphite powder; the bending strength of the carbon fiber composite material added with the modified expanded graphite powder in the third group is reduced by 5.5 percent compared with the carbon fiber composite material not added with the modified expanded graphite powder; the bending strength of the fourth group of carbon fiber composite materials added with the modified expanded graphite powder is reduced by 4.4 percent compared with the carbon fiber composite materials not added with the modified expanded graphite powder; the bending strength of the carbon fiber composite material added with the modified expanded graphite powder in the fifth group is reduced by 3.4 percent compared with the carbon fiber composite material not added with the modified expanded graphite powder; and compared with the carbon fiber composite material without the modified expanded graphite powder, the bending strength of the carbon fiber composite material added with the modified expanded graphite powder in the sixth group is reduced by 6.8%.
Therefore, it can be seen from the above data that the bending strength of the carbon fiber composite material to which the modified expanded graphite powder is added is reduced to a low extent as compared with the bending strength of the carbon fiber composite material to which the modified expanded graphite powder is not added, and there is substantially no change in the bending strength.
Table 6 shows the bending strength of the carbon fiber composite material to which the modified expanded graphite powder was not added, the bending strength of the carbon fiber composite material to which the unmodified expanded graphite powder was added, and the bending strength of the carbon fiber composite material to which the modified expanded graphite powder was added. With specific reference to table 6:
TABLE 6
Figure BDA0003568085520000121
Wherein, the bending strength of the carbon fiber composite material is measured according to the method provided by the national standard GB/T2567-2008.
As can be seen from table 6, the bending strength of the carbon fiber composite material to which the unmodified expanded graphite powder was added was reduced by 22% as compared to the bending strength of the carbon fiber composite material to which the modified expanded graphite powder was not added. Taking the fourth group of examples as an example, the bending strength of the carbon fiber composite material to which the modified expanded graphite powder was added was reduced by 4.4% as compared with the carbon fiber composite material to which the modified expanded graphite powder was not added. Therefore, the expanded graphite powder modified by the gamma-aminopropyltriethoxysilane is more beneficial to the retention of the strength of the carbon fiber composite material, so that the strength loss of the carbon fiber composite material can be smaller.
Therefore, the technical effects of improving the recovery rate of the carbon fiber composite material on the basis of not changing the bending strength of the carbon fiber composite material and saving resources in the recovery of the carbon fiber composite material are achieved in the process of preparing the carbon fiber composite material by using the modified expanded graphite powder.
The relative arrangement of the components and steps, the numerical expressions, and numerical values set forth in these embodiments do not limit the scope of the present disclosure unless specifically stated otherwise. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be discussed further in subsequent figures.
The above description is only for the preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present application should be covered within the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.

Claims (8)

1. The carbon fiber composite material is characterized by comprising the following components in parts by weight:
100 parts of epoxy resin, 7-15 parts of modified expanded graphite powder, 15-25 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive;
the modified expanded graphite powder comprises the following components in parts by weight:
100 parts of expanded graphite powder, 0.5-1.5 parts of gamma-aminopropyl triethoxysilane, 90 parts of absolute ethyl alcohol and 510 parts of deionized water.
2. The carbon fiber composite material according to claim 1, wherein the curing agent is methyltetrahydrophthalic anhydride.
3. A method for preparing a carbon fiber composite material is characterized by comprising the following steps:
preparing materials according to the following parts by weight: 100 parts of epoxy resin, 7-15 parts of modified expanded graphite powder, 15-25 parts of carbon fiber, 80 parts of curing agent and 3 parts of additive;
adding the modified expanded graphite powder, the carbon fibers, the curing agent and the additive into the epoxy resin to obtain a mixture consisting of the modified expanded graphite powder, the carbon fibers, the curing agent, the additive and the epoxy resin; and
and filling the mixture into a mold, and heating to prepare the carbon fiber composite material.
4. The method according to claim 3, wherein the step of filling the mixture into a mold and heating the mold to obtain the carbon fiber composite material comprises:
filling the mixture into a mold;
uniformly heating the die to 85-95 ℃ under the condition that the die closing pressure of the die is 2-8 Mpa, and heating the die at the temperature of 85-95 ℃ in a first period; and
and heating the mold to 110-120 ℃, and heating the mold at the temperature of 110-120 ℃ in the second period.
5. The method of claim 4, wherein the modified expanded graphite powder is prepared by a process comprising:
preparing materials according to the following parts by weight: 100 parts of expanded graphite powder, 0.5-1.5 parts of gamma-aminopropyltriethoxysilane, 90 parts of absolute ethyl alcohol and 510 parts of deionized water; and
and preparing the modified expanded graphite powder by using the expanded graphite powder, the gamma-aminopropyltriethoxysilane, the absolute ethyl alcohol and the deionized water.
6. The method of claim 5, wherein the preparing the modified expanded graphite powder from the expanded graphite powder, the gamma-aminopropyltriethoxysilane, the absolute ethanol and the deionized water comprises:
mixing the absolute ethyl alcohol and the deionized water to obtain a first mixed solution, wherein the deionized water accounts for 10 parts;
dissolving the gamma-aminopropyltriethoxysilane in the first mixed solution to obtain a gamma-aminopropyltriethoxysilane solution;
dispersing the expanded graphite powder in the deionized water to obtain an expanded graphite powder dispersion liquid, wherein the deionized water accounts for 500 parts; and
and preparing the modified expanded graphite powder by using the gamma-aminopropyltriethoxysilane solution and the expanded graphite powder dispersion liquid.
7. The method of claim 6, wherein preparing the modified expanded graphite powder from the gamma-aminopropyltriethoxysilane solution and the expanded graphite powder dispersion comprises:
dripping the gamma-aminopropyltriethoxysilane solution into the expanded graphite powder dispersion liquid to obtain a second mixed solution;
stirring the second mixed solution, and continuously heating the second mixed solution in the stirring process; and
filtering to obtain the modified expanded graphite powder.
8. A method for recycling the carbon fiber composite material as set forth in any one of claims 1 to 2 or the carbon fiber composite material produced by the method as set forth in any one of claims 3 to 7, comprising:
crushing the carbon fiber composite material into carbon fiber composite material blocks with the diameter less than 5 cm;
heating the carbon fiber composite material block to 180 ℃, and maintaining for 2h to obtain a burst carbon fiber composite material block;
crushing the carbon fiber composite material blocks subjected to spalling, and screening and collecting a mixture obtained by crushing to obtain a carbon fiber crude product, wherein the extrusion pressure is 6 Mpa; and
and extruding the carbon fiber crude product, and screening and collecting the extruded carbon fiber crude product to obtain the recycled carbon fiber, wherein the extrusion pressure is 1.2 Mpa.
CN202210313665.2A 2022-03-28 2022-03-28 Carbon fiber composite material and preparation and recovery method thereof Pending CN114957914A (en)

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