CN115850741A - Carbon fiber reinforced composite material and preparation method thereof - Google Patents
Carbon fiber reinforced composite material and preparation method thereof Download PDFInfo
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- CN115850741A CN115850741A CN202310152779.8A CN202310152779A CN115850741A CN 115850741 A CN115850741 A CN 115850741A CN 202310152779 A CN202310152779 A CN 202310152779A CN 115850741 A CN115850741 A CN 115850741A
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- carbon fiber
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- composite material
- reinforced composite
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 76
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 76
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000011208 reinforced composite material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 38
- 239000000725 suspension Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims description 42
- 239000011347 resin Substances 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000007731 hot pressing Methods 0.000 claims description 14
- 229920005992 thermoplastic resin Polymers 0.000 claims description 13
- 239000012046 mixed solvent Substances 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 239000002131 composite material Substances 0.000 claims description 9
- 239000004697 Polyetherimide Substances 0.000 claims description 7
- 229920001601 polyetherimide Polymers 0.000 claims description 7
- 238000000748 compression moulding Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 150000002894 organic compounds Chemical class 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 5
- -1 polypropylene Polymers 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 239000004800 polyvinyl chloride Substances 0.000 claims description 5
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 3
- 239000004626 polylactic acid Substances 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 2
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 2
- 229920000297 Rayon Polymers 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 238000007723 die pressing method Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920002530 polyetherether ketone Polymers 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- 239000002964 rayon Substances 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 abstract description 15
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 210000000078 claw Anatomy 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000003733 fiber-reinforced composite Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229920002292 Nylon 6 Polymers 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000004918 carbon fiber reinforced polymer Substances 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
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- Reinforced Plastic Materials (AREA)
Abstract
The invention provides a carbon fiber reinforced composite material and a preparation method thereof. The suspension is used as a medium, and solution impregnation and powder impregnation are combined, so that the prepared carbon fiber reinforced composite material is uniformly impregnated, the method is suitable for large-scale production, the production flow is convenient to operate, the process is simple, the equipment investment is low, the production efficiency is convenient to improve, and flexible production is realized.
Description
Technical Field
The invention relates to a carbon fiber reinforced composite material and a preparation method thereof, belonging to the field of composite materials.
Background
Thermoplastic resins and their composites have developed rapidly over the last decade. Compared with thermosetting materials, the thermoplastic resin has a series of advantages of excellent impact toughness, fatigue damage resistance, short molding period, high production efficiency, long-term storage, capability of repairing and recycling, and the like.
At present, fiber reinforced composite materials have the defects of uneven distribution and the like in reinforced fiber resin-making base materials, which greatly influences the performance of the materials. The traditional fiber reinforced resin material also has the defects of complex process and high price. Taking a traditional carbon fiber reinforced resin as an example, the preparation method comprises the following steps: the suspension is used as a medium, the advantages of powder impregnation and solution impregnation are combined, the fiber has good dispersibility in the suspension, the thermoplastic resin powder is fully combined, the solution impregnation can play a role in graft modification, and the suspension is used as the medium to obtain the carbon fiber composite material by combining two advantages. Powder impregnation and solution impregnation each have advantages and disadvantages and the high price limits the large number of applications of the fiber-reinforced resin material.
The main problem of the existing carbon fiber reinforced thermoplastic resin matrix composite material is uneven impregnation, which greatly influences the performance of the composite material.
Disclosure of Invention
In order to overcome the above disadvantages, the present invention provides a carbon fiber reinforced composite material and a method for preparing the same, wherein the method combines the advantages of solution impregnation and powder impregnation by using a suspension as a medium.
The carbon fiber reinforced composite material provided by the invention is prepared by the method comprising the following steps:
1) Dissolving soluble resin into a mixed solvent to obtain a solution 1, and adding ethanol into the obtained solution 1 to prepare a solution 2;
2) Adding PEG-100000 into the obtained solution 2 to increase the density of the solution 2;
3) Adding insoluble thermoplastic resin powder into the solution 2, and stirring and ultrasonically oscillating to obtain a resin powder suspension;
4) Adding short carbon fibers into the obtained resin powder suspension, and stirring and ultrasonically oscillating to obtain a carbon fiber suspension;
5) And taking out the carbon fiber suspension, filtering and drying to prepare a carbon fiber felt, and carrying out compression molding to obtain the carbon fiber reinforced composite material.
In step 1) of the method, the mixed solvent is prepared by mixing an organic compound and acetone, wherein the mass ratio of the organic compound to the acetone can be 1-3:7-9, specifically 3:7 or 2:8;
the organic compound is at least one of polyacrylic acid, N-dimethylacetamide and N, N-dimethylformamide;
the easily soluble resin is at least one of polymethyl methacrylate, polyvinyl chloride and polyetherimide;
the mass fraction range of the easily soluble resin in the mixed solvent is 2-8%;
the mass ratio of solution 1 to ethanol may be 1:1-3.
The soluble resin is added in the form of powder, and the particle size of the powder is 50-100 meshes.
In step 2) of the method, PEG-100000 is added in a proportion of 1-1.5% (specifically, 1.25%) by mass of the solution 2;
in the step 3), the insoluble thermoplastic resin powder is at least one of nylon, polyether-ether-ketone, polypropylene and polylactic acid;
the particle size of the indissolvable thermoplastic resin powder is 300-500 meshes;
the mass ratio of the insoluble thermoplastic resin powder to the soluble resin in the step 1) can be 30-50:1-3;
the stirring is realized by mechanical arms, the mechanical arms are opposite in groups, the front ends of the mechanical arms are claws, the width of the middle front end is consistent with that of the claws, and the mechanical arms stir back and forth;
the time of the stirring and the ultrasonic oscillation can be 10-20min;
in step 4), the carbon fiber may be at least one of PAN-based carbon fiber, pitch-based carbon fiber, rayon carbon fiber, and recycled carbon fiber;
the length of the carbon fiber is 30-80mm;
the mass ratio of the carbon fibers to the hardly soluble thermoplastic resin in the step 3) may be 4-6:4-6;
the stirring is realized by mechanical arms, the mechanical arms are opposite in groups, the front ends of the mechanical arms are claws, the width of the middle front end is consistent with that of the claws, and the mechanical arms stir back and forth;
the time of the stirring and the ultrasonic oscillation can be 10-20min;
in the step 5) of the method, the carbon fiber suspension is dried by adopting a suction filtration or a hot dry method to obtain a carbon fiber felt, and then the carbon fiber felt is molded to form the carbon fiber reinforced composite material;
specifically, drying the carbon fiber suspension by a hot dry method, needling the dried carbon fiber mixture to obtain a carbon fiber felt, and performing mould pressing to obtain a carbon fiber composite material; wherein the drying temperature is 150-200 ℃ and the drying time is 0.5-1h; the die pressing adopts hot pressing, and the hot pressing condition is that the hot pressing temperature is 200-400 ℃; the hot pressing time is 0.5-10min, preferably 5min.
The carbon fiber reinforced composite material prepared by the method also belongs to the protection scope of the invention.
The suspension liquid powder impregnation method is suitable for uniform mixing of various fibers, integrates the advantages of a liquid phase impregnation method and a powder impregnation method, is suitable for large-scale production, is convenient to operate in a production process, simple in process and small in equipment investment, facilitates improvement of production efficiency, and performs flexible production.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1 preparation of a carbon fiber-reinforced composite Material
Dissolving polyetherimide resin powder (200 meshes) into a mixed solvent of N, N-dimethylacetamide and acetone in a ratio of 3:7 to obtain a solution 1; wherein the polyetherimide resin accounts for 5 percent of the mixed solvent by mass;
adding ethanol into the obtained solution 1 according to the mass ratio of 1:2 to prepare a solution 2;
adding PEG-100000 with the mass of 1.25% of the solution 2 into the obtained solution 2, and increasing the density of the solution 2;
adding insoluble nylon 6 resin powder (400 meshes) (the mass ratio of the nylon 6 resin to the polyetherimide resin is 30: 1) into the solution 2, and stirring and ultrasonically oscillating for 10min by a mechanical arm to obtain resin powder suspension;
adding short carbon fibers (with the length of 50 mm) into the resin powder suspension to obtain a carbon fiber suspension (the mass ratio of the short carbon fibers to the nylon 6 resin is 5:5); stirring by a mechanical arm and vibrating for 10min with the assistance of an ultrasonic device to obtain a uniformly mixed carbon fiber suspension;
heating the carbon fiber suspension at high temperature of 150 ℃ for 1h by a hot dry method to obtain a dried carbon fiber felt; compression molding the dried carbon fiber felt at the hot pressing temperature of 300 ℃; and (5) carrying out hot pressing for 5min to obtain the carbon fiber reinforced composite material.
Example 2 preparation of a carbon fiber-reinforced composite Material
Dissolving polyvinyl chloride resin powder (80 meshes) into a mixed solvent of N, N dimethylformamide and acetone in a mass ratio of 2:8 to obtain a solution 1; the mass fraction of the polyvinyl chloride resin powder and the mixed solvent is 5 percent;
adding ethanol into the obtained solution 1 according to the mass ratio of 1:3 to prepare a solution 2;
adding PEG-100000 with the mass content of 1.25% into the obtained solution 2, and increasing the density of the suspension;
adding insoluble polypropylene resin powder into the solution 2, stirring by a mechanical arm and carrying out ultrasonic oscillation for 10min, wherein the mass ratio of the polypropylene resin to the polyvinyl chloride resin is 50: 1) Obtaining a resin powder suspension;
adding short carbon fibers (the length is 40 mm) into the resin powder suspension to obtain a carbon fiber suspension (the ratio of the carbon fibers to the polypropylene resin is 4:6); stirring by a mechanical arm and vibrating for 10min with the assistance of an ultrasonic device to obtain a uniformly mixed carbon fiber suspension;
heating the carbon fiber suspension at high temperature of 150 ℃ for 1h by a hot dry method to obtain a dried carbon fiber felt; compression molding the dried carbon fiber felt at the hot pressing temperature of 350 ℃; and (5) carrying out hot pressing for 5min to obtain the carbon fiber reinforced composite material.
Example 3 preparation of a carbon fiber-reinforced composite Material
Dissolving polyetherimide resin powder (100 meshes) into a mixed solvent of N, N-dimethylacetamide and acetone in a mass ratio of 3:7 to obtain a solution 1; the mass fraction of the polyetherimide resin and the mixed solvent is 6 percent;
adding ethanol into the obtained solution 1 according to the mass ratio of 1:3 to prepare a solution 2;
adding PEG-100000 with the mass content of 1.25% into the obtained solution 2 to increase the density of the suspension;
adding insoluble polylactic resin powder into the solution 2, and stirring and ultrasonically oscillating for 10min by a mechanical arm to obtain a resin powder suspension;
adding short carbon fiber (the length is 30 mm) into the resin powder suspension to obtain carbon fiber suspension (the mass ratio of the short carbon fiber to the polylactic acid resin is 5:5); stirring by a mechanical arm and vibrating for 10min with the assistance of an ultrasonic device to obtain a uniformly mixed carbon fiber suspension;
heating the carbon fiber suspension at high temperature for 1h at 150 ℃ by a hot dry method to obtain a dried carbon fiber felt; compression molding the dried carbon fiber felt at the hot pressing temperature of 300 ℃; and (5) carrying out hot pressing for 5min to obtain the carbon fiber reinforced composite material.
The invention combines solution impregnation and powder impregnation by taking suspension as a medium, the suspension with certain density can disperse carbon fibers uniformly to ensure that the carbon fibers are fully impregnated with resin powder to obtain a composite material with excellent performance, and the carbon fibers and the resin are uniformly impregnated as shown by the excellent impact performance of the carbon fiber composite material in the table 1.
TABLE 1 data of performance tests on carbon fiber reinforced resin composites prepared in examples 1-3
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. A method of making a carbon fiber reinforced composite, the method comprising the steps of:
1) Dissolving soluble resin into a mixed solvent to obtain a solution 1, and adding ethanol into the obtained solution 1 to prepare a solution 2;
2) Adding PEG-100000 into the obtained solution 2 to increase the density of the solution 2;
3) Adding insoluble thermoplastic resin powder into the solution 2, and stirring and ultrasonically oscillating to obtain a resin powder suspension;
4) Adding short carbon fibers into the obtained resin powder suspension, and stirring and ultrasonically oscillating to obtain a carbon fiber suspension;
5) And taking out the carbon fiber suspension, filtering and drying to prepare a carbon fiber felt, and carrying out compression molding to obtain the carbon fiber reinforced composite material.
2. The method according to claim 1, wherein in the step 1), the mixed solvent is prepared by mixing an organic compound and acetone, wherein the mass ratio of the organic compound to the acetone is 1-3:7-9;
the organic compound is at least one of polyacrylic acid, N-dimethylacetamide and N, N-dimethylformamide;
the easily soluble resin is at least one of polymethyl methacrylate, polyvinyl chloride and polyetherimide;
the mass fraction of the easily soluble resin in the mixed solvent is 2-8%.
3. The method of claim 1 or 2, wherein the mass ratio of solution 1 to ethanol is 1:1-3;
the soluble resin is added in the form of powder, and the particle size of the powder is 50-100 meshes.
4. The method of claim 1, wherein in step 2), PEG-100000 is added in a proportion of 1-1.5% by mass of solution 2.
5. The method according to claim 1, wherein in the step 3), the poorly soluble thermoplastic resin powder is at least one of nylon, polyetheretherketone, polypropylene, and polylactic acid;
the particle size of the resin powder is 300-500 meshes;
the mass ratio of the insoluble thermoplastic resin powder to the soluble resin in the step 1) is 30-50:1-3.
6. The method of claim 1, wherein in step 4) of the method, the carbon fibers are at least one of PAN-based carbon fibers, pitch-based carbon fibers, rayon carbon fibers, and recycled carbon fibers;
the length of the carbon fiber is 30-80mm;
the mass ratio of the carbon fibers to the hardly soluble thermoplastic resin in the step 3) is in the range of 4-6:4-6;
the time of stirring and ultrasonic oscillation is 10-20min.
7. The method as claimed in claim 1, wherein in the step 5), the carbon fiber suspension is taken out, filtered, dried to prepare a carbon fiber felt, and then compression molding is carried out to obtain the carbon fiber reinforced composite material, wherein the drying temperature is 150-200 ℃ and the time is 0.5-1h; the die pressing adopts hot pressing, and the hot pressing condition is that the hot pressing temperature is 200-400 ℃; the hot pressing time is 0.5-10min, preferably 5min.
8. A carbon fiber reinforced composite material produced by the method of claim 1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310152779.8A CN115850741A (en) | 2023-02-23 | 2023-02-23 | Carbon fiber reinforced composite material and preparation method thereof |
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| CN202310152779.8A CN115850741A (en) | 2023-02-23 | 2023-02-23 | Carbon fiber reinforced composite material and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417600A (en) * | 2011-10-08 | 2012-04-18 | 中国科学院山西煤炭化学研究所 | Method for preparing continuous carbon fiber-reinforced thermoplastic resin composite material |
| CN104723577A (en) * | 2015-03-15 | 2015-06-24 | 吉林大学 | Preparation method for carbon fibre fabric-reinforced polyetheretherketone polymer composite material |
| CN105885072A (en) * | 2016-06-13 | 2016-08-24 | 吉林大学 | One-way continuous fiber-reinforced resin-based composite prepreg and preparation method thereof |
| US20190194404A1 (en) * | 2013-03-11 | 2019-06-27 | Aonix Advanced Materials Corp. | Compositions and methods for making thermoplastic composite materials |
| CN115648739A (en) * | 2022-11-08 | 2023-01-31 | 吉林大学 | Method for preparing carbon fiber reinforced thermoplastic resin-based felt material and composite material by suspension blending method |
-
2023
- 2023-02-23 CN CN202310152779.8A patent/CN115850741A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417600A (en) * | 2011-10-08 | 2012-04-18 | 中国科学院山西煤炭化学研究所 | Method for preparing continuous carbon fiber-reinforced thermoplastic resin composite material |
| US20190194404A1 (en) * | 2013-03-11 | 2019-06-27 | Aonix Advanced Materials Corp. | Compositions and methods for making thermoplastic composite materials |
| CN104723577A (en) * | 2015-03-15 | 2015-06-24 | 吉林大学 | Preparation method for carbon fibre fabric-reinforced polyetheretherketone polymer composite material |
| CN105885072A (en) * | 2016-06-13 | 2016-08-24 | 吉林大学 | One-way continuous fiber-reinforced resin-based composite prepreg and preparation method thereof |
| CN115648739A (en) * | 2022-11-08 | 2023-01-31 | 吉林大学 | Method for preparing carbon fiber reinforced thermoplastic resin-based felt material and composite material by suspension blending method |
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Application publication date: 20230328 |