CN108623730A - A kind of fiber reinforcement Polydicyclopentadiencomposite composite material and preparation method - Google Patents
A kind of fiber reinforcement Polydicyclopentadiencomposite composite material and preparation method Download PDFInfo
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- CN108623730A CN108623730A CN201810434794.0A CN201810434794A CN108623730A CN 108623730 A CN108623730 A CN 108623730A CN 201810434794 A CN201810434794 A CN 201810434794A CN 108623730 A CN108623730 A CN 108623730A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F132/00—Homopolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system
- C08F132/08—Homopolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system having condensed rings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/06—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen
- C08F4/12—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen of boron, aluminium, gallium, indium, thallium or rare earths
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/06—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen
- C08F4/22—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen of chromium, molybdenum or tungsten
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- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- 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
- C08K9/02—Ingredients treated with inorganic substances
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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
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- 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
- C08J2345/00—Characterised by the use of homopolymers or copolymers of compounds having no unsaturated aliphatic radicals in side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic or in a heterocyclic ring system; Derivatives of such polymers
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Abstract
The present invention relates to a kind of fiber reinforcement Polydicyclopentadiencomposite composite materials, are formed by the raw material blending polymerization of following weight percent：93~99.99% dicyclopentadienes, 0.01~7% fiber, above-mentioned fiber is carbon fiber, a kind of fiber reinforcement Polydicyclopentadiencomposite composite material of the present invention, select carbon fiber as reinforcing material and dicyclopentadiene blending polymerization at composite material, and carbon fiber by nitric acid silane coupling agent after being handled early period, so that the groove of carbon fiber surface is deepened, surface becomes coarse, load can effectively be transmitted, give full play to the characteristic of carbon fiber, improve the mechanical property of composite material, tensile property, bending strength and impact strength are obtained for promotion, in addition preparation method of the invention is easy to operate, and aluminium oxide and aryloxy group tungsten catalyst are used as catalyst, so that the conjugation of both carbon fiber and dicyclopentadiene is more preferable.
Description
Technical field
The invention belongs to the technical field of Polydicyclopentadiencomposite composite material more particularly to the poly bis rings of a kind of fiber reinforcement penta
Diene composite material and preparation method.
Background technology
It wears in one's hair with the hair of modern science and technology, more and more meets material because of its high-performance, low cost causes people
Common concern, especially fibre reinforced composites are most widely used, dosage is maximum.The characteristics of this kind of material, is that density is small, compares
Intensity and specific modulus are big, alternative traditional material and applied in military, building and daily life.
Polydicyclopentadiene is a kind of novel Thermoset engineering plastics made of dicyclopentadiene ring-opening polymerisation, is had
The characteristics such as preferable shock strength, bending modulus, heat resistance, dimensional stability, corrosion resistance, creep resistance.But it also deposits simultaneously
In some shortcomings, for example the intensity of product is only capable of reaching the requirement of general performance, to being used for as Gran turismo, luxury car speedboat shell
These high performance requirements of material then seem insufficient.
People are mainly want using fibrous material as enhancing to be modified PDCPD materials, to improve the physics of PDCDP materials at present
Mechanical performance.If withdrawing deposit the excellent physical mechanical property of place's fiber reinforcement PDCDP composite materials, fiber has with PDCDP
Good compatibility is crucial；And fiber and this compatibilities of PDCDP can increase Van der Waals force by chemical bonding, improve fine
Wettability, roughening and the mechanical snap on surface in dimension table face come or.Therefore it needs to be modified fiber surface, make
Fiber interface and the interfaces PDCDP can brought close, to make the performance of product reach optimization.
Invention content
It is good that a kind of tensile property is provided the invention aims to overcome the deficiencies in the prior art, and impact strength and curved
The fiber reinforcement Polydicyclopentadiencomposite composite material and preparation method of Qu Qiangdu high.
In order to achieve the above objectives, the technical solution adopted by the present invention is：A kind of fiber reinforcement polydicyclopentadiene composite wood
Material, is formed by the raw material blending polymerization of following weight percent：93~99.99% dicyclopentadienes, 0.01~7% fiber,
Above-mentioned fiber is carbon fiber.
A kind of preparation method of fiber reinforcement Polydicyclopentadiencomposite composite material, in：Include the following steps：
One, carbon fiber is surface-treated first：
1. liquid phase oxidation：Clean carbon fiber is added in the round-bottomed flask for the hydrogen peroxide for being 35% equipped with mass fraction, into
Row magnetic agitation aoxidizes 3h at 110 DEG C, is cleaned with deionized water after filtering, then is put into concentrated nitric acid and handles 12h in 120 DEG C.Clearly
It is dried in vacuo at 100 DEG C after washing, for use；
2. coupling agent treatment：Clean carbon fiber is added to the silane coupling agent ethanol solution for being 15% equipped with mass fraction
In, it is 5-6 to adjust PH with hydrochloric acid, after handling 6h at 60-65 DEG C, is dried in vacuo for 24 hours, for use at 80 DEG C again after cleaning；
3. the carbon fiber of liquid phase oxidation is handled with coupling agent treatment again；After haveing broken up again 120 DEG C vacuum drying for 24 hours, for use；
Two, high-shear homogenizer by treated carbon fiber with 0.01~7% in 93~99.99% liquid dicyclopentadiene
Matter is disperseed, and dispersion liquid is obtained；
Three, under inert gas protection, aryloxy group tungsten catalyst and co-catalyst are added into dispersion liquid, is uniformly mixing to obtain mixed
Liquid is closed, then above-mentioned mixed liquor is injected in mold, is molded after 30min, obtains compound batten.
Preferably, the inert gas is nitrogen.
Preferably, the co-catalyst is aluminium oxide.
Due to the application of the above technical scheme, the present invention has following advantages compared with prior art：
A kind of fiber reinforcement Polydicyclopentadiencomposite composite material of the present invention program, select carbon fiber as reinforcing material with it is bicyclic
Pentadiene blending polymerization is at composite material, and carbon fiber is after early period is by nitric acid-silane coupling agent processing so that carbon fiber surface
The groove in face is deepened, and surface becomes coarse, can effectively transmit load, gives full play to the characteristic of carbon fiber, improves composite material
Mechanical property, tensile property, bending strength and impact strength be obtained for promotion, in addition preparation method of the invention operation letter
It is single, and use aluminium oxide and aryloxy group tungsten catalyst as catalyst so that the combination of both carbon fiber and dicyclopentadiene
Degree is more preferable.
Specific implementation mode
With reference to specific embodiment, the present invention is described in further detail.
A kind of fiber reinforcement Polydicyclopentadiencomposite composite material is formed by the raw material blending polymerization of following weight percent：
93~99.99% dicyclopentadienes, 0.01~7% fiber, above-mentioned fiber are carbon fiber.
Preparation method is as follows：
Embodiment one：
One, carbon fiber is surface-treated first：
1. liquid phase oxidation：Clean carbon fiber is added in the round-bottomed flask for the hydrogen peroxide for being 35% equipped with mass fraction, into
Row magnetic agitation aoxidizes 3h at 110 DEG C, is cleaned with deionized water after filtering, then is put into concentrated nitric acid and handles 12h in 120 DEG C.Clearly
It is dried in vacuo at 100 DEG C after washing, for use；
2. coupling agent treatment：Clean carbon fiber is added to the silane coupling agent ethanol solution for being 15% equipped with mass fraction
In, it is 5 to adjust PH with hydrochloric acid, after handling 6h at 60 DEG C, is dried in vacuo for 24 hours, for use at 80 DEG C again after cleaning；
3. the carbon fiber of liquid phase oxidation is handled with coupling agent treatment again；After haveing broken up again 120 DEG C vacuum drying for 24 hours, for use；
Two, high-shear homogenizer by treated carbon fiber with 0.01 in 99.99% liquid dicyclopentadiene homogenous disperse, obtain
To dispersion liquid；
Three, under nitrogen protection, aryloxy group tungsten catalyst and aluminium oxide are added into dispersion liquid, is uniformly mixing to obtain mixed liquor,
Then above-mentioned mixed liquor is injected in mold, is molded after 30min, obtains compound batten.
Embodiment two：
One, carbon fiber is surface-treated first：
1. liquid phase oxidation：Clean carbon fiber is added in the round-bottomed flask for the hydrogen peroxide for being 35% equipped with mass fraction, into
Row magnetic agitation aoxidizes 3h at 110 DEG C, is cleaned with deionized water after filtering, then is put into concentrated nitric acid and handles 12h in 120 DEG C.Clearly
It is dried in vacuo at 100 DEG C after washing, for use；
2. coupling agent treatment：Clean carbon fiber is added to the silane coupling agent ethanol solution for being 15% equipped with mass fraction
In, it is 6 to adjust PH with hydrochloric acid, after handling 6h at 65 DEG C, is dried in vacuo for 24 hours, for use at 80 DEG C again after cleaning；
3. the carbon fiber of liquid phase oxidation is handled with coupling agent treatment again；After haveing broken up again 120 DEG C vacuum drying for 24 hours, for use；
Two, high-shear homogenizer by treated carbon fiber with 7% in 93% liquid dicyclopentadiene homogenous disperse, divided
Dispersion liquid；
Three, under nitrogen protection, aryloxy group tungsten catalyst and aluminium oxide are added into dispersion liquid, is uniformly mixing to obtain mixed liquor,
Then above-mentioned mixed liquor is injected in mold, is molded after 30min, obtains compound batten.
The present invention a kind of fiber reinforcement Polydicyclopentadiencomposite composite material, select carbon fiber as reinforcing material with it is bicyclic
Pentadiene blending polymerization is at composite material, and carbon fiber is after early period is by nitric acid-silane coupling agent processing so that carbon fiber surface
The groove in face is deepened, and surface becomes coarse, can effectively transmit load, gives full play to the characteristic of carbon fiber, improves composite material
Mechanical property, tensile property, bending strength and impact strength be obtained for promotion, in addition preparation method of the invention operation letter
It is single, and use aluminium oxide and aryloxy group tungsten catalyst as catalyst so that the combination of both carbon fiber and dicyclopentadiene
Degree is more preferable.
The specific application example that the above is only the present invention, is not limited in any way protection scope of the present invention.All uses
Equivalent transformation or equivalent replacement and the technical solution formed, all fall within rights protection scope of the present invention.
Claims (4)
1. a kind of fiber reinforcement Polydicyclopentadiencomposite composite material, it is characterised in that：It is blended by the raw material of following weight percent
It is polymerized：93~99.99% dicyclopentadienes, 0.01~7% fiber, above-mentioned fiber are carbon fiber.
2. a kind of preparation method of fiber reinforcement Polydicyclopentadiencomposite composite material as described in claim 1, it is characterised in that：
Include the following steps：
One, carbon fiber is surface-treated first：
1. liquid phase oxidation：Clean carbon fiber is added in the round-bottomed flask for the hydrogen peroxide for being 35% equipped with mass fraction, into
Row magnetic agitation aoxidizes 3h at 110 DEG C, is cleaned with deionized water after filtering, then is put into concentrated nitric acid and handles 12h in 120 DEG C;Clearly
It is dried in vacuo at 100 DEG C after washing, for use；
2. coupling agent treatment：Clean carbon fiber is added to the silane coupling agent ethanol solution for being 15% equipped with mass fraction
In, it is 5-6 to adjust PH with hydrochloric acid, after handling 6h at 60-65 DEG C, is dried in vacuo for 24 hours, for use at 80 DEG C again after cleaning；
3. the carbon fiber of liquid phase oxidation is handled with coupling agent treatment again；After haveing broken up again 120 DEG C vacuum drying for 24 hours, for use；
Two, high-shear homogenizer by treated carbon fiber with 0.01~7% in 93~99.99% liquid dicyclopentadiene
Matter is disperseed, and dispersion liquid is obtained；
Three, under inert gas protection, aryloxy group tungsten catalyst and co-catalyst are added into dispersion liquid, is uniformly mixing to obtain mixed
Liquid is closed, then above-mentioned mixed liquor is injected in mold, is molded after 30min, obtains compound batten.
3. fiber reinforcement Polydicyclopentadiencomposite composite material preparation method according to claim 2, it is characterised in that：It is described
Inert gas is nitrogen.
4. fiber reinforcement Polydicyclopentadiencomposite composite material preparation method according to claim 2, it is characterised in that：It is described
Co-catalyst is aluminium oxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810434794.0A CN108623730A (en) | 2018-05-09 | 2018-05-09 | A kind of fiber reinforcement Polydicyclopentadiencomposite composite material and preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483744A (en) * | 2019-08-28 | 2019-11-22 | 山东腾创新材料科技有限公司 | A kind of Polydicyclopentadiencomposite composite material and its reaction and injection molding process |
| TWI736208B (en) * | 2020-04-01 | 2021-08-11 | 國家中山科學研究院 | Preparation method of high-performance carbon fiber composite material derived from dicyclopentadiene |
| CN115895160A (en) * | 2022-12-28 | 2023-04-04 | 东实汽车科技集团股份有限公司 | Polyester fiber reinforced polydicyclopentadiene composite material and preparation method thereof |
-
2018
- 2018-05-09 CN CN201810434794.0A patent/CN108623730A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483744A (en) * | 2019-08-28 | 2019-11-22 | 山东腾创新材料科技有限公司 | A kind of Polydicyclopentadiencomposite composite material and its reaction and injection molding process |
| TWI736208B (en) * | 2020-04-01 | 2021-08-11 | 國家中山科學研究院 | Preparation method of high-performance carbon fiber composite material derived from dicyclopentadiene |
| CN115895160A (en) * | 2022-12-28 | 2023-04-04 | 东实汽车科技集团股份有限公司 | Polyester fiber reinforced polydicyclopentadiene composite material and preparation method thereof |
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