CN109867916B - Plant fiber reinforced resin matrix composite material and preparation method thereof - Google Patents
Plant fiber reinforced resin matrix composite material and preparation method thereof Download PDFInfo
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- 229920005989 resin Polymers 0.000 title claims abstract description 33
- 239000011347 resin Substances 0.000 title claims abstract description 33
- 239000011159 matrix material Substances 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 43
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 43
- 239000013078 crystal Substances 0.000 claims abstract description 35
- 229920002678 cellulose Polymers 0.000 claims abstract description 20
- 239000001913 cellulose Substances 0.000 claims abstract description 20
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000004744 fabric Substances 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 15
- 239000000725 suspension Substances 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000009461 vacuum packaging Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000805 composite resin Substances 0.000 claims description 2
- 230000002787 reinforcement Effects 0.000 abstract description 8
- 238000013459 approach Methods 0.000 abstract description 2
- 239000011208 reinforced composite material Substances 0.000 abstract description 2
- 241000196324 Embryophyta Species 0.000 description 42
- 240000008564 Boehmeria nivea Species 0.000 description 19
- 238000005452 bending Methods 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 244000198134 Agave sisalana Species 0.000 description 3
- 240000000491 Corchorus aestuans Species 0.000 description 3
- 235000011777 Corchorus aestuans Nutrition 0.000 description 3
- 235000010862 Corchorus capsularis Nutrition 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000003733 fiber-reinforced composite Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 2
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- 238000009755 vacuum infusion Methods 0.000 description 2
- 235000011624 Agave sisalana Nutrition 0.000 description 1
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- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- 240000000797 Hibiscus cannabinus Species 0.000 description 1
- 240000006240 Linum usitatissimum Species 0.000 description 1
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
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- 229920000728 polyester Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 230000008023 solidification Effects 0.000 description 1
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- 239000012209 synthetic fiber Substances 0.000 description 1
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Abstract
The invention relates to a plant fiber reinforced resin matrix composite material, which is characterized by consisting of a reinforcement and a resin matrix, wherein: the reinforcement body comprises nano cellulose crystals, carbon nano tubes and continuous plant fibers, wherein the nano cellulose crystals and the carbon nano tubes are attached to the surfaces of the continuous plant fibers. The composite material reinforcement is a complex of cellulose crystals, carbon nanotubes and continuous plant fibers, has two scales of nanometer and decimeter, and the prepared composite material is a double-scale reinforced composite material. The method provides a technical approach for high performance of the continuous plant fiber reinforced resin matrix composite.
Description
Technical Field
The invention relates to a double-scale plant fiber reinforced composite material and a preparation method thereof, belonging to the technical field of high performance of plant fiber reinforced resin matrix composite materials.
Background
The compounding is an important direction for the development of new materials, and polymer matrix composite materials taking fibers as reinforcements are an important branch of composite materials. Among many reinforcing fibers, plant fibers are valued for their properties of being degradable, renewable, high specific strength, low cost, and easy to process. However, compared to synthetic fibers represented by carbon fibers, glass fibers, etc., the hydrophilic structure of the surface of the plant fiber and the hydrophobic polymer matrix are difficult to form a high-quality interface, and stress cannot be effectively transmitted between the reinforcing fiber and the matrix, so that the mechanical properties of the composite material are poor. The shortage of mechanical properties directly results in the limitation of the application field of the plant fiber reinforced polymer matrix composite material. Therefore, the method obviously improves the loaded service performance of the plant fiber composite material by strengthening the interface bonding performance between the matrix and the fiber, and is an important research direction for high-performance modification of the plant fiber reinforced composite material
It is a new technology developed in recent years to attach carbon nanotubes to the surface of plant fibers to obtain surface-modified plant fibers, and to use the plant fibers with the carbon nanotubes attached to the surface as a reinforcement. In order to attach the carbon nanotubes to the surface of the plant fiber, a suspension in which the carbon nanotubes are uniformly dispersed is first prepared. In published literature, one has dispersed carboxylated carbon nanotubes in an aqueous solvent to obtain a suspension of carbon nanotubes, and mixed the suspension with an aqueous solution of short jute fibers, and strongly stirred to attach the carbon nanotubes to the surface of the jute fibers. This method requires chemical modification of carbon nanotubes and requires strong stirring to disperse the carbon nanotubes in an aqueous solvent, and the resulting carbon nanotube suspension has poor stability.
Disclosure of Invention
The invention provides a plant fiber reinforced resin matrix composite material and a preparation method thereof, aims to solve the problem that carbon nanotubes are uniformly attached to the surface of plant fibers, provides a high-performance plant fiber reinforced resin matrix composite material, and provides a green, simple and feasible preparation method.
The technical scheme of the invention is as follows: the plant fiber reinforced resin matrix composite material is composed of a reinforcement and a resin matrix, wherein: the reinforcement body comprises a nano cellulose crystal, a carbon nano tube and continuous plant fibers, wherein the nano cellulose crystal and the carbon nano tube are attached to the surfaces of the continuous plant fibers. The reinforcement has two scales of nanometer and decimeter, and the prepared composite material is a dual-scale reinforced composite material.
Specifically, the composite material comprises, by weight, 40-55 parts of continuous plant fibers, 0.1-0.5 part of nano-crystalline cellulose, 0.1-2 parts of carbon nanotubes, 30-45 parts of resin and 1.0-30 parts of curing agents.
The continuous plant fiber comprises any one of, but not limited to, ramie, sisal, flax, kenaf, jute and bamboo fiber, or a combination of several of the foregoing.
The resin base adopts thermosetting resin or thermoplastic resin, and the thermosetting resin comprises any one of epoxy resin and vinyl resin; the thermoplastic resin includes, but is not limited to, any one of thermoplastic polyester and polyurethane.
The specific process steps of the invention are as follows:
(1) Adding the hydroxylated or carboxylated modified carbon nano tubes into the nano-cellulose crystal aqueous solution, and then dispersing and mixing to obtain a nano-cellulose crystal and carbon nano tube mixed suspension liquid with uniformly dispersed carbon nano tubes;
(2) Cutting the continuous plant fiber fabric into a proper size, soaking the continuous plant fiber fabric in a sodium hydroxide solution with the mass fraction of 4% for 2 hours, taking out the continuous plant fiber fabric, washing the soaked continuous plant fiber fabric with deionized water until the washing liquid is neutral, and drying the washed continuous plant fiber fabric for later use;
(3) Uniformly spraying the mixed suspension of the nano cellulose crystals and the carbon nano tubes uniformly mixed in the step (1) on the surface of the continuous plant fiber dried in the step (2), and then drying for later use;
(4) Layering the continuous plant fiber fabric attached with the nano cellulose crystals and the carbon nano tubes obtained in the step (3) in sequence to obtain a plant fiber prefabricated body, and carrying out vacuum packaging;
(5) Pouring the resin matrix into the plant fiber prefabricated body in the step (4) through a vacuum pouring process to fully dip the resin matrix and the plant fiber;
(6) And (5) putting the vacuum-sealed plant fiber preform impregnated with the resin base obtained in the step (5) into a curing furnace or curing the plant fiber preform at room temperature.
Preferably, in the step (3), the concentration of the nano-cellulose crystal and the carbon nano-tube suspension is 0.15wt% -2.5 wt%, and the spraying times are 2-10. By controlling the concentration and spraying times of the nano-cellulose crystal and the carbon nano-tube suspension, the mass fraction of the nano-cellulose crystal is ensured to be 0.1-0.5%, and the mass fraction of the carbon nano-tube is ensured to be 0.1-2%.
The specific curing temperature and time in step (6) are determined by the curing characteristics of the resin matrix used.
Compared with the prior plant fiber reinforced resin matrix composite material, the invention has the following characteristics and advantages:
1) The nano-cellulose crystal aqueous solution is used as the carbon nano-tube dispersing agent, so that the nano-cellulose nano-tube dispersing agent has the advantages of greenness and no pollution;
2) The nano-cellulose crystal is a reinforcing material with very high mechanical property, and the nano-cellulose crystal and the carbon nano-tube can play a role in reinforcing together by the method;
3) The nano-cellulose crystal and the plant fiber have good adhesiveness, and the carbon nano-tube in the invention is firstly adhered to the surface of the nano-cellulose crystal and then adhered to the surface of the plant fiber through the nano-cellulose crystal, so that the adhesiveness is strong and the reinforcing effect is good.
In conclusion, the novel method for preparing the high-performance plant fiber composite material discovered in the experimental process provides a green, simple and feasible technical approach for preparing the high-performance plant fiber reinforced composite material, and has a positive effect on expanding the application field of the plant fiber composite material.
Detailed Description
For better understanding of the present invention, the following examples are provided to further illustrate the present invention, but the present invention is not limited to the following examples.
Example 1: the material composition ratios (mass parts ratios) of the examples are shown in table 1.
Table 1 the material of this example comprises the following components (mass ratio):
| plain ramie fiber fabric | Epoxy resin base | Curing agent | Nano cellulose crystal | Hydroxylated carbon nanotubes |
| 45 | 50 | 4 | 0.1 | 0.9 |
The preparation steps are as follows:
(1) Adding a certain amount of hydroxylated carbon nano tubes into the nano-cellulose crystal aqueous solution, and then dispersing and mixing to obtain a uniformly dispersed nano-cellulose crystal and carbon nano-tube mixed suspension with the mass fraction of the carbon nano-tubes of about 1%.
(2) Cutting a 0.2mm thick plain ramie fiber fabric into pieces with the size of 10cm wide by 5cm, cutting the pieces into 7 pieces, soaking the pieces in a sodium hydroxide solution with the mass fraction of 4% for 2 hours, taking out the pieces, washing the soaked continuous ramie fiber fabric with deionized water until the washing liquid is neutral, and drying the washed continuous ramie fiber fabric for later use.
(3) And (3) uniformly spraying the mixed suspension of the nano cellulose crystals and the carbon nano tubes uniformly mixed in the step (1) on the surface of the continuous ramie fiber fabric dried in the step (2), uniformly spraying the front and the back of the continuous ramie fiber fabric for three times, and drying the continuous ramie fiber fabric for later use.
(4) And (4) sequentially layering the continuous ramie fiber fabric attached with the nano cellulose crystals and the carbon nano tubes obtained in the step (3) to obtain a plant fiber prefabricated body, carrying out vacuum packaging, and repeatedly vacuumizing and compacting for more than 20 times.
(5) And (4) pouring the resin matrix mixed with the curing agent into the ramie fiber preform in the step (4) through a vacuum infusion process, so that the resin matrix and the ramie fibers are fully impregnated.
(6) And (4) putting the vacuum-sealed resin-base-impregnated plant fiber preform obtained in the step (5) into a curing furnace for curing for 2 hours at the curing temperature of 120 ℃.
After the solidification is finished, the solidified part is placed in a room temperature environment under the action of vacuum pressure for cooling, is cooled to room temperature for demoulding, and is cut into standard bending and impact test sample strips for standby.
Through detection, the bending strength of the composite material reaches 185MPa, the bending modulus reaches 8.6GPa, and the impact strength of the unnotched simply supported beam is 20KJ/m 2 。
Example 2: the material composition ratios (mass parts ratios) of the examples are shown in table 2.
Table 2 the material composition ratio (mass ratio) of this example is:
| plain ramie fiber fabric | Vinyl resin base | Curing agent | Nano cellulose crystal | Hydroxylated carbon nanotubes |
| 45 | 40 | 13 | 0.2 | 1.8 |
The preparation steps are as follows:
(1) Adding a certain amount of hydroxylated carbon nano tubes into the nano-cellulose crystal aqueous solution, and then dispersing and mixing to obtain a uniformly dispersed nano-cellulose crystal and carbon nano-tube mixed suspension with the mass fraction of the carbon nano-tubes of about 1%.
(2) Cutting a 0.2mm thick plain ramie fiber fabric into pieces with the size of 10cm wide by 5cm, cutting the pieces into 7 pieces, soaking the pieces in a sodium hydroxide solution with the mass fraction of 4% for 2 hours, taking the pieces out, washing the soaked continuous ramie fiber fabric with deionized water until the washing liquid is neutral, and drying the washed continuous ramie fiber fabric for later use.
(3) And (3) uniformly spraying the nano cellulose crystal and carbon nano tube mixed suspension uniformly mixed in the step (1) on the surface of the continuous ramie fiber fabric dried in the step (2), uniformly spraying the front and back surfaces for six times, and then drying for later use.
(4) And (4) sequentially layering the continuous ramie fiber fabric attached with the nano cellulose crystals and the carbon nano tubes obtained in the step (3) to obtain a plant fiber prefabricated body, carrying out vacuum packaging, and repeatedly vacuumizing and compacting for more than 20 times.
(5) And (4) pouring the resin matrix mixed with the curing agent into the ramie fiber preform in the step (4) through a vacuum infusion process, so that the resin matrix and the ramie fibers are fully impregnated.
(6) And (5) curing the vacuum-sealed resin-base-impregnated plant fiber preform obtained in the step (5) for 6 hours at room temperature.
Demolding is carried out in a room temperature environment, and then cutting is carried out to obtain standard bending and impact test sample strips for standby.
Through detection, the bending strength of the composite material reaches 176MPa, the bending modulus reaches 7.3GPa, and the impact strength of the unnotched simply supported beam is 18KJ/m 2 。
Example 3: the material composition ratios (mass part ratios) of the examples are shown in table 3.
Table 3 the material of this example comprises the following components (mass ratio):
| unidirectional sisal fiber | Vinyl resin base | Curing agent | Nano cellulose crystal | Hydroxylated carbon nanotubes |
| 45 | 50 | 4 | 0.1 | 0.9 |
The procedure of this example is the same as example 2
Through detection, the bending strength of the composite material reaches 296MPa, the bending modulus reaches 16.2GPa, and the impact strength of the unnotched simply supported beam is 37.5KJ/m 2 。
Example 4: the material composition ratios (mass parts ratios) of the examples are shown in table 4.
Table 4 the material of this example comprises the following components (mass ratio):
| unidirectional sisal hemp fiber | Epoxy resin base | Curing agent | Nano cellulose crystal | Hydroxylated carbon nanotubes |
| 45 | 40 | 13 | 02 | 1.8 |
The procedure of this example is the same as example 1.
Through detection, the bending strength of the composite material reaches 325MPa, the bending modulus reaches 17.3GPa, and the impact strength of the unnotched simply supported beam is 42.5KJ/m 2 。
All resins are not added with a base, and the resin per se is a complete term, but a resin-based composite material, simply "resin-based", is not true.
The laboratory only performed the hydroxylation modification experiment, but the carboxylation modification is theoretically possible. However, since the carbon nanotube which is not modified with the hydrophilic functional group is not always the case, the carbon nanotube which is modified with the hydroxylation or the carboxylation is herein referred to.
Claims (2)
1. The preparation method of the plant fiber reinforced resin matrix composite material is characterized by comprising the following steps: (1) Adopting a hydroxylated carbon nanotube or a hydroxylated modified carbon nanotube; adding carbon nano tubes into a nano-cellulose crystal aqueous solution, and then dispersing and mixing to obtain a nano-cellulose crystal and carbon nano tube mixed suspension liquid with uniformly dispersed carbon nano tubes; (2) Cutting the continuous plant fiber fabric into a proper size, soaking the continuous plant fiber fabric in a sodium hydroxide solution with the mass fraction of 4% for 2 hours, taking out the continuous plant fiber fabric, washing the soaked continuous plant fiber fabric with deionized water until the washing liquid is neutral, and drying the washed continuous plant fiber fabric for later use; (3) Uniformly spraying the mixed suspension of the nano cellulose crystals and the carbon nano tubes uniformly mixed in the step (1) on the surface of the continuous plant fiber dried in the step (2), and then drying for later use; (4) Layering the continuous plant fiber fabric attached with the nano cellulose crystals and the carbon nano tubes obtained in the step (3) in sequence to obtain a plant fiber prefabricated body, and carrying out vacuum packaging; (5) Pouring the resin matrix into the plant fiber prefabricated body in the step (4) through a vacuum pouring process to fully dip the resin matrix and the plant fiber; (6) And (5) putting the vacuum-sealed plant fiber preform impregnated with the resin base obtained in the step (5) into a curing furnace or curing the plant fiber preform at room temperature.
2. The method for preparing a plant fiber reinforced resin-based composite material according to claim 1, wherein in the step (3), the concentration of the nanocellulose crystal and the carbon nanotube suspension is 0.15wt% to 2.5wt%, and the number of spraying is 2 to 10.
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| CN110938304A (en) * | 2019-12-17 | 2020-03-31 | 湖南工程学院 | Hybrid fiber composite material and preparation method thereof |
| CN111154138B (en) * | 2020-01-19 | 2022-07-12 | 陕西科技大学 | Carbon black/cellulose composite photo-thermal material for seawater desalination and preparation method thereof |
| CN112980026A (en) * | 2021-03-09 | 2021-06-18 | 山东非金属材料研究所 | Preparation method of carbon nanotube modified fiber reinforced thermosetting resin-based prepreg |
| CN113248867B (en) * | 2021-04-22 | 2022-07-26 | 北京汽车研究总院有限公司 | Epoxy resin-based composite material and preparation method and application thereof |
| CN114603953B (en) * | 2022-02-11 | 2023-05-05 | 安徽农业大学 | Bamboo fiber woven filling material and preparation method thereof |
| CN114606772B (en) * | 2022-04-13 | 2024-01-26 | 国际竹藤中心 | Preparation method of interface-enhanced continuous plant fiber unit |
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|---|---|---|---|---|
| CN104088136A (en) * | 2014-07-03 | 2014-10-08 | 河海大学 | Preparation method of carbon nano-tube grafted glass fiber fabric reinforcement |
| CN104936895A (en) * | 2013-01-24 | 2015-09-23 | 日本瑞翁株式会社 | Carbon nanotube dispersion, method for manufacturing same, carbon nanotube composition, and method for manufacturing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104936895A (en) * | 2013-01-24 | 2015-09-23 | 日本瑞翁株式会社 | Carbon nanotube dispersion, method for manufacturing same, carbon nanotube composition, and method for manufacturing same |
| CN104088136A (en) * | 2014-07-03 | 2014-10-08 | 河海大学 | Preparation method of carbon nano-tube grafted glass fiber fabric reinforcement |
Non-Patent Citations (2)
| Title |
|---|
| Cellulose Microcrystal Improved Interphase of Ramie Fiber-Reinforced Epoxy Resin Composites;Kaomin Zhang et al;《Polymer Composites》;20181231;第39卷;第2207-2216页 * |
| 快速固化碳纳米管／苎麻纤维／环氧树脂复合材料层板的制备与性能;张靠民等;《材料导报Ｂ：研究篇》;20181231;第32卷(第12期);第4370-4373,4380页 * |
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