CN114752094A - Preparation method of high-strength light epoxy resin composite thermal insulation material for motor home - Google Patents
Preparation method of high-strength light epoxy resin composite thermal insulation material for motor home Download PDFInfo
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Abstract
The invention relates to the technical field of high polymer materials, in particular to a preparation method of a high-strength light epoxy resin composite heat-insulating material for a caravan; the method comprises the following steps: obtaining a functionalized carbon nanotube for later use; preparing a micro-nano graphene sheet for later use; carrying out liquid-phase oxidation treatment on the micro-nano graphene sheet to prepare an oxidized micro-nano graphene sheet; acquiring a forecast; soaking the honeycomb-shaped glass fiber into the expectation, so that the liquid phase expectation is continuously expanded along the surface of the glass fiber and fused with each other; after the epoxy resin composite heat-insulating material is expected to be cured, the high-strength light epoxy resin composite heat-insulating material can be obtained, and the preparation method is correspondingly improved, so that the comprehensive performance of the composite material is improved.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a preparation method of a high-strength light epoxy resin composite thermal insulation material for a motor home.
Background
When the motor home is used, the shell is easy to break and break due to accidents, and most of the reasons are that the shell is made of a sandwich plate, namely a mode of glass fiber reinforced plastic, foam and a multilayer plate, and the shock resistance is poor, so that the safety of drivers is difficult to ensure when the accidents occur;
In the prior art, some composite materials are provided for improving the safety of the shell, but the comprehensive performance cannot meet the requirement.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength light-weight epoxy resin composite thermal insulation material for a motor home, and aims to solve the problem that the composite material in the prior art is insufficient in impact resistance.
In order to realize the aim, the invention provides a preparation method of a high-strength light-weight epoxy resin composite thermal insulation material for a caravan, which comprises the following steps:
taking a carbon nano tube as a raw material, and carrying out functional treatment on the carbon nano tube to obtain a functional carbon nano tube for later use;
preparing a micro-nano graphene sheet for later use by taking expanded graphite as a raw material;
carrying out liquid-phase oxidation treatment on the micro-nano graphene sheet to prepare a micro-nano graphene oxide sheet;
and shearing the micro-nano graphene oxide sheet to prepare the micro-nano graphene oxide sheet.
Mixing micro-nano graphene oxide sheets, a silane coupling agent, a dispersing agent, ethyl acetate, a functionalized carbon nano tube, absolute ethyl alcohol and liquid-phase epoxy resin, performing ultrasonic dispersion uniformly, heating to remove ethyl acetate and absolute ethyl alcohol, and adding a curing agent to obtain a forecast;
Immersing cellular glass fibers into the preform so that the preform of liquid phase continuously expands and fuses with each other along the surfaces of the glass fiber fibers;
and after the expectation is cured, obtaining the high-strength light epoxy resin composite thermal insulation material.
Wherein the functionalization process comprises the steps of:
using a carbon nano tube as a raw material, submerging the carbon nano tube by using mixed acid of sulfuric acid and nitric acid with a volume ratio of 3:1, carrying out constant-temperature water bath and carrying out ultrasonic treatment;
after ultrasonic treatment, cooling to room temperature, and repeatedly washing the solid surface with deionized water until the pH value is neutral;
and then carrying out vacuum filtration, soaking the solid obtained by vacuum filtration in acetone, and after the surface moisture is fully exchanged with the acetone, carrying out vacuum drying to obtain the functionalized carbon nanotube.
Wherein the functionalized carbon nanotube is a carboxylated carbon nanotube.
The preparation method of the micro-nano graphene sheet comprises the following steps of:
mixing expanded graphite with epoxy resin according to a mass ratio to obtain a preparation raw material;
heating the preparation raw materials, and stirring until the expanded graphite and the epoxy resin in the preparation raw materials are in a uniform state;
after the raw materials are cooled to room temperature, grinding the raw materials by using a three-roll grinder, and collecting the mixture after stripping;
And adding acetone into the mixture, ultrasonically cleaning and centrifuging, pouring into a magnetic boat, waiting for acetone to volatilize, and drying in vacuum to obtain the micro-nano graphene sheet.
Wherein the mass ratio is that the expanded graphite accounts for 0.5-5% of the mass of the epoxy resin.
Wherein the liquid phase oxidation treatment comprises the steps of:
placing the micro-nano graphene sheet in concentrated nitric acid, carrying out constant-temperature water bath, and then cleaning the soaked micro-nano graphene sheet until the pH value is neutral;
and (3) carrying out air-blast drying on the treated micro-nano graphene sheet, and shearing to 1-3 mm to obtain the micro-nano graphene oxide sheet.
The invention relates to a preparation method of a high-strength light epoxy resin composite heat-insulating material for a caravan, which is characterized in that on the basis of the prior art, the preparation method of the epoxy resin composite material is improved, the impact resistance of the composite material is improved by additionally arranging a carbon nano tube and a micro-nano graphene oxide sheet, the structure of the composite material is improved, and the impact resistance of the composite material is further improved by utilizing the stability of a honeycomb structure.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a mechanical property diagram of the oxidized micro-nano graphene sheet/epoxy resin composite material with different contents provided by the invention.
Fig. 2 is a graph showing the relationship between the tensile strength and the mass content of the oxidized micro-nano graphene sheet/functionalized carbon nanotube/epoxy resin composite material provided by the invention.
Fig. 3 is a schematic diagram of the bending strength and the content of the oxidized micro-nano graphene sheet/functionalized carbon nanotube/epoxy resin composite material provided by the present invention.
FIG. 4 is a step diagram of a preparation method of the high-strength light-weight epoxy resin composite thermal insulation material for the caravan.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 to 4, the present invention provides a method for preparing a high-strength light-weight epoxy resin composite thermal insulation material for a caravan, comprising the following steps:
s101: taking a carbon nano tube as a raw material, and carrying out functional treatment on the carbon nano tube to obtain a functional carbon nano tube for later use;
s102: preparing a micro-nano graphene sheet for later use by taking expanded graphite as a raw material;
s103: carrying out liquid-phase oxidation treatment on the micro-nano graphene sheet to prepare an oxidized micro-nano graphene sheet;
s104: shearing the oxidized micro-nano graphene sheet to prepare the oxidized micro-nano graphene sheet;
s105: mixing the oxidized micro-nano graphene sheet, a silane coupling agent, a dispersing agent, ethyl acetate, a functionalized carbon nano tube, absolute ethyl alcohol and liquid-phase epoxy resin, then ultrasonically dispersing the mixture uniformly, heating the mixture to remove the ethyl acetate and the absolute ethyl alcohol, and adding a curing agent to obtain a prediction;
s106: immersing cellular glass fibers into the pre-forms so that the pre-forms of the liquid phase are continuously expanded and fused with each other along the surfaces of the glass fiber fibers;
s107: and curing the anticipated material to obtain the high-strength light-weight epoxy resin composite heat-insulating material.
The preparation process of the composite material is improved, the carbon nano tube and the micro-nano graphene oxide sheet are additionally arranged in the epoxy resin, the structural strength of the epoxy resin is effectively improved, the process of preparing the caravan by using the epoxy resin is improved, the structural strength of the honeycomb is utilized, the epoxy resin is prepared into a honeycomb structure, and the composite material applied to the caravan has good impact resistance and heat preservation capability.
Further, the functionalization process comprises the following steps:
using a carbon nano tube as a raw material, submerging the carbon nano tube by using mixed acid of sulfuric acid and nitric acid in a volume ratio of 3:1, carrying out constant-temperature water bath and carrying out ultrasonic treatment;
after ultrasonic treatment, cooling to room temperature, and repeatedly washing the solid surface with deionized water until the pH value is neutral;
and then carrying out vacuum filtration, soaking the solid obtained by vacuum filtration in acetone, and after the surface moisture is fully exchanged with the acetone, carrying out vacuum drying to obtain the functionalized carbon nanotubes.
The carbon nanotubes are functionalized, so that the impact resistance of the composite material can be effectively improved after the carbon nanotubes are mixed with the epoxy resin.
Further, the functionalized carbon nanotubes are carboxylated carbon nanotubes.
The carboxylated carbon nanotubes can be compounded with the oxidized micro-nano graphene sheets, and after epoxy resin is blended, the anti-combustion capacity of the epoxy resin is improved.
Further, the preparation of the micro-nano graphene sheet by using the expanded graphite as a raw material comprises the following steps:
mixing the expanded graphite with epoxy resin according to a mass ratio to obtain a preparation raw material;
heating the preparation raw materials and then stirring the raw materials until the expanded graphite and the epoxy resin in the preparation raw materials are in a uniform state;
After the preparation raw materials are cooled to room temperature, grinding the raw materials by using a three-roll grinder, and collecting a mixture after stripping;
and adding acetone into the mixture, ultrasonically cleaning and centrifuging, pouring into a magnetic boat, waiting for acetone to volatilize, and drying in vacuum to obtain the micro-nano graphene sheet.
By improving the preparation process of the micro-nano graphene sheet, on one hand, the subsequent preparation of the micro-nano graphene oxide sheet is facilitated, and on the other hand, the forming quality of the micro-nano graphene oxide sheet can be improved.
Further, the mass ratio of the expanded graphite to the epoxy resin is 0.5-5%.
Further, the liquid phase oxidation treatment comprises the following steps:
placing the micro-nano graphene sheet in concentrated nitric acid, carrying out constant-temperature water bath, and then cleaning the soaked micro-nano graphene sheet until the pH value is neutral;
and (3) carrying out air-blast drying on the treated micro-nano graphene sheet, and shearing to 1-3 mm to obtain the micro-nano graphene oxide sheet.
Further, the high-strength light epoxy resin composite thermal insulation material for the caravan comprises the following components in parts by weight: 0.5-1 part of oxidized micro-nano graphene sheet, 0.5-1 part of functionalized carbon nano tube, 100 parts of liquid-phase epoxy resin, 34 parts of curing agent, 1-4 parts of silane coupling agent, 2-30 parts of dispersing agent and further, the silane coupling agent is an aqueous solution of aminopropyltriethoxysilane and ethanol.
And (3) performance test:
the stretching and bending test of the micro-nano graphene sheet on epoxy resin comprises the following steps:
according to the GB/T2567-2008 resin casting body performance test method, a sample is subjected to a tensile test and a three-point bending test, so that the influence of the micro-nano graphene sheet on the mechanical performance of the composite material is researched.
Micro-nano graphene sheets with the mass contents of 0%, 0.5%, 1% and 1.5% are respectively mixed into the epoxy resin, the test result is shown in figure 1,
according to fig. 1, when the content of the micro-nano graphene sheet is 0.5 wt%, the strength of the micro-nano graphene sheet is reduced compared with that of epoxy resin, which may be because the micro-nano graphene sheet is added to damage a resin matrix structure, and a certain defect is formed inside the resin matrix structure, and because the content of the micro-nano graphene sheet is small, the micro-nano graphene sheet can bear less stress, when the content of the micro-nano graphene sheet is 0.7 wt%, the bending strength reaches 89.69Mpa at the maximum, which is increased by 30%, and when the content of the micro-nano graphene sheet is 1.0 wt%, the tensile strength reaches 55.61Mpa at the maximum, which is increased by 5.2%, and meanwhile, the bending performance of the epoxy resin composite material is enhanced by the micro-nano graphene sheet is better than the tensile performance of the epoxy resin composite material, which may be because the micro-nano graphene sheet generates a certain orientation when being mixed in the epoxy resin, and the orientation is often the direction of the micro-nano graphene sheet dispersing stress effect, the orientation effect is possibly more beneficial to the dispersion effect of stress in a bending test, when the content of the micro-nano graphene sheets is 1.5 wt%, the strength of the micro-nano graphene sheets is obviously reduced compared with that of a base body and reaches the minimum, probably because the micro-nano graphene sheets have more content and are agglomerated in the resin base body, the micro-nano graphene sheets cannot be fully infiltrated by resin, a plurality of weak bonding interfaces are formed, and when a material is stressed, the micro-nano graphene sheets are desorbed and pulled out from the weak interfaces, so that the stress transfer loses effect.
And (3) performance test:
the functionalized carbon nanotubes and the oxidized micro-nano graphene sheets are used for performing a tensile and bending test on the epoxy resin in a synergistic manner:
the proportions of the oxidized micro-nano graphene sheet and the functionalized carbon nanotube are respectively 0.5-0.5%, 0.5-1%, 0.75-0.75% and 1-0.5%, which are respectively defined as F5N5, F7N7, F5N10 and F10N5, namely, the composite material containing 0.5 wt% of the oxidized micro-nano graphene sheet, 0.5 wt% of the carbon nanotube and the epoxy resin, the composite material containing 0.7 wt% of the oxidized micro-nano graphene sheet, 0.7 wt% of the carbon nanotube and the epoxy resin, the composite material containing 0.5 wt% of the oxidized micro-nano graphene sheet, 1.0 wt% of the carbon nanotube and the epoxy resin, the composite material containing 1.0 wt% of the oxidized micro-nano graphene sheet, 0.5 wt% of the carbon nanotube and the epoxy resin, and the F7, F10 and the like in the following text refer to the oxidized micro-nano graphene sheet/epoxy resin composite material containing the oxidized graphene sheet in corresponding mass percentage.
The results of the test are shown in figure 2,
according to fig. 2, the tensile strength of the epoxy resin composite material added with the micro-nano graphene oxide sheets shows a trend of firstly decreasing and then increasing, the tensile strength of F10 reaches the maximum and is increased by 5.9%, and the tensile strength of the three-phase composite material shows that the tensile strength of F5N5 is increased by 19.2% to the maximum; the F7N7 and F10N5 are smaller than the matrix, but it can be found that the tensile strength of the composite material is gradually increased along with the increase of the content of the functionalized carbon nanotubes, and the strength of the F5N10 is only inferior to that of the F5N5, which indicates that the tensile property of the material can be improved by adding the carbon nanotubes.
According to fig. 3, the bending strength of all materials shows a trend of increasing and then decreasing, in the micro-nano graphene oxide sheet/epoxy resin composite material, when the content of the micro-nano graphene oxide sheet is 0.5 wt%, the bending strength reaches 89.69Mpa at most, F5N5 and F5F10 are reduced, and the bending strength is smaller as the content of the micro-nano graphene oxide sheet increases, wherein the bending strength of F7 is reduced to 65Mpa and smaller than that of a matrix, the bending strength of F7N7 is represented to be the largest and reaches 104Mpa and is improved by 50.7% than that of the matrix resin, the bending strength of F10N5 is also improved relative to that of F10, which shows that the functionalized carbon nanotubes and the micro-nano graphene oxide sheet under a certain proportion can fully exert the synergistic enhancement effect on mechanics, the enhancement effect mainly depends on the bonding strength of an interface, according to a stress transfer theory, when the composite material is stressed, load is applied to the resin matrix, then the matrix transmits stress to the reinforcement through the interface, and the reinforcement plays a role in dispersing force to a certain extent; in the theory of chemical bonds, functional groups such as carboxyl groups can be added to the functionalized carbon nanotubes to generate certain bonding with the modified micro-nano graphene oxide sheets, and the functionalized carbon nanotubes can also react with epoxy resin through epoxy functions of the functionalized carbon nanotubes to form a three-dimensional network cured substance, so that the bonding strength of the interface between the matrix and the reinforcement is increased, wherein the unique nanostructure of the carbon nanotubes and the high strength of the micro-nano graphene oxide sheets are the basis of mechanical reinforcement.
The invention relates to a preparation method of a high-strength light epoxy resin composite heat-insulating material for a caravan, which is characterized in that on the basis of the prior art, the preparation method of the epoxy resin composite material is improved, the impact resistance of the composite material is improved by additionally arranging a carbon nano tube and a micro-nano graphene oxide sheet, the structure of the composite material is improved, and the impact resistance of the composite material is further improved by utilizing the stability of a honeycomb structure.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A preparation method of a high-strength light-weight epoxy resin composite heat-insulating material for a motor home, which is characterized in that,
the method comprises the following steps:
taking a carbon nano tube as a raw material, and carrying out functional treatment on the carbon nano tube to obtain a functional carbon nano tube for later use;
preparing a micro-nano graphene sheet for later use by taking expanded graphite as a raw material;
carrying out liquid-phase oxidation treatment on the micro-nano graphene sheet to prepare an oxidized micro-nano graphene sheet;
Mixing micro-nano graphene oxide sheets, a silane coupling agent, a dispersing agent, ethyl acetate, a functionalized carbon nano tube, absolute ethyl alcohol and liquid-phase epoxy resin, performing ultrasonic dispersion uniformly, heating to remove ethyl acetate and absolute ethyl alcohol, and adding a curing agent to obtain a forecast;
immersing cellular glass fibers into the preform so that the preform of liquid phase continuously expands and fuses with each other along the surfaces of the glass fiber fibers;
and after the expectation is cured, obtaining the high-strength light epoxy resin composite thermal insulation material.
2. The method for preparing the high-strength light-weight epoxy resin composite thermal insulation material for the caravan according to claim 1,
the functionalization processing comprises the following steps:
using a carbon nano tube as a raw material, submerging the carbon nano tube by using mixed acid of sulfuric acid and nitric acid in a volume ratio of 3:1, carrying out constant-temperature water bath and carrying out ultrasonic treatment;
after ultrasonic treatment, cooling to room temperature, and repeatedly washing the solid surface with deionized water until the pH value is neutral;
and then carrying out vacuum filtration, soaking the solid obtained by vacuum filtration in acetone, and after the surface moisture is fully exchanged with the acetone, carrying out vacuum drying to obtain the functionalized carbon nanotubes.
3. The method for preparing the high-strength light-weight epoxy resin composite thermal insulation material for the caravan according to claim 2,
The functionalized carbon nano-tube is a carboxylated carbon nano-tube.
4. The method for preparing the high-strength light-weight epoxy resin composite thermal insulation material for the caravan according to claim 3,
the preparation method of the micro-nano graphene sheet by using the expanded graphite as the raw material comprises the following steps:
mixing the expanded graphite with epoxy resin according to a mass ratio to obtain a preparation raw material;
heating the preparation raw materials and then stirring the raw materials until the expanded graphite and the epoxy resin in the preparation raw materials are in a uniform state;
after the preparation raw materials are cooled to room temperature, grinding the raw materials by using a three-roll grinder, and collecting a mixture after stripping;
and adding acetone into the mixture, ultrasonically cleaning and centrifuging, pouring into a magnetic boat, waiting for acetone to volatilize, and drying in vacuum to obtain the micro-nano graphene sheet.
5. The method for preparing the high-strength light-weight epoxy resin composite thermal insulation material for the caravan according to claim 4,
the mass ratio is that the expanded graphite accounts for 0.5-5% of the mass of the epoxy resin.
6. The method for preparing the high-strength light-weight epoxy resin composite thermal insulation material for the caravan according to claim 5,
the liquid phase oxidation treatment comprises the following steps:
Placing the micro-nano graphene sheet in concentrated nitric acid, carrying out constant-temperature water bath, and then cleaning the soaked micro-nano graphene sheet until the pH value is neutral;
and (4) carrying out air blast drying on the treated micro-nano graphene sheet, and shearing to 1-3 mm to obtain the micro-nano graphene oxide sheet.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448239A (en) * | 2014-10-11 | 2015-03-25 | 浙江大学 | High-strength epoxy resin composite material and preparation method thereof |
| CN105968717A (en) * | 2016-05-20 | 2016-09-28 | 北京化工大学 | Preparation of carbon fiber/graphene/carbon nanotube/epoxy resin prepreg and carbon fiber composite material |
| WO2017219944A1 (en) * | 2016-06-20 | 2017-12-28 | 山东欧铂新材料有限公司 | Method for preparing graphene-epoxy resin composite material |
| CN109504036A (en) * | 2018-11-16 | 2019-03-22 | 南昌航空大学 | A kind of micro-nano graphite flake epoxy resin-matrix/modified carbon fiber composite material and preparation method |
| CN111073222A (en) * | 2019-12-17 | 2020-04-28 | 江苏理工学院 | Preparation method of graphene oxide/carbon nanotube reinforced glass fiber laminated plate |
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- 2022-05-05 CN CN202210477891.4A patent/CN114752094A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448239A (en) * | 2014-10-11 | 2015-03-25 | 浙江大学 | High-strength epoxy resin composite material and preparation method thereof |
| CN105968717A (en) * | 2016-05-20 | 2016-09-28 | 北京化工大学 | Preparation of carbon fiber/graphene/carbon nanotube/epoxy resin prepreg and carbon fiber composite material |
| WO2017219944A1 (en) * | 2016-06-20 | 2017-12-28 | 山东欧铂新材料有限公司 | Method for preparing graphene-epoxy resin composite material |
| CN109504036A (en) * | 2018-11-16 | 2019-03-22 | 南昌航空大学 | A kind of micro-nano graphite flake epoxy resin-matrix/modified carbon fiber composite material and preparation method |
| CN111073222A (en) * | 2019-12-17 | 2020-04-28 | 江苏理工学院 | Preparation method of graphene oxide/carbon nanotube reinforced glass fiber laminated plate |
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