CN110606914B - Sizing agent for PDCPD carbon fiber fabric composite material and preparation method thereof - Google Patents
Sizing agent for PDCPD carbon fiber fabric composite material and preparation method thereof Download PDFInfo
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- CN110606914B CN110606914B CN201910929474.7A CN201910929474A CN110606914B CN 110606914 B CN110606914 B CN 110606914B CN 201910929474 A CN201910929474 A CN 201910929474A CN 110606914 B CN110606914 B CN 110606914B
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 50
- 239000004744 fabric Substances 0.000 title claims abstract description 36
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 35
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 35
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000004513 sizing Methods 0.000 title claims abstract description 31
- 229920001153 Polydicyclopentadiene Polymers 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000003999 initiator Substances 0.000 claims abstract description 19
- 239000000178 monomer Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- DHGUSWLGCLGWEG-UHFFFAOYSA-N 1-[2-(cyclopenten-1-yloxy)ethoxy]cyclopentene prop-2-enoic acid Chemical compound OC(=O)C=C.C=1CCCC=1OCCOC1=CCCC1 DHGUSWLGCLGWEG-UHFFFAOYSA-N 0.000 claims abstract description 11
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000835 fiber Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 23
- 238000001723 curing Methods 0.000 claims description 15
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 6
- QHPQWRBYOIRBIT-UHFFFAOYSA-N 4-tert-butylphenol Chemical compound CC(C)(C)C1=CC=C(O)C=C1 QHPQWRBYOIRBIT-UHFFFAOYSA-N 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 208000020584 Polyploidy Diseases 0.000 claims description 5
- 239000003963 antioxidant agent Substances 0.000 claims description 5
- 230000003078 antioxidant effect Effects 0.000 claims description 5
- PNPBGYBHLCEVMK-UHFFFAOYSA-N benzylidene(dichloro)ruthenium;tricyclohexylphosphanium Chemical compound Cl[Ru](Cl)=CC1=CC=CC=C1.C1CCCCC1[PH+](C1CCCCC1)C1CCCCC1.C1CCCCC1[PH+](C1CCCCC1)C1CCCCC1 PNPBGYBHLCEVMK-UHFFFAOYSA-N 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000011984 grubbs catalyst Substances 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000010419 fine particle Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000007142 ring opening reaction Methods 0.000 abstract description 5
- 238000007493 shaping process Methods 0.000 abstract description 5
- 238000010550 living polymerization reaction Methods 0.000 abstract description 4
- 238000000016 photochemical curing Methods 0.000 abstract description 4
- -1 cyclic olefin Chemical class 0.000 abstract description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 abstract description 2
- 230000037048 polymerization activity Effects 0.000 abstract description 2
- 238000009745 resin transfer moulding Methods 0.000 description 8
- 239000003292 glue Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000007152 ring opening metathesis polymerisation reaction Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 150000001925 cycloalkenes Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/40—Esters of unsaturated alcohols, e.g. allyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Moulding By Coating Moulds (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
A shaping agent for PDCPD carbon fiber fabric composite material and a preparation method thereof comprise the following raw material components in parts by weight: the dosage of the ethylene glycol dicyclopentenyl ether acrylic acid is 160-240 g; the dosage of butyl acrylate is 20-30 g; the amount of the initiator is 3mL-5 mL. The reactive powder sizing agent obtained by UV photocuring has moderate price and more convenient use, can meet the use requirement of a carbon fiber preform in the process, has a structure similar to that of a cyclic olefin with a DCPD monomer, has better compatibility and formability, has no obvious negative influence on the ring-opening living polymerization activity of the DCPD and the performance of a fiber composite material thereof, and has good formability and reaction compatibility.
Description
Technical Field
The invention relates to the field of organic synthesis, in particular to a setting agent for a PDCPD carbon fiber fabric composite material and a preparation method thereof.
Background
Polydicyclopentadiene (PDCPD) is an engineering plastic with good performance, has low monomer viscosity (about 0.3 Pa.s), high reaction speed and adjustable polymerization speed, and is also suitable for Resin Transfer Molding (RTM) to prepare high-performance fiber reinforced composite materials. However, the sizing agents reported for the RTM process are mainly epoxy resins and are not compatible with DCPD resins and interface adhesive force, pure DCPD has pungent smell and is not suitable for being used as the sizing agent of the PDCPD-RTM process, on the other hand, ROMP polymerization of DCPD is easily influenced by environment such as compounds containing polar functional groups like water oxygen, most commercial ordinary binders contain negative influence components, and a certain report is suitable for binder commodities of PDCPD, the price of the binder is high, and the market is obvious, so that the development of the sizing agent matched with the PDCPD-RTM process is very significant.
Disclosure of Invention
The invention aims to provide a setting agent for a PDCPD carbon fiber fabric composite material and a preparation method thereof, and the setting agent has the advantages of having a structure similar to that of a cycloolefin of a DCPD monomer, good compatibility and setting property, having no obvious negative influence on the ring-opening active polymerization activity of the DCPD and the performance of a fiber composite material thereof, and having good setting property and reaction compatibility.
In order to achieve the purpose, the invention provides the following technical scheme: a shaping agent for a PDCPD carbon fiber fabric composite material comprises the following raw material components in parts by weight:
the dosage of the ethylene glycol dicyclopentenyl ether acrylic acid is 160-240 g;
the dosage of butyl acrylate is 20-30 g;
the amount of the initiator is 3mL-5 mL.
Further, the feed comprises the following raw material components in parts by weight:
the dosage of the ethylene glycol dicyclopentenyl ether acrylic acid is 200 g;
the dosage of butyl acrylate is 25 g;
the amount of the initiator used was 4 mL.
Further, the initiator is a solution made of 2, 4, 6-trimethylbenzoyl-diphenylphosphine oxide.
The invention also provides a preparation method of the setting agent for the PDCPD carbon fiber fabric composite material, which comprises the following steps:
s1: 240g of ethylene glycol dicyclopentenyl ether acrylic acid and 30g of butyl acrylate are poured into a reaction kettle, a stirring rod is used for stirring at 25d/min, a dropper is used for adding 3mL of initiator, the stirring rod is used for stirring at the rotating speed of 25d/min when the initiator is dripped, the mixture is poured into a vessel after stirring for 5-10min, the vessel is placed into a vessel with the wavelength of 365nm and the illumination intensity of 120-2Reacting for 8min under ultraviolet light to obtain solid of the setting agent;
s2: pouring the solid of the sizing agent into an ultrafine grinder, rotating a grinding shaft of the ultrafine grinder at 800d/min, and grinding the sizing agent into powder to obtain powder with the diameter of 600 meshes;
s3: uniformly spreading the sizing agent powder obtained in the step S2 on plain woven carbon fiber fabric with the surface density of 400gsm, presetting by using a vacuum bag method, and baking for 20min at 130 ℃ to obtain a carbon fiber plate fabric preforming body containing the sizing agent with the mass fraction of 0-8%;
s4: and (4) preparing the preformed body obtained in the step S3 into the PDCPD carbon fiber fabric composite material by a vacuum bag method, wherein the DCPD is divided into AB components, and the mixing amount of the AB components is controlled, so that the ratio of the catalyst to the monomer is 0.01-0.02%, the curing temperature is 50-70 ℃, and the curing time is 10-30 min.
Further, in step S2, the ultrafine pulverizer winnowing the material particles with the final desired fineness by using a cyclone separator.
Further, in step S4, the composite fiber fabric of PDCPD is laid on the mold body by vacuum bag method, the vacuum absorption bag layer that is inserted into the outside of the mold body is laid on the mold, air in the vacuum absorption bag layer is evacuated by vacuum, and then glue injection, curing and molding are performed, and finally, the mold is released.
Further, in step S4, the a component of DCPD includes a polyploid-containing DCPD monomer, 1% by mass of antioxidant p-tert-butylphenol, 0.1-0.5% by mass of inhibitor triphenylphosphine, and the B component is a xylene solution of Grubbs catalyst.
Compared with the prior art, the invention has the beneficial effects that:
the reactive powder sizing agent obtained by UV photocuring has moderate price and more convenient use, can meet the use requirement of a carbon fiber preform in a PDCPD-RTM process, has a structure similar to that of a cyclic olefin with a DCPD monomer, has better compatibility and formability, has no obvious negative influence on the ring-opening living polymerization (ROMP) reaction activity of the DCPD and the performance of a fiber composite material thereof, and has good formability and reaction compatibility.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings, but the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a shaping agent for a PDCPD carbon fiber fabric composite material comprises the following raw material components in parts by weight:
the dosage of the ethylene glycol dicyclopentenyl ether acrylic acid is 160 g;
the dosage of butyl acrylate is 20 g;
the amount of the initiator used was 3 mL.
The initiator is a solution prepared from 2, 4, 6-trimethylbenzoyl-diphenylphosphine oxide.
The invention provides another technical scheme, and a preparation method of a setting agent for a PDCPD carbon fiber fabric composite material comprises the following steps:
the method comprises the following steps: 160g of ethylene glycol dicyclopentenyl ether acrylic acid and 20g of butyl acrylate are poured into a reaction kettle, a stirring rod is used for stirring at 20d/min, 3mL of initiator is added by a dropper, the stirring rod is stirred at the rotating speed of 25d/min when the initiator is dripped, the mixture is poured into a vessel after stirring for 6min, the vessel is placed into the reaction kettle, the wavelength of the vessel is 365nm, and the illumination intensity is 120mM/m2Reacting for 8min under ultraviolet light to obtain solid of the setting agent;
step two: pouring the solid of the sizing agent into an ultrafine grinder, winnowing out the material particles with the final needed fineness in the ultrafine grinder through a cyclone separator, rotating a grinding shaft of the ultrafine grinder at 800d/min, and grinding the sizing agent into powder to obtain the powder with the diameter of 600 meshes;
step three: uniformly spreading the sizing agent powder obtained in the step S2 on plain woven carbon fiber fabric with the surface density of 400gsm, presetting by using a vacuum bag method, and baking for 20min at 130 ℃ to obtain a carbon fiber plate fabric preforming body containing the sizing agent with the mass fraction of 0-8%;
step four: and (2) preparing the preformed body obtained in the step (S3) into a PDCPD carbon fiber fabric composite material by a vacuum bag method, paving the PDCPD composite material fiber fabric on a mould body by the vacuum bag method, coating a vacuum absorption bag layer sleeved on the outer side of the mould body on the mould, vacuumizing and sucking air in the vacuum absorption bag layer, injecting glue, curing and forming, and finally demoulding, wherein the DCPD is divided into an AB component, the mixing amount of the AB component is controlled, the A component of the DCPD comprises a polyploid DCPD monomer, antioxidant p-tert-butylphenol with the mass fraction of 1%, inhibitor triphenylphosphine with the mass fraction of 0.2%, and the B component is a xylene solution of a Grubbs catalyst, so that the ratio of the catalyst to the monomer is 0.02%, the curing temperature is 50 ℃, and the curing time is 10 min.
Example two:
a shaping agent for a PDCPD carbon fiber fabric composite material comprises the following raw material components in parts by weight:
the dosage of the ethylene glycol dicyclopentenyl ether acrylic acid is 200 g;
the dosage of butyl acrylate is 25 g;
the amount of the initiator used was 4 mL.
The invention provides another technical scheme, and a preparation method of a setting agent for a PDCPD carbon fiber fabric composite material comprises the following steps:
the method comprises the following steps: pouring 200g of ethylene glycol dicyclopentenyl ether acrylic acid and 25g of butyl acrylate into a reaction kettle, stirring with a stirring rod at 25d/min, adding 4mL of initiator with a dropper, stirring with the stirring rod at 25d/min while dropping the initiator, stirring for 7min, pouring the mixed solution into a vessel, placing the vessel into the vessel, wherein the wavelength of the mixed solution is 365nm, and the illumination intensity is 160mM/m2Reacting for 8min under ultraviolet light to obtain solid of the setting agent;
step two: pouring the solid of the sizing agent into an ultrafine grinder, winnowing out the material particles with the final needed fineness in the ultrafine grinder through a cyclone separator, rotating a grinding shaft of the ultrafine grinder at 800d/min, and grinding the sizing agent into powder to obtain the powder with the diameter of 600 meshes;
step three: uniformly spreading the sizing agent powder obtained in the step S2 on plain woven carbon fiber fabric with the surface density of 400gsm, presetting by using a vacuum bag method, and baking for 20min at 130 ℃ to obtain a carbon fiber plate fabric preforming body containing the sizing agent with the mass fraction of 0-8%;
step four: and (2) preparing the preformed body obtained in the step (S3) into a PDCPD carbon fiber fabric composite material by a vacuum bag method, paving the PDCPD composite material fiber fabric on a mould body by the vacuum bag method, coating a vacuum absorption bag layer sleeved on the outer side of the mould body on the mould, vacuumizing and sucking air in the vacuum absorption bag layer, injecting glue, curing and forming, and finally demoulding, wherein the DCPD is divided into an AB component, the mixing amount of the AB component is controlled, the A component of the DCPD comprises a polyploid DCPD monomer, antioxidant p-tert-butylphenol with the mass fraction of 1%, inhibitor triphenylphosphine with the mass fraction of 0.3%, and the B component is a xylene solution of a Grubbs catalyst, so that the ratio of the catalyst to the monomer is 0.01%, the curing temperature is 60 ℃, and the curing time is 20 min.
Example three:
a shaping agent for a PDCPD carbon fiber fabric composite material comprises the following raw material components in parts by weight:
the dosage of the ethylene glycol dicyclopentenyl ether acrylic acid is 240 g;
the dosage of butyl acrylate is 30 g;
the amount of the initiator used was 5 mL.
The invention provides another technical scheme, and a preparation method of a setting agent for a PDCPD carbon fiber fabric composite material comprises the following steps:
the method comprises the following steps: 240g of ethylene glycol dicyclopentenyl ether acrylic acid and 30g of butyl acrylate are poured into a reaction kettle, a stirring rod is used for stirring at 25d/min, 5mL of initiator is added by a dropper, the stirring rod is stirred at the rotating speed of 25d/min when the initiator is dripped, the mixture is poured into a vessel after stirring for 7min, the vessel is placed into the vessel, the wavelength of the vessel is 365nm, and the illumination intensity is 160mM/m2Reacting for 8min under ultraviolet light to obtain solid of the setting agent;
step two: pouring the solid of the sizing agent into an ultrafine grinder, winnowing out the material particles with the final needed fineness in the ultrafine grinder through a cyclone separator, rotating a grinding shaft of the ultrafine grinder at 800d/min, and grinding the sizing agent into powder to obtain the powder with the diameter of 600 meshes;
step three: uniformly spreading the sizing agent powder obtained in the step S2 on plain woven carbon fiber fabric with the surface density of 400gsm, presetting by using a vacuum bag method, and baking for 20min at 130 ℃ to obtain a carbon fiber plate fabric preforming body containing the sizing agent with the mass fraction of 0-8%;
step four: and (2) preparing the preformed body obtained in the step (S3) into a PDCPD carbon fiber fabric composite material by a vacuum bag method, paving the PDCPD composite material fiber fabric on a mould body by the vacuum bag method, coating a vacuum absorption bag layer sleeved on the outer side of the mould body on the mould, vacuumizing and sucking air in the vacuum absorption bag layer, injecting glue, curing and forming, and finally demoulding, wherein the DCPD is divided into an AB component, the mixing amount of the AB component is controlled, the A component of the DCPD comprises a polyploid DCPD monomer, antioxidant p-tert-butylphenol with the mass fraction of 1%, inhibitor triphenylphosphine with the mass fraction of 0.3%, and the B component is a xylene solution of a Grubbs catalyst, so that the ratio of the catalyst to the monomer is 0.01%, the curing temperature is 60 ℃, and the curing time is 20 min.
The different setting agents in the first, second and third examples and the PDCPD carbon fiber fabric composite material are tested, and the test results are shown in the table I
TABLE-PDCPD carbon fiber fabric composite material performance under different setting agent contents
The experiment proves that the DCPD-RTM reactive powder sizing agent can be used as a PDCPD-RTM reactive powder sizing agent, the reactive powder sizing agent obtained by UV photocuring is moderate in price and convenient to use, can meet the use requirement of a carbon fiber preform in a PDCPD-RTM process, has a similar cycloolefin structure with a DCPD monomer, is good in compatibility and formability, has no obvious negative influence on the ring-opening living polymerization (ROMP) reactivity of the DCPD and the performance of a fiber composite material thereof, and has good formability and reaction compatibility.
In conclusion, the reactive powder sizing agent obtained by UV photocuring is moderate in price and convenient to use, can meet the use requirement of a carbon fiber preform in a PDCPD-RTM process, has a similar cycloolefin structure with a DCPD monomer, is good in compatibility and formability, has no obvious negative influence on the ring-opening living polymerization (ROMP) reaction activity of the DCPD and the performance of a fiber composite material thereof, and has good formability and reaction compatibility.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (3)
1. A preparation method of a PDCPD carbon fiber fabric composite material is characterized by comprising the following steps:
s1: 240g of ethylene glycol dicyclopentenyl ether acrylic acid and 30g of butyl acrylate are poured into a reaction kettle, a stirring rod is used for stirring at 25r/min, a dropper is used for adding 3mL of initiator, the stirring rod is used for stirring at the rotating speed of 25r/min when the initiator is dripped, the mixture is poured into a vessel after stirring for 5-10min, the vessel is placed into a vessel with the wavelength of 365nm and the illumination intensity of 120-2Reacting for 8min under ultraviolet light to obtain solid of the setting agent;
s2: pouring the solid of the sizing agent into an ultrafine grinder, rotating a grinding shaft of the ultrafine grinder at 800r/min, and grinding the sizing agent into powder to obtain powder with the diameter of 600 meshes;
s3: uniformly spreading the sizing agent powder obtained in the step S2 on plain woven carbon fiber fabric with the surface density of 400gsm, presetting by using a vacuum bag method, and baking for 20min at 130 ℃ to obtain a carbon fiber plate fabric preforming body containing the sizing agent with the mass fraction of 8%;
s4: preparing the preformed body obtained in the step S3 into a PDCPD carbon fiber fabric composite material by a vacuum bag method, wherein the used DCPD is divided into A, B components, the mixing amount of A, B components is controlled, the ratio of the catalyst to the monomer is 0.01-0.02%, the curing temperature is 50-70 ℃, and the curing time is 10-30 min;
wherein, the A component of the DCPD comprises polyploid DCPD monomer, antioxidant p-tert-butylphenol with the mass fraction of 1 percent, inhibitor triphenylphosphine with the mass fraction of 0.1 to 0.5 percent, and the B component is xylene solution of Grubbs catalyst; the initiator used was a solution of 2, 4, 6-trimethylbenzoyl-diphenylphosphine oxide.
2. The method of claim 1, wherein in step S2, the ultrafine pulverizer winnowing the fine particles of the material with the final desired fineness by a cyclone.
3. The preparation method according to claim 1, wherein in step S4, the composite fiber fabric of PDCPD is laid on the mold body by vacuum bag method, the vacuum absorption bag layer sleeved outside the mold body is laid on the mold, air in the vacuum absorption bag layer is evacuated by vacuum, and then the injection, curing and molding are performed, and finally the mold is released.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910929474.7A CN110606914B (en) | 2019-09-28 | 2019-09-28 | Sizing agent for PDCPD carbon fiber fabric composite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910929474.7A CN110606914B (en) | 2019-09-28 | 2019-09-28 | Sizing agent for PDCPD carbon fiber fabric composite material and preparation method thereof |
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|---|---|
| CN110606914A CN110606914A (en) | 2019-12-24 |
| CN110606914B true CN110606914B (en) | 2021-05-18 |
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Denomination of invention: A Setting Agent and Preparation Method for PDCPD Carbon Fiber Fabric Composite Materials Effective date of registration: 20231127 Granted publication date: 20210518 Pledgee: Guangdong Qingxin Rural Commercial Bank Co.,Ltd. Taiping Branch Pledgor: GUANGDONG JUHANG INSTITUTE FOR ADVANCED MATERIALS Co.,Ltd. Registration number: Y2023980067643 |