CN110079258B - High-toughness high-temperature-resistant impact-resistant road material and preparation method thereof - Google Patents
High-toughness high-temperature-resistant impact-resistant road material and preparation method thereof Download PDFInfo
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- CN110079258B CN110079258B CN201910288252.1A CN201910288252A CN110079258B CN 110079258 B CN110079258 B CN 110079258B CN 201910288252 A CN201910288252 A CN 201910288252A CN 110079258 B CN110079258 B CN 110079258B
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- 239000000463 material Substances 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000835 fiber Substances 0.000 claims abstract description 186
- 239000003822 epoxy resin Substances 0.000 claims abstract description 88
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 88
- ICXAPFWGVRTEKV-UHFFFAOYSA-N 2-[4-(1,3-benzoxazol-2-yl)phenyl]-1,3-benzoxazole Chemical class C1=CC=C2OC(C3=CC=C(C=C3)C=3OC4=CC=CC=C4N=3)=NC2=C1 ICXAPFWGVRTEKV-UHFFFAOYSA-N 0.000 claims abstract description 74
- -1 acrylic ester Chemical class 0.000 claims abstract description 64
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 46
- 229920000927 poly(p-phenylene benzobisoxazole) Polymers 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 40
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 238000005266 casting Methods 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000003892 spreading Methods 0.000 claims abstract description 10
- LYLHVKVAISPJHX-UHFFFAOYSA-N CO.C(CN)N Chemical compound CO.C(CN)N LYLHVKVAISPJHX-UHFFFAOYSA-N 0.000 claims abstract description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007259 addition reaction Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000012153 distilled water Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000011541 reaction mixture Substances 0.000 claims description 4
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical group CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 30
- 230000000694 effects Effects 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 4
- 229920000137 polyphosphoric acid Polymers 0.000 description 4
- 239000010426 asphalt Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- DNONRONPDMTKGS-UHFFFAOYSA-N 1,1,2-trimethylsilinane Chemical compound C[Si]1(C(CCCC1)C)C DNONRONPDMTKGS-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- DPYROBMRMXHROQ-UHFFFAOYSA-N 4,6-diaminobenzene-1,3-diol Chemical compound NC1=CC(N)=C(O)C=C1O DPYROBMRMXHROQ-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 230000029936 alkylation Effects 0.000 description 2
- 238000005804 alkylation reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 229940098779 methanesulfonic acid Drugs 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- DCERHCFNWRGHLK-UHFFFAOYSA-N C[Si](C)C Chemical compound C[Si](C)C DCERHCFNWRGHLK-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 125000006615 aromatic heterocyclic group Chemical group 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000032798 delamination Effects 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
- 229920000587 hyperbranched polymer Polymers 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052990 silicon hydride Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical group Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- 229940094989 trimethylsilane Drugs 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
- D06M13/2246—Esters of unsaturated carboxylic acids
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- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/325—Amines
- D06M13/332—Di- or polyamines
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- 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
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- 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
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- Chemical & Material Sciences (AREA)
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- Epoxy Resins (AREA)
Abstract
The invention provides a high-toughness high-temperature-resistant impact-resistant road material and a preparation method thereof, wherein the method comprises the following steps: soaking pretreated poly (p-phenylene benzobisoxazole) fibers in an ethylenediamine methanol solution to obtain ammoniated poly (p-phenylene benzobisoxazole) fibers; step two, mixing the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one with acrylic ester for addition reaction to obtain acrylic ester-poly-p-phenylene benzobisoxazole fiber; step three, grafting the acrylate-poly (p-phenylene benzobisoxazole) fiber prepared in the step two with hyperbranched polysiloxane to prepare modified poly (p-phenylene benzobisoxazole) fiber; and step four, uniformly spreading and flatly spreading the modified poly-p-phenylene benzobisoxazole fibers prepared in the step three to form fibers, adding a curing agent into epoxy resin to prepare a casting material, uniformly casting the casting material on a flatly laid fiber framework, and curing to prepare the high-toughness high-temperature-resistant impact-resistant road material.
Description
Technical Field
The invention belongs to the field of road materials, relates to a road material, and particularly relates to a high-toughness high-temperature-resistant impact-resistant road material and a preparation method thereof.
Background
The interlayer bonding effect of the asphalt road influences the service performance of the road surface, and the insufficient interlayer bonding can cause the problems of slippage, delamination, fatigue crack and the like of the asphalt road surface. The same problem exists for bridge deck pavements. As the weakest system in the bridge deck pavement structure, the quality of a waterproof bonding layer (namely between bridge deck layers) is related to the service quality of bridge deck pavement, and even the service life and service performance of the whole bridge are influenced. In the long-term research and application process at home and abroad, the epoxy resin is found to have obvious advantages in the aspect of bonding between bridge deck pavement layers and has obvious effects of consolidating loose aggregates and improving waterproofness. However, most epoxy resins are room temperature curable materials, and have high crosslinking density after curing, and cured products thereof have the disadvantages of low toughness, poor impact resistance and the like. In the face of increasing heavy traffic road requirements, the insufficient flexibility and impact resistance of the epoxy resin influences the road performance of the bridge deck pavement layer to a certain extent, and further reduces the road driving service level. Therefore, the toughness and strength of the epoxy resin are required to be enhanced so as to have more excellent performance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a high-toughness high-temperature-resistant impact-resistant road material and a preparation method thereof, which solve the problems of low toughness and poor high-temperature resistance after epoxy resin is cured.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a high-toughness high-temperature-resistant impact-resistant road material comprises the following steps:
step one, preparing ammoniated poly-p-phenylene benzobisoxazole fibers:
soaking the pretreated poly-p-phenylene benzobisoxazole fiber in an ethylenediamine methanol solution to obtain an ammoniated poly-p-phenylene benzobisoxazole fiber;
step two, preparing acrylate-poly (p-Phenylene Benzobisoxazole) (PBO) fibers:
mixing the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one with acrylic ester for addition reaction to obtain acrylic ester-poly-p-phenylene benzobisoxazole fiber;
step three, preparing modified poly-p-phenylene benzobisoxazole fiber:
grafting the acrylate-poly (p-phenylene benzobisoxazole) fiber prepared in the step two with hyperbranched polysiloxane to prepare modified poly (p-phenylene benzobisoxazole) fiber;
the molecular formula of the hyperbranched polysiloxane is as follows:
wherein: r is methacryloxypropyl or glycidoxypropyl;
step four, preparing the high-toughness high-temperature-resistant impact-resistant road material:
and (3) uniformly spreading and paving the modified poly-p-phenylene benzobisoxazole fibers prepared in the step (three) to form fibers, adding a curing agent into epoxy resin to prepare a casting material, uniformly casting the casting material on the paved fiber framework, and curing to prepare the high-toughness high-temperature-resistant impact-resistant road material.
The invention also has the following technical characteristics:
in the first step, the pretreatment process is as follows: soaking the poly-p-phenylene benzobisoxazole fiber in acetone for 12h to remove surface attachments, taking out the poly-p-phenylene benzobisoxazole fiber, and drying the poly-p-phenylene benzobisoxazole fiber in a blast drying oven at 100 ℃ for 4 h. And (2) immersing the dried poly-p-phenylene benzobisoxazole fiber into an epichlorohydrin solution, irradiating by using gamma rays, repeatedly washing by using acetone for 12 hours, and drying at 100 ℃ for 1 hour.
In the first step, the pretreated poly-p-phenylene benzobisoxazole fiber is soaked in an ethylenediamine methanol solution at 25 ℃ for 12 hours in an environment filled with nitrogen, and then is washed until the pH value is 7, so as to obtain the aminated poly-p-phenylene benzobisoxazole fiber.
In the second step, the specific process of the addition reaction is as follows: and (2) mixing the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one with acrylic ester, adding the mixture into methanol, heating and stirring the mixture for 24 hours at the temperature of 50 ℃, and repeatedly washing the mixture with deionized water to obtain the acrylic ester-poly-p-phenylene benzobisoxazole fiber.
In the third step, the grafting treatment specifically comprises the following steps: and (3) drying the acrylate-poly (p-phenylene benzobisoxazole) fiber prepared in the second step at 100 ℃ for 0.5h, adding transparent viscous liquid hyperbranched polysiloxane, diluting the reaction mixture with methanol, heating at 30 ℃ for 12h, washing with deionized water, and drying at 100 ℃ for 1.5h to prepare the modified poly (p-phenylene benzobisoxazole) fiber.
In the third step, the preparation process of the hyperbranched polysiloxane comprises the following steps: uniformly mixing MPS, GPTMS, distilled water and absolute ethyl alcohol in proportion, adjusting the pH value of the solution to 5.0-6.0, heating to 60 ℃, reacting for 4 hours, and carrying out vacuum drying on the obtained product and removing the mixed solvent generated in the reaction to obtain the hyperbranched polysiloxane.
Specifically, the weight portions are as follows:
8-16 parts of curing agent is correspondingly added into every 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework, and 25-45 parts of poly (p-phenylene benzobisoxazole) fiber raw materials are adopted to prepare the epoxy resin fiber;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8-20 parts of MPS, 8-25 parts of GPTMS, 16-30 parts of distilled water and 40-55 parts of absolute ethyl alcohol.
More preferably, the weight parts of:
12-16 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework, and 25-30 parts of poly (p-phenylene benzobisoxazole) fiber raw materials are adopted to prepare the epoxy resin fiber;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8-10 parts of MPS, 8-12 parts of GPTMS, 16-20 parts of distilled water and 40-50 parts of absolute ethyl alcohol.
Most preferably, the weight parts of:
12 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 25 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8 parts of MPS, 8 parts of GPTMS, 6 parts of distilled water and 40 parts of absolute ethyl alcohol.
In the fourth step, the curing temperature is 80 ℃.
The material for the high-toughness high-temperature-resistant impact-resistant road is prepared by the preparation method of the material for the high-toughness high-temperature-resistant impact-resistant road.
Compared with the prior art, the invention has the following technical effects:
the invention firstly applies the hyperbranched polysiloxane and the poly-p-phenylene benzobisoxazole fiber to the field of road asphalt modified fiber. The hyperbranched polysiloxane has a highly branched structure and excellent performance, and has various and simple synthesis modes and controllable process.
The poly-p-phenylene benzobisoxazole fiber adopted by the invention is heterocyclic aromatic polyamide prepared by taking 4, 6-diaminoresorcinol and trimethyl silazane as raw materials and adopting a trimethyl silane alkylation method, has the excellent performances of high strength, high thermal stability, corrosion resistance, oxidation resistance, moisture resistance and the like, can be dissolved in solvents such as polyphosphoric acid, polyphosphoric acid methanesulfonic acid and the like, and has obvious effect of improving the impact resistance and the high temperature resistance of epoxy resin, and the heat resistance temperature reaches 600 ℃.
The hyperbranched polysiloxane (III) is a highly branched polymer with Si-O as a main chain and-OH as a side group, has the high heat resistance of an organic silicon polymer and the excellent performances of high fluidity, corrosion resistance, weather resistance, low viscosity and the like of a hyperbranched polymer, can be used as a modifier of epoxy resin, and improves the impact resistance and toughness of the epoxy resin while ensuring the stability.
(IV) the hyperbranched polysiloxane molecule prepared by the invention carries active functional groups, the molecular terminal of the hyperbranched polysiloxane molecule contains a large number of branched chains and groups such as silicon chloride, silicon hydride and the like, the functional modification is easy, the hyperbranched polysiloxane molecule can be used for fiber surface grafting treatment, the activity of the poly (p-phenylene benzobisoxazole) fiber is obviously improved, the roughness of the fiber surface is enhanced, and the bonding effect of the fiber and epoxy resin is improved.
The modified poly (p-phenylene benzobisoxazole) fiber prepared by the method can effectively improve the defects of low toughness, poor impact resistance, high temperature difference resistance and the like of epoxy resin, and can be widely applied to various bridge deck pavement layers.
The present invention will be explained in further detail with reference to examples.
Detailed Description
In the following examples and comparative examples, MPS is γ -methacryloxypropyltrimethoxysilane; GPTMS is gamma-glycidoxypropyltrimethoxysilane.
The molecular formula of the hyperbranched polysiloxane is as follows:
wherein: r is methacryloxypropyl or glycidoxypropyl.
The curing agent is phthalic anhydride.
The epoxy resin is E-42 epoxy resin.
The structural formula of the poly-p-phenylene benzobisoxazole fiber is as follows:
wherein: n is 50 to 120.
The preparation process of the poly-p-phenylene benzobisoxazole fiber comprises the following steps: 4, 6-diamino resorcinol and trimethyl silazane are used as raw materials, and the catalyst is prepared by adopting a trimethyl silicon alkylation method.
The heat-resisting temperature of the poly-p-phenylene benzobisoxazole fiber reaches 600 ℃, the poly-p-phenylene benzobisoxazole fiber has excellent thermal stability and can be dissolved in solvents such as polyphosphoric acid, polyphosphoric acid methanesulfonic acid and the like.
The following embodiments of the present invention are provided, and it should be noted that the present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention are within the protection scope of the present invention.
Example 1:
this example provides a method for preparing a high-toughness, high-temperature-resistant, and impact-resistant material for roads, which includes the following steps:
step one, preparing ammoniated poly-p-phenylene benzobisoxazole fibers:
soaking the pretreated poly-p-phenylene benzobisoxazole fiber in an ethylenediamine methanol solution to obtain an ammoniated poly-p-phenylene benzobisoxazole fiber;
in the first step, the pretreatment process is as follows: soaking the poly-p-phenylene benzobisoxazole fiber in acetone for 12h to remove surface attachments, taking out the poly-p-phenylene benzobisoxazole fiber, and drying the poly-p-phenylene benzobisoxazole fiber in a blast drying oven at 100 ℃ for 4 h. And (2) immersing the dried poly-p-phenylene benzobisoxazole fiber into an epichlorohydrin solution, irradiating by using gamma rays, repeatedly washing by using acetone for 12 hours, and drying at 100 ℃ for 1 hour.
In the first step, the pretreated poly-p-phenylene benzobisoxazole fiber is soaked in an ethylenediamine methanol solution at 25 ℃ for 12 hours in an environment filled with nitrogen, and then is washed until the pH value is 7, so as to obtain the aminated poly-p-phenylene benzobisoxazole fiber.
Step two, preparing acrylate-poly (p-Phenylene Benzobisoxazole) (PBO) fibers:
mixing the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one with acrylic ester for addition reaction to obtain acrylic ester-poly-p-phenylene benzobisoxazole fiber;
in the second step, the specific process of the addition reaction is as follows: and (2) mixing the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one with acrylic ester, adding the mixture into methanol, heating and stirring the mixture for 24 hours at the temperature of 50 ℃, and repeatedly washing the mixture with deionized water to obtain the acrylic ester-poly-p-phenylene benzobisoxazole fiber.
Step three, preparing modified poly-p-phenylene benzobisoxazole fiber:
grafting the acrylate-poly (p-phenylene benzobisoxazole) fiber prepared in the step two with hyperbranched polysiloxane to prepare modified poly (p-phenylene benzobisoxazole) fiber;
in the third step, the grafting treatment comprises the following specific processes: and (3) drying the acrylate-poly (p-phenylene benzobisoxazole) fiber prepared in the second step at 100 ℃ for 0.5h, adding transparent viscous liquid hyperbranched polysiloxane, diluting the reaction mixture with methanol, heating at 30 ℃ for 12h, washing with deionized water, and drying at 100 ℃ for 1.5h to prepare the modified poly (p-phenylene benzobisoxazole) fiber.
In the third step, the preparation process of the hyperbranched polysiloxane comprises the following steps: uniformly mixing MPS, GPTMS, distilled water and absolute ethyl alcohol in proportion, adjusting the pH value of the solution to 5.0-6.0, heating to 60 ℃, reacting for 4 hours, and carrying out vacuum drying on the obtained product and removing the mixed solvent generated in the reaction to obtain the hyperbranched polysiloxane.
Step four, preparing the high-toughness high-temperature-resistant impact-resistant road material:
and (3) uniformly spreading and paving the modified poly-p-phenylene benzobisoxazole fibers prepared in the step (three) to form fibers, adding a curing agent into epoxy resin to prepare a casting material, uniformly casting the casting material on the paved fiber framework, and curing to prepare the high-toughness high-temperature-resistant impact-resistant road material.
In the fourth step, the curing temperature is 80 ℃.
In the preparation method of the material for the high-toughness high-temperature-resistant impact-resistant road of the embodiment, the ratio of the main raw materials is as follows by weight:
12 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 25 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8 parts of MPS, 8 parts of GPTMS, 6 parts of distilled water and 40 parts of absolute ethyl alcohol.
The high-toughness high-temperature-resistant impact-resistant road material is prepared by the preparation method of the high-toughness high-temperature-resistant impact-resistant road material.
Example 2:
this example provides a method for preparing a high-toughness, high-temperature-resistant, and impact-resistant material for a road, which includes the following steps in parts by weight:
10 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 30 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8 parts of MPS, 10 parts of GPTMS, 16 parts of distilled water and 40 parts of absolute ethyl alcohol.
The high-toughness high-temperature-resistant impact-resistant road material is prepared by the preparation method of the high-toughness high-temperature-resistant impact-resistant road material.
Example 3:
this example provides a method for preparing a high-toughness, high-temperature-resistant, and impact-resistant material for a road, which includes the following steps in parts by weight:
12 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 25 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8 parts of MPS, 8 parts of GPTMS, 16 parts of distilled water and 40 parts of absolute ethyl alcohol.
The high-toughness high-temperature-resistant impact-resistant road material is prepared by the preparation method of the high-toughness high-temperature-resistant impact-resistant road material.
Example 4:
this example provides a method for preparing a high-toughness, high-temperature-resistant, and impact-resistant material for a road, which includes the following steps in parts by weight:
12 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 25 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 10 parts of MPS, 12 parts of GPTMS, 20 parts of distilled water and 50 parts of absolute ethyl alcohol.
The high-toughness high-temperature-resistant impact-resistant road material is prepared by the preparation method of the high-toughness high-temperature-resistant impact-resistant road material.
Example 5:
this example provides a method for preparing a high-toughness, high-temperature-resistant, and impact-resistant material for a road, which includes the following steps in parts by weight:
adding 16 parts of curing agent into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 30 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 10 parts of MPS, 12 parts of GPTMS, 20 parts of distilled water and 50 parts of absolute ethyl alcohol.
The high-toughness high-temperature-resistant impact-resistant road material is prepared by the preparation method of the high-toughness high-temperature-resistant impact-resistant road material.
Example 6:
this example provides a method for preparing a high-toughness, high-temperature-resistant, and impact-resistant material for a road, which includes the following steps in parts by weight:
adding 16 parts of curing agent into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 30 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 15 parts of MPS, 16 parts of GPTMS, 25 parts of distilled water and 50 parts of absolute ethyl alcohol.
The high-toughness high-temperature-resistant impact-resistant road material is prepared by the preparation method of the high-toughness high-temperature-resistant impact-resistant road material.
Example 7:
this example provides a method for preparing a high-toughness, high-temperature-resistant, and impact-resistant material for a road, which includes the following steps in parts by weight:
10 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 40 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 15 parts of MPS, 20 parts of GPTMS, 25 parts of distilled water and 50 parts of absolute ethyl alcohol.
The high-toughness high-temperature-resistant impact-resistant road material is prepared by the preparation method of the high-toughness high-temperature-resistant impact-resistant road material.
Example 8:
this example provides a method for preparing a high-toughness, high-temperature-resistant, and impact-resistant material for a road, which includes the following steps in parts by weight:
8 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework which is made of 45 parts of poly-p-phenylene benzobisoxazole fiber raw materials;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 20 parts of MPS, 25 parts of GPTMS, 30 parts of distilled water and 55 parts of absolute ethyl alcohol.
The high-toughness high-temperature-resistant impact-resistant road material is prepared by the preparation method of the high-toughness high-temperature-resistant impact-resistant road material.
Comparative example 1:
this comparative example provides a method of making a pavement material comprising the steps of:
and adding a curing agent into the epoxy resin to prepare a casting material, and directly curing the casting material at 80 ℃ to prepare the road material.
As in example 1, 12 parts of curing agent per 100 parts of epoxy resin was added.
The raw materials used in this comparative example were the same as in example 1.
Comparative example 2:
this comparative example provides a method of making a pavement material comprising the steps of:
the preparation method comprises the steps of uniformly spreading and flatly paving the poly-p-phenylene benzobisoxazole fibers to form fibers, adding a curing agent into epoxy resin to prepare a casting material, uniformly casting the casting material on a flatly paved fiber framework, and curing at 80 ℃ to prepare the road material.
12 parts of curing agent per 100 parts of epoxy resin, as in example 1;
every 100 parts of epoxy resin is added with 25 parts of poly-p-phenylene benzobisoxazole fiber correspondingly.
The raw materials used in this comparative example were the same as in example 1.
Comparative example 3:
this comparative example provides a method of making a pavement material comprising the steps of:
and adding a curing agent and hyperbranched polysiloxane into the epoxy resin to prepare a casting material, uniformly casting the casting material on a flat fiber framework, and curing at 80 ℃ to prepare the road material.
12 parts of curing agent per 100 parts of epoxy resin, as in example 1;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8 parts of MPS, 8 parts of GPTMS, 6 parts of distilled water and 40 parts of absolute ethyl alcohol.
The raw materials used in this comparative example were the same as in example 1.
Comparative example 4:
this comparative example provides a method of making a pavement material comprising the steps of:
step one, preparing ammoniated poly-p-phenylene benzobisoxazole fibers:
the procedure for preparing the aminated poly (p-phenylene benzobisoxazole) fiber according to this comparative example was the same as the procedure for preparing the aminated poly (p-phenylene benzobisoxazole) fiber according to the first step of example 1.
Step two, preparing the road material:
uniformly spreading and paving the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one to form a fiber framework, adding a curing agent into epoxy resin to prepare a casting material, uniformly casting the casting material on the paved fiber framework, and curing at 80 ℃ to prepare the road material.
12 parts of curing agent per 100 parts of epoxy resin, as in example 1;
every 100 parts of epoxy resin is correspondingly added with a fiber skeleton which is an ammoniated poly-p-phenylene benzobisoxazole fiber made of 25 parts of poly-p-phenylene benzobisoxazole fiber.
The raw materials used in this comparative example were the same as in example 1.
Comparative example 5:
this comparative example provides a method of making a pavement material comprising the steps of:
step one, preparing ammoniated poly-p-phenylene benzobisoxazole fibers:
the procedure for preparing the aminated poly (p-phenylene benzobisoxazole) fiber according to this comparative example was the same as the procedure for preparing the aminated poly (p-phenylene benzobisoxazole) fiber according to the first step of example 1.
Step two, preparing acrylate-poly (p-Phenylene Benzobisoxazole) (PBO) fibers:
the procedure for preparing the acryl-p-phenylene benzobisoxazole fiber in this comparative example was the same as the method for preparing the acryl-p-phenylene benzobisoxazole fiber in step two of example 1.
Step three, preparing the road material:
and (3) uniformly spreading and flatly spreading the acrylate-poly (p-phenylene benzobisoxazole) fibers prepared in the step (II) to form a fiber framework, adding a curing agent into epoxy resin to prepare a casting material, uniformly casting the casting material on the flatly spread fiber framework, and curing at the temperature of 80 ℃ to prepare the road material.
12 parts of curing agent per 100 parts of epoxy resin, as in example 1;
the fiber skeleton added correspondingly to each 100 parts of epoxy resin is acrylate-poly (p-phenylene benzobisoxazole) fiber made of 25 parts of poly (p-phenylene benzobisoxazole) fiber.
The raw materials used in this comparative example were the same as in example 1.
Comparative example 6:
this comparative example provides a method of making a pavement material comprising the steps of:
step one, preparing ammoniated poly-p-phenylene benzobisoxazole fibers:
the procedure for preparing the aminated poly (p-phenylene benzobisoxazole) fiber according to this comparative example was the same as the procedure for preparing the aminated poly (p-phenylene benzobisoxazole) fiber according to the first step of example 1.
Step two, preparing modified poly-p-phenylene benzobisoxazole fiber:
the modified poly (p-phenylene benzobisoxazole) fiber prepared in this comparative example is different from the modified poly (p-phenylene benzobisoxazole) fiber prepared in step three of example 1 in that the aminated poly (p-phenylene benzobisoxazole) fiber prepared in step one is directly modified without using an acrylic ester. The method comprises the following specific steps:
carrying out grafting treatment on the modified fiber and hyperbranched polysiloxane of the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one to prepare modified poly-p-phenylene benzobisoxazole fiber;
in the second step, the grafting treatment comprises the following specific processes: and (2) drying the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one at 100 ℃ for 0.5h, adding transparent viscous liquid hyperbranched polysiloxane, diluting the reaction mixture with methanol, heating at 30 ℃ for 12h, washing with deionized water, and drying at 100 ℃ for 1.5h to prepare the modified poly-p-phenylene benzobisoxazole fiber.
In step two, the procedure for preparing the hyperbranched polysiloxane was the same as that of the hyperbranched polysiloxane in step three of example 1.
Step three, preparing the road material:
and (3) uniformly spreading and paving the modified poly-p-phenylene benzobisoxazole fibers prepared in the step (II) to form a fiber framework, adding a curing agent into epoxy resin to prepare a casting material, uniformly casting the casting material on the paved fiber framework, and curing at the temperature of 80 ℃ to prepare the road material.
12 parts of curing agent per 100 parts of epoxy resin, as in example 1;
the fiber skeleton added correspondingly to each 100 parts of epoxy resin is modified poly-p-phenylene benzobisoxazole fiber made of 25 parts of poly-p-phenylene benzobisoxazole fiber.
The hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8 parts of MPS, 8 parts of GPTMS, 6 parts of distilled water and 40 parts of absolute ethyl alcohol.
The raw materials used in this comparative example were the same as in example 1.
And (3) performance testing:
in order to verify the tensile strength, elongation at break, flexibility at low temperature, and shear, tensile and impact strengths of the road material, the road material prepared in the examples and comparative examples of the present invention was subjected to basic performance tests and indoor simulation tests according to the relevant specifications of the test method for waterproof coating for construction (GB/T16777-.
TABLE 1 results of the property test of the road materials prepared in examples and comparative examples
Analysis of Table 1 reveals that:
(1) analysis of comparative examples 1-6 shows that compared with untreated epoxy resin, the hyperbranched polysiloxane and the poly (p-phenylene benzobisoxazole) fiber can significantly improve the toughness and strength of the epoxy resin; compared with the epoxy resin treated by the poly-p-phenylene benzobisoxazole fiber, the hyperbranched polysiloxane can improve the tensile strength of the epoxy resin.
(2) As can be seen from the analysis of examples 1-7 and comparative examples 1-6, compared with untreated epoxy resin, the tensile strength, elongation at break and impact strength of the road material prepared by the invention are obviously improved, which indicates that the toughness, adhesive property and strength of the material are improved; the material does not crack under the conditions of minus 20 ℃ and 90 ℃, which shows that the low-temperature toughness of the material is enhanced, and the shear strength and the bonding strength are not obviously reduced under the high-temperature (70 ℃) condition compared with the shear strength and the bonding strength under the normal-temperature (25 ℃) condition, which shows that the material has better high-temperature resistance.
(3) It can be seen from the analysis of examples 1 to 8 and comparative example 2 that the pavement material of the present invention has better performance than the epoxy resin treated with the poly (p-phenylene benzobisoxazole) fiber, because the hyperbranched polysiloxane has a large number of functional groups on the surface of the molecule, and can react with the poly (p-phenylene benzobisoxazole) fiber to improve the fiber activity, and the bonding effect between the poly (p-phenylene benzobisoxazole) fiber and the epoxy resin can be significantly improved.
(4) Analysis of comparative examples 2, 4, and 6 shows that compared with the road material prepared by directly grafting hyperbranched polysiloxane after fiber ammoniation, the aminated poly-p-phenylene benzobisoxazole fiber treated by acrylate has better bonding effect and flexibility with epoxy resin, because acrylate has good bonding strength, and the bonded part has certain impact resistance and toughness.
(5) As can be seen from the analysis of the examples 1 to 8, the best index performance of the example 1 can be found comprehensively, and the best raw material composition is as follows: 8 parts of gamma-Methacryloxypropyltrimethoxysilane (MPS), 8 parts of gamma-Glycidoxypropyltrimethoxysilane (GPTMS), 16 parts of distilled water, 40 parts of absolute ethyl alcohol, 25 parts of poly-p-phenylene benzobisoxazole fibers, 100 parts of epoxy resin and 12 parts of curing agent.
Claims (9)
1. A preparation method of a high-toughness high-temperature-resistant impact-resistant road material is characterized by comprising the following steps:
step one, preparing ammoniated poly-p-phenylene benzobisoxazole fibers:
soaking the pretreated poly-p-phenylene benzobisoxazole fiber in an ethylenediamine methanol solution to obtain an ammoniated poly-p-phenylene benzobisoxazole fiber;
step two, preparing acrylate-poly (p-Phenylene Benzobisoxazole) (PBO) fibers:
mixing the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one with acrylic ester for addition reaction to obtain acrylic ester-poly-p-phenylene benzobisoxazole fiber;
step three, preparing modified poly-p-phenylene benzobisoxazole fiber:
grafting the acrylate-poly (p-phenylene benzobisoxazole) fiber prepared in the step two with hyperbranched polysiloxane to prepare modified poly (p-phenylene benzobisoxazole) fiber;
the molecular formula of the hyperbranched polysiloxane is as follows:
wherein: r is methacryloxypropyl or glycidoxypropyl;
in the third step, the preparation process of the hyperbranched polysiloxane comprises the following steps: uniformly mixing MPS, GPTMS, distilled water and absolute ethyl alcohol in proportion, adjusting the pH value of the solution to 5.0-6.0, heating to 60 ℃, reacting for 4 hours, and carrying out vacuum drying on the obtained product and removing the mixed solvent generated in the reaction to obtain hyperbranched polysiloxane;
step four, preparing the high-toughness high-temperature-resistant impact-resistant road material:
and (3) uniformly spreading and paving the modified poly-p-phenylene benzobisoxazole fibers prepared in the step (three) to form fibers, adding a curing agent into epoxy resin to prepare a casting material, uniformly casting the casting material on the paved fiber framework, and curing to prepare the high-toughness high-temperature-resistant impact-resistant road material.
2. The method for preparing the high-toughness high-temperature-resistant impact-resistant road material as claimed in claim 1, wherein in the step one, the pretreatment process comprises the following steps: soaking the poly-p-phenylene benzobisoxazole fiber in acetone for 12h to remove surface attachments, taking out the poly-p-phenylene benzobisoxazole fiber and drying the poly-p-phenylene benzobisoxazole fiber in a blast drying oven at 100 ℃ for 4 h; and (2) immersing the dried poly-p-phenylene benzobisoxazole fiber into an epichlorohydrin solution, irradiating by using gamma rays, repeatedly washing by using acetone for 12 hours, and drying at 100 ℃ for 1 hour.
3. The method for preparing a high-toughness high-temperature-resistant impact-resistant road material as claimed in claim 1, wherein in the step one, the pretreated polyparaphenylene benzobisoxazole fiber is soaked in an ethylenediamine methanol solution at 25 ℃ for 12h in an environment filled with nitrogen, and then washed until the pH value is 7, so as to obtain the aminated polyparaphenylene benzobisoxazole fiber.
4. The method for preparing the high-toughness high-temperature-resistant impact-resistant road material as claimed in claim 1, wherein in the step two, the specific process of the addition reaction is as follows: and (2) mixing the aminated poly-p-phenylene benzobisoxazole fiber prepared in the step one with acrylic ester, adding the mixture into methanol, heating and stirring the mixture for 24 hours at the temperature of 50 ℃, and repeatedly washing the mixture with deionized water to obtain the acrylic ester-poly-p-phenylene benzobisoxazole fiber.
5. The method for preparing the high-toughness high-temperature-resistant impact-resistant road material as claimed in claim 1, wherein in the third step, the grafting treatment comprises the following specific steps: and (3) drying the acrylate-poly (p-phenylene benzobisoxazole) fiber prepared in the second step at 100 ℃ for 0.5h, adding transparent viscous liquid hyperbranched polysiloxane, diluting the reaction mixture with methanol, heating at 30 ℃ for 12h, washing with deionized water, and drying at 100 ℃ for 1.5h to prepare the modified poly (p-phenylene benzobisoxazole) fiber.
6. The method for preparing the high-toughness high-temperature-resistant impact-resistant road material as claimed in claim 1, wherein the weight portions are as follows:
8-16 parts of curing agent is correspondingly added into every 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework, and 25-45 parts of poly (p-phenylene benzobisoxazole) fiber raw materials are adopted to prepare the epoxy resin fiber;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8-20 parts of MPS, 8-25 parts of GPTMS, 16-30 parts of distilled water and 40-55 parts of absolute ethyl alcohol.
7. The method for preparing the high-toughness high-temperature-resistant impact-resistant road material as claimed in claim 1, wherein the weight portions are as follows:
12-16 parts of curing agent is correspondingly added into each 100 parts of epoxy resin;
every 100 parts of epoxy resin is correspondingly added into a fiber framework, and 25-30 parts of poly (p-phenylene benzobisoxazole) fiber raw materials are adopted to prepare the epoxy resin fiber;
the hyperbranched polysiloxane prepared from the following raw materials is adopted for each 100 parts of the fiber framework correspondingly added in the epoxy resin; 8-10 parts of MPS, 8-12 parts of GPTMS, 16-20 parts of distilled water and 40-50 parts of absolute ethyl alcohol.
8. The method for preparing a high-toughness high-temperature-resistant impact-resistant road material as claimed in claim 1, wherein the curing agent is phthalic anhydride; the epoxy resin is E-42 epoxy resin;
the structural formula of the poly-p-phenylene benzobisoxazole fiber is as follows:
wherein: n is 50 to 120.
9. A high-toughness high-temperature-resistant impact-resistant road material, which is prepared by the method for preparing the high-toughness high-temperature-resistant impact-resistant road material as claimed in any one of claims 1 to 8.
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|---|---|---|---|---|
| CN101319084A (en) * | 2008-07-17 | 2008-12-10 | 上海交通大学 | Preparation method for poly-p-phenylene-benzo-dioxazole fibre/epoxy resin composite material |
| CN109265922A (en) * | 2018-08-17 | 2019-01-25 | 西北工业大学 | A kind of high tenacity self-catalysis epoxy resin and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319084A (en) * | 2008-07-17 | 2008-12-10 | 上海交通大学 | Preparation method for poly-p-phenylene-benzo-dioxazole fibre/epoxy resin composite material |
| CN109265922A (en) * | 2018-08-17 | 2019-01-25 | 西北工业大学 | A kind of high tenacity self-catalysis epoxy resin and preparation method |
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| Title |
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