CN112029299A - Modified epoxy asphalt and preparation method thereof - Google Patents
Modified epoxy asphalt and preparation method thereof Download PDFInfo
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- CN112029299A CN112029299A CN201910475702.8A CN201910475702A CN112029299A CN 112029299 A CN112029299 A CN 112029299A CN 201910475702 A CN201910475702 A CN 201910475702A CN 112029299 A CN112029299 A CN 112029299A
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- asphalt
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- anhydride
- shearing
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- 239000010426 asphalt Substances 0.000 title claims abstract description 165
- 239000004593 Epoxy Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003822 epoxy resin Substances 0.000 claims abstract description 33
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 26
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 22
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000010008 shearing Methods 0.000 claims description 70
- 238000003756 stirring Methods 0.000 claims description 62
- 238000006243 chemical reaction Methods 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 19
- 150000008064 anhydrides Chemical group 0.000 claims description 14
- 125000003118 aryl group Chemical group 0.000 claims description 12
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 12
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 239000000084 colloidal system Substances 0.000 claims description 8
- 229920006395 saturated elastomer Polymers 0.000 claims description 8
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 8
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims description 7
- 239000001116 FEMA 4028 Substances 0.000 claims description 7
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 7
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 7
- 229960004853 betadex Drugs 0.000 claims description 7
- 229920001450 Alpha-Cyclodextrin Polymers 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- HFHDHCJBZVLPGP-RWMJIURBSA-N alpha-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO HFHDHCJBZVLPGP-RWMJIURBSA-N 0.000 claims description 6
- 229940043377 alpha-cyclodextrin Drugs 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 5
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 5
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 claims description 4
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- HTZCNXWZYVXIMZ-UHFFFAOYSA-M benzyl(triethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC1=CC=CC=C1 HTZCNXWZYVXIMZ-UHFFFAOYSA-M 0.000 claims description 4
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims description 4
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 4
- 229920002647 polyamide Polymers 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims description 3
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 2
- WVRNUXJQQFPNMN-VAWYXSNFSA-N 3-[(e)-dodec-1-enyl]oxolane-2,5-dione Chemical compound CCCCCCCCCC\C=C\C1CC(=O)OC1=O WVRNUXJQQFPNMN-VAWYXSNFSA-N 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 claims description 2
- GDSRMADSINPKSL-HSEONFRVSA-N gamma-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO GDSRMADSINPKSL-HSEONFRVSA-N 0.000 claims description 2
- 229940080345 gamma-cyclodextrin Drugs 0.000 claims description 2
- 229920000141 poly(maleic anhydride) Polymers 0.000 claims description 2
- 229920005652 polyisobutylene succinic anhydride Polymers 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 2
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 2
- 230000004048 modification Effects 0.000 abstract description 7
- 238000012986 modification Methods 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 13
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 239000003208 petroleum Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000002383 tung oil Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/329—Phosphorus containing acids
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- 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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/30—Adapting or protecting infrastructure or their operation in transportation, e.g. on roads, waterways or railways
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Civil Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses modified epoxy asphalt and a preparation method thereof. The modified epoxy asphalt comprises the following raw material components in parts by weight: modified mixed asphalt: 100 parts of (A); cyclodextrin: 1-8 parts; initiator: 0.1-0.9 part; epoxy resin: 35-64 parts of a solvent; accelerator (b): 0.04-0.6 part; curing agent A: 5-20 parts of a solvent; curing agent B: 20-45 parts. The invention effectively solves the problem of poor compatibility of the modified epoxy asphalt, uses the natural modified material which is environment-friendly, and uses less organic reagent in the modification process.
Description
Technical Field
The invention relates to modified asphalt and a preparation method thereof, in particular to high-compatibility modified epoxy asphalt and a preparation method thereof.
Background
Thermosetting epoxy asphalt is an excellent material for paving a large-span steel bridge deck, and road workers put a great deal of effort on the research and development of the epoxy asphalt material, but the compatibility of the asphalt and epoxy resin is extremely poor due to the difference of the physical and chemical properties of the asphalt and the epoxy resin, so that the development and application of the epoxy asphalt material are influenced.
The physical and chemical properties of petroleum asphalt and epoxy resin are greatly different, and if the petroleum asphalt and the epoxy resin are directly mixed, the petroleum asphalt and the epoxy resin are easy to separate. The difference of the physical and chemical properties is mainly reflected in the solubility parameter, density, dielectric constant and the like. The solubility parameter of petroleum asphalt is about 8.71, while the solubility parameter of epoxy resin is about 10.42, which have a large difference and belong to thermodynamically incompatible systems. The density of the petroleum asphalt is about 0.98-1.01 g/cm3The density of the common epoxy resin is about 1.15-1.20 g/cm3And the two are easy to biologically settle and delaminate after being mixed. The petroleum asphalt is a very complex mixture with chemical components, the dielectric constant of the petroleum asphalt is 2.5-3.0, the petroleum asphalt belongs to nonpolar or low-polarity substances, and the dielectric constant of the more common epoxy resin is about 3.9, and the petroleum asphalt belongs to polar substances. After the petroleum asphalt and the resin are mixed, the non-polar asphalt and the polar resin are difficult to form a homogeneous phase and cannot achieve the integral uniformity, the asphalt is separated out after the epoxy resin is cured, the thermoplasticity of the asphalt is not changed by a curing system, the capability of the asphalt for improving the flexibility of the curing system is not released, and the integral related performance of the material is poor.
CN1837290A discloses a thermosetting epoxy asphalt material for roads and bridges and a preparation method thereof. The preparation method improves the compatibility of the epoxy resin and the matrix asphalt by carrying out the maleic anhydrization modification on the matrix asphalt, although the compatibility is improved to a certain degree, the conversion rate in the maleic anhydrization process is very low, and a large amount of acid mist can appear during the heating of the asphalt to influence the safety and the environmental protection; the presence of unconverted anhydride monomer in the asphalt causes the cured system to exhibit many voids, affecting the strength and tensile properties of the final cured system, which is undesirable in this way.
CN101255276A discloses an epoxy asphalt material for roads and bridges and a preparation method thereof, which mainly improves the problems of improving compatibility by maleic anhydride modification, and prevents the pollution of the volatilization of maleic anhydride to the environment by adding organic alcohol substances to neutralize and convert unreacted maleic anhydride monomers. However, the method has the defects of more reactions, difficult control of reaction process, difficult complete conversion of the maleic anhydride monomer and influence on the strength of a later-period curing system due to excessive addition of organic alcohols.
CN107603248A discloses an epoxy tung oil thermosetting asphalt compatibilizer, modified thermosetting epoxy asphalt and a preparation method thereof. But the compatibility of the compatibilizer prepared by the method with epoxy resin and asphalt is improved mainly through physical action, and the effect is not great; and the prepared compatibilizer contains epoxy groups, so that a curing agent cannot be contacted with the compatibilizer in advance, and the using process becomes complicated.
In conclusion, the prior art has defects of different degrees when solving the problem of compatibility of asphalt and epoxy resin, has the problems of environmental pollution due to large use amount of acid substances and organic solvents, and has small improvement degree of compatibility, thereby having adverse effect on the overall performance of a final curing system.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides modified epoxy asphalt and a preparation method thereof. The modified epoxy asphalt has high compatibility, effectively solves the problem of poor compatibility of the modified epoxy asphalt, uses environment-friendly natural modified materials, and has less use amount of organic reagents in the modification process.
The invention provides modified epoxy asphalt which comprises the following raw material components in parts by weight:
modified mixed asphalt: 100 parts of (A);
cyclodextrin: 1-8 parts, preferably 2-6 parts;
initiator: 0.1 to 0.9 part, preferably 0.2 to 0.6 part;
epoxy resin: 35-64 parts, preferably 40-55 parts;
accelerator (b): 0.04-0.6 part;
curing agent A: 5-20 parts of a solvent;
curing agent B: 20-45 parts.
The modified blended asphalt comprises the following components in parts by weight:
base asphalt I: 20-70 parts, preferably 30-65 parts;
matrix asphalt II: 30-80 parts, preferably 35-70 parts;
modifying agent: 0.03 to 0.5 part, preferably 0.05 to 0.4 part.
The modifier is polyphosphoric acid (PPA).
The matrix asphalt I: the aromatic asphalt comprises, by mass, 20-30% of saturated components, 25-35% of aromatic components, 30-45% of colloid and 0.1-2% of asphaltene.
The matrix asphalt II: the aromatic asphalt comprises, by mass, 15-30% of saturated components, 20-40% of aromatic components, 10-20% of colloid and 15-30% of asphaltene.
The cyclodextrin is one or more of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin, and is preferably alpha-cyclodextrin and/or beta-cyclodextrin.
The initiator is one or more of dicumyl peroxide, tert-butyl hydroperoxide, benzoyl peroxide and sodium metabisulfite.
The epoxy resin is E-44 bisphenol A type epoxy resin and E-51 bisphenol A type epoxy resin, and preferably E-51 bisphenol A type epoxy resin.
The accelerant is one or more of DMP-30, triethylamine, triethanolamine, benzyltriethylammonium chloride, resorcinol and m-cresol.
The curing agent A is an amine curing agent, and specifically is one or more of low molecular polyamide 651, m-phenylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, low molecular polyamide 650, diethylaminopropylamine, N-aminoethyl piperazine and isophorone diamine.
The curing agent B is an anhydride curing agent, specifically one or more of maleic anhydride, polyisobutylene succinic anhydride, methyl nadic anhydride, modified methyl nadic anhydride, dodecenyl succinic anhydride, methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, elaeostearic anhydride, polyazelaic anhydride, polyglutamic anhydride, polyazelaic anhydride or hydrolyzed polymaleic anhydride, and preferably one or more of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride and elaeostearic anhydride.
The invention also provides a preparation method of the modified epoxy asphalt, which comprises the following steps:
(1) preparing modified blended asphalt;
(2) heating the modified blended asphalt prepared in the step (1) to a flowing state, pouring the heated modified blended asphalt into a high-pressure reaction kettle, adjusting the temperature in the kettle, stirring, adding cyclodextrin, carrying out programmed heating, and continuing stirring;
(3) adding an initiator into a high-pressure reaction kettle, stirring, and filling inert gas for reaction;
(4) and (4) shearing the material reacted in the step (3), mixing the sheared material with epoxy resin, a curing agent A, a curing agent B and an accelerator, and shearing to obtain the modified epoxy asphalt.
The method for preparing the modified blended asphalt in the step (1) comprises the following steps: preheating the base asphalt I and the base asphalt II to a flowing state, mixing, and stirring under a heating condition to obtain mixed asphalt; and then adding polyphosphoric acid, continuing heating and stirring to obtain the modified blended asphalt.
In the method for preparing the modified blended asphalt, the heating temperature is 100-180 ℃, the preferred heating temperature is 120-160 ℃, the stirring time is 1-6 hours, the preferred stirring time is 3-6 hours, and the stirring speed is 200-500 r/min. After the polyphosphoric acid is added, the heating temperature is 120-170 ℃, the preferable temperature is 135-170 ℃, the stirring time is 4-10 hours, and the stirring speed is 300-600 r/min.
In the step (2), the temperature in the kettle is adjusted to be 100-120 ℃.
In the step (2), the cyclodextrin is added within 0.5-1.5 h, the temperature programming rate is 0.5-1 ℃/min, and the temperature programming is carried out to 130-160 ℃, preferably 135-150 ℃.
The stirring speed in the step (2) is 200-400 r/min, and the stirring time is 0.5-2.0 h.
In the step (3), the stirring speed is 500-800 r/min. The inert gas is preferably N2The inert gas is filled in the reactor in an amount which ensures that the pressure in the reactor is 0.2-0.8 MPa, preferably 0.4-0.8 MPa, and the reaction time is 3-9 h, preferably 5-8 h.
In the step (4), the conditions for shearing the material reacted in the step (3) are as follows: the shearing temperature is 120-160 ℃, the preferred shearing time is 30-200 min, the preferred shearing time is 50-160 min, and the shearing speed is 4000-7000 r/min.
In the step (4), preferably, the substances added before mixing are preheated, wherein the epoxy resin, the curing agent A, the curing agent B and the accelerator are preheated at the preheating temperature of 50-75 ℃, preferably 55-70 ℃, and the preheated temperature of the sheared modified and blended asphalt is 105-130 ℃, preferably 115-125 ℃.
In the step (4), the temperature of the mixed shearing is 110-120 ℃, the time of the shearing is 10-30 min, preferably 15-30 min, and the speed of the shearing is 3000-8000 r/min, preferably 5000-8000 r/min.
Compared with the prior art, the modified epoxy asphalt and the preparation method thereof have the following advantages:
(1) the asphalt adopted by the modified epoxy asphalt is modified mixed asphalt which is matched with epoxy resin, cyclodextrin, an accelerant and a curing agent, and the compatibility of the modified epoxy asphalt can be obviously improved. Two kinds of special-composition matrix asphalt are selected and blended under the action of a modifier polyphosphoric acid, and different components of the two kinds of asphalt are mutually influenced, so that the preparation of the high-compatibility modified epoxy asphalt is facilitated.
(2) The cyclodextrin is introduced into an asphalt system to further modify the modified blended asphalt. The cyclodextrin molecule has an 'inner hydrophobic and outer hydrophilic' structure and a 'cone barrel' structure with narrow top and wide bottom, the inner hydrophobic structure can perform chemical reaction with specific modified harmonic asphalt, the outer hydrophilic structure can react with epoxy resin, the modified harmonic asphalt and the epoxy resin are in mutual contact with each other, the compatibility modification of the modified harmonic asphalt and the epoxy resin is effectively improved, and the two are guaranteed not to be layered after being stored for a long time.
(3) The modifier cyclodextrin used in the invention is a natural macromolecular substance, is harmless to human bodies, does not need to use a large amount of organic solvent in the modification process, does not generate polluting substances, is safe and environment-friendly in the whole modification process, and is simple to operate and easy to control reaction conditions.
Drawings
FIG. 1 is a fluorescent image of the upper and lower sections of modified epoxy asphalt A33 prepared in example 3 after being stored for 4 hours;
FIG. 2 is a fluorescent image of the upper and lower sections of modified epoxy asphalt B22 prepared in comparative example 2 after being stored for 4 hours;
FIG. 3 is a fluorescent image of the upper and lower sections of modified epoxy asphalt B44 prepared in comparative example 4 after being stored for 4 hours;
in each figure, the reference numeral (a) is an upper fluorescent image, and the reference numeral (b) is a lower fluorescent image.
Detailed Description
The technical features of the present invention are further described below by way of examples, but these examples are not intended to limit the present invention, and wt% referred to is mass fraction.
Example 1
(1) Preheating 60 parts by weight of base asphalt I (the saturated component accounts for 25.4wt%, the aromatic component accounts for 29.5wt%, the colloid accounts for 44.9wt%, and the asphaltene accounts for 0.2 wt%) and 40 parts by weight of base asphalt II (the saturated component accounts for 28.6wt%, the aromatic component accounts for 36.4wt%, the colloid accounts for 19.2wt%, and the asphaltene accounts for 15.8 wt%) to a flowing state, mixing, and stirring at 140 ℃ for 4 hours at a stirring speed of 300 r/min to obtain mixed asphalt; and then slowly adding 0.2 part by weight of polyphosphoric acid, continuously heating to 160 ℃, adjusting the stirring speed to 500r/min, and stirring for 6 hours to obtain the modified harmonic asphalt a 1.
(2) Pouring 100 parts by weight of modified and mixed asphalt a1 heated to a flowing state into a high-pressure reaction kettle, adjusting the temperature in the kettle to be 110 ℃, stirring at a speed of 300 r/min, and continuously stirring for 0.5h after the temperature is constant; slowly adding 4 parts by weight of beta-cyclodextrin into a reaction kettle within 1 hour, raising the temperature to 135 ℃ at a speed of 0.5 ℃/min, stirring at a speed of 300 r/min in the adding process, and continuously stirring for 0.5 hour after the temperature is constant;
(3) slowly adding 0.4 weight part of dicumyl peroxide into the reaction kettle, readjusting the stirring speed to 600r/min after the addition is finished, and filling N into the reaction kettle when the pressure in the reaction kettle is kept unchanged2Keeping the pressure constant at 0.5 MPa, and reacting for 5 hours under the condition;
(4) slowly releasing pressure after the reaction is finished, pouring out the material reacted in the step (3), shearing the material at a high speed by a shearing machine, wherein the shearing temperature is 140 ℃, the shearing time is 60min, the shearing speed is 5000r/min, preheating to 120 ℃,
i) half weight of the preheated asphalt material is taken and mixed with 20 weight parts of E-51 bisphenol A epoxy resin heated to 60 ℃, 4 weight parts of m-phenylenediamine, 20 weight parts of methyl tetrahydrophthalic anhydride and 0.125 weight part of triethanolamine, and the mixture is sheared for 30min by a high-speed shearing machine, wherein the shearing temperature is 120 ℃, and the shearing speed is 6000r/min, so as to obtain the modified epoxy asphalt A11.
ii) the remaining half of the weight of the preheated asphalt mass was taken therefrom and mixed with 20 parts by weight of E-51 bisphenol A epoxy resin heated to 60 ℃ and sheared with a high speed shearing machine at 120 ℃ and a shearing speed of 6000r/min for 30min to obtain test sample A1.
Example 2
(1) Preheating 45 parts by weight of matrix asphalt I (saturated component accounting for 27.1wt%, aromatic component accounting for 32.2wt%, colloid accounting for 40.1wt%, and asphaltene accounting for 0.6 wt%) and 55 parts by weight of matrix asphalt II (saturated component accounting for 26.4wt%, aromatic component accounting for 33.8wt%, colloid accounting for 17.8wt%, and asphaltene accounting for 22.0 wt%) to a flowing state, mixing, and stirring at 150 ℃ for 4 hours at a stirring speed of 300 r/min to obtain mixed asphalt; and then slowly adding 0.3 part by weight of polyphosphoric acid, continuously heating to 170 ℃, adjusting the stirring speed to be 500r/min, and stirring for 6 hours to obtain the modified harmonic asphalt a 2.
(2) Pouring 100 parts by weight of modified and mixed asphalt a2 heated to a flowing state into a high-pressure reaction kettle, adjusting the temperature in the kettle to 120 ℃, stirring at a speed of 300 r/min, and continuously stirring for 0.5h after the temperature is constant; slowly adding 5 parts by weight of beta-cyclodextrin into a reaction kettle within 1.5h, raising the temperature to 135 ℃ at a speed of 0.5 ℃/min, stirring at a speed of 300 r/min in the adding process, and continuously stirring for 0.5h after the temperature is constant;
(3) slowly adding 0.2 weight part of tert-butyl hydroperoxide into the reaction kettle, readjusting the stirring speed to 600r/min after the addition is finished, and filling N into the reaction kettle when the pressure in the reaction kettle is kept unchanged2Keeping the pressure constant at 0.5 MPa, and reacting for 5 hours under the condition;
(4) slowly releasing pressure after the reaction is finished, pouring out the material reacted in the step (3), shearing the material at a high speed by a shearing machine, wherein the shearing temperature is 140 ℃, the shearing time is 60min, the shearing speed is 5000r/min, obtaining the pre-modified asphalt after the shearing is finished, preheating the pre-modified asphalt to 120 ℃,
i) taking half weight of the preheated asphalt material, mixing with 20 weight parts of heated E-51 bisphenol A epoxy resin heated to 60 ℃, 2.5 weight parts of diethylaminopropylamine, 18 weight parts of methyl tetrahydrophthalic anhydride and 0.1 weight part of DMP-30, and shearing for 30min by using a high-speed shearing machine at the shearing temperature of 118 ℃ and the shearing speed of 6000r/min to obtain the modified epoxy asphalt A22.
ii) the remaining half of the weight of the preheated asphalt mass was taken therefrom and mixed with 20 parts by weight of heated E-51 bisphenol A epoxy resin heated to 60 ℃ and sheared with a high speed shearing machine at a shearing temperature of 118 ℃ and a shearing speed of 6000r/min to give test sample A2.
Example 3
(1) Preheating 40 parts by weight of base asphalt I (same as example 2) and 60 parts by weight of base asphalt II (same as example 2) to a flowing state, mixing, and stirring at 150 ℃ for 4h at the stirring speed of 300 r/min to obtain mixed asphalt; and then slowly adding 0.2 part by weight of polyphosphoric acid, continuously heating to 170 ℃, adjusting the stirring speed to be 500r/min, and stirring for 6 hours to obtain the modified harmonic asphalt a 3.
(2) Pouring 100 parts by weight of modified and mixed asphalt a3 heated to a flowing state into a high-pressure reaction kettle, adjusting the temperature in the kettle to 120 ℃, keeping stirring at the speed of 300 r/min, and continuing stirring for 1.5 hours after the temperature is constant; slowly adding 5 parts by weight of beta-cyclodextrin into a reaction kettle within 1.5h, raising the temperature to 135 ℃ at a speed of 0.5 ℃/min, stirring at a speed of 300 r/min in the adding process, and continuously stirring for 0.5h after the temperature is constant;
(3) slowly adding 0.4 weight part of dicumyl peroxide into the reaction kettle, readjusting the stirring speed to 600r/min after the addition is finished, and filling N into the reaction kettle when the pressure in the reaction kettle is kept unchanged2Keeping the pressure constant at 0.6 MPa, and reacting for 6h under the condition;
(4) slowly releasing pressure after the reaction is finished, pouring out the material reacted in the step (3), shearing the material at a high speed by a shearing machine, wherein the shearing temperature is 140 ℃, the shearing time is 60min, the shearing speed is 5000r/min, obtaining the pre-modified asphalt after the shearing is finished, preheating the pre-modified asphalt to 120 ℃,
i) half weight of the preheated asphalt material is taken and mixed with 22.5 weight parts of E-51 bisphenol A epoxy resin, 2.5 weight parts of diethylaminopropylamine, 18 weight parts of methylhexahydrophthalic anhydride and 0.1 weight part of DMP-30 which are heated to 65 ℃, and the mixture is sheared for 20min by a high-speed shearing machine, wherein the shearing temperature is 120 ℃, and the shearing speed is 6000r/min, so that the modified epoxy asphalt A33 is obtained.
ii) the remaining half of the weight of the preheated bituminous material was taken therefrom and mixed with 22.5 parts by weight of E-51 bisphenol A epoxy resin heated to 65 ℃ and sheared with a high speed shearing machine for 20min at a shearing temperature of 120 ℃ and a shearing speed of 6000r/min, giving test sample A3.
Example 4
(1) Preheating 65 parts by weight of base asphalt I (same as example 2) and 35 parts by weight of base asphalt II (same as example 2) to a flowing state, mixing, and stirring at 140 ℃ for 4h at the stirring speed of 400r/min to obtain mixed asphalt; and then slowly adding 0.3 part by weight of polyphosphoric acid, continuously heating to 170 ℃, adjusting the stirring speed to be 500r/min, and stirring for 5 hours to obtain the modified harmonic asphalt a 4.
(2) Pouring 100 parts by weight of modified and mixed asphalt a4 heated to a flowing state into a high-pressure reaction kettle, adjusting the temperature in the kettle to be 110 ℃, stirring at a speed of 200 r/min, and continuing stirring for 1.5 hours after the temperature is constant; slowly adding 4 parts by weight of alpha-cyclodextrin into a reaction kettle within 1.5h, raising the temperature to 145 ℃ at the speed of 1 ℃/min, stirring at the speed of 300 r/min in the adding process, and continuously stirring for 0.5h after the temperature is constant;
(3) slowly adding 0.5 weight part of tert-butyl hydroperoxide into the reaction kettle, readjusting the stirring speed to 600r/min after the addition is finished, and filling N when the pressure in the kettle is kept unchanged2Keeping the pressure constant at 0.5 MPa, and reacting for 7 hours under the condition;
(4) slowly releasing pressure after the reaction is finished, pouring out the material reacted in the step (3), shearing the material at a high speed by a shearing machine, wherein the shearing temperature is 150 ℃, the shearing time is 60min, the shearing speed is 5000r/min, preheating to 120 ℃,
i) taking half weight of preheated asphalt material, mixing with 23 weight parts of E-51 bisphenol A epoxy resin heated to 65 ℃, 4 weight parts of N-aminoethyl piperazine, 16.5 weight parts of tung oil anhydride and 0.125 weight part of DMP-30, and shearing for 25min by using a high-speed shearing machine, wherein the shearing temperature is 115 ℃, and the shearing speed is 6500r/min, so as to obtain the modified epoxy asphalt A44.
ii) the remaining half of the weight of the preheated asphalt mass was taken therefrom and mixed with 23 parts by weight of E-51 bisphenol A epoxy resin heated to 65 ℃ and sheared with a high speed shearer for 25min at a shearing temperature of 115 ℃ and a shearing speed of 6500r/min to give test sample A4.
Comparative example 1
100 parts by weight of base asphalt I (same as in example 1) was heated to 120 ℃ and mixed with 40 parts by weight of E-51 bisphenol A epoxy resin heated to 60 ℃ and sheared with a high-speed shearing machine at 120 ℃ and a shearing speed of 6000r/min for 30 minutes to obtain test sample B1.
100 parts by weight of base asphalt I (same as in example 1) was heated to 120 ℃ and mixed with 40 parts by weight of E-51 bisphenol A epoxy resin heated to 60 ℃, 8 parts by weight of m-phenylenediamine, 40 parts by weight of methyltetrahydrophthalic anhydride and 0.25 part by weight of triethanolamine, and the mixture was sheared with a high-speed shearing machine at 120 ℃ and a shearing speed of 6000r/min for 30 minutes to obtain modified epoxy asphalt B11.
Comparative example 2
Test samples B2 and modified epoxy asphalt B22 were obtained in the same manner as in example 3 except that 40 parts by weight of base asphalt I and 60 parts by weight of base asphalt II were changed to 100 parts of base asphalt I.
Comparative example 3
As in example 3, except that 40 parts by weight of the base asphalt I and 60 parts by weight of the base asphalt II were changed to 100 parts of the base asphalt II, test samples B3 and modified epoxy asphalt B33 were obtained.
Comparative example 4
Test samples B4 and modified epoxy asphalt B44 were obtained as in example 3, except that no alpha-cyclodextrin was added to the preparation formulation.
Test example
The test samples obtained in the examples and the comparative examples were subjected to storage stability tests (similar to the test specification JTG E20-2011 for road engineering asphalt and asphalt mixtures) for different periods of time, and after the tests were finished, the softening point difference and the viscosity ratio of the upper and lower samples were tested, and the comparison results are shown in table 1.
TABLE 1 Upper and lower Properties after storage stabilization of examples and comparative examples
| Test sample | A1 | A2 | A3 | A4 | B1 | B2 | B3 | B4 |
| Softening point difference/DEG C after 4h storage at 163 DEG C | 0.24 | 0 | 0 | 0.10 | 4.63 | 1.63 | 0.92 | 2.57 |
| Viscosity ratio of 120 ℃ after 4h storage at 163 ℃ | 1.0027 | 1.0004 | 1.0002 | 1.0011 | 1.4402 | 1.1147 | 1.0827 | 1.3359 |
| Softening point difference/DEG C after 8h storage at 163 DEG C | 0.61 | 0.10 | 0.04 | 0.12 | 4.91 | 3.51 | 1.62 | 3.81 |
| Viscosity ratio of 120 ℃ after 8h storage at 163 ℃ | 1.0266 | 1.0044 | 1.0010 | 1.0068 | 1.5902 | 1.4421 | 1.1179 | 1.4472 |
The invention detects the compatibility of the modified epoxy asphalt material obtained by the embodiment and the comparative example, and the specific process is as follows: the modified epoxy asphalt A11-A44 obtained in the example and the modified epoxy asphalt B11-B44 obtained in the comparative example are poured into a segregation tube, the segregation tube is placed in an oven at 163 ℃ and is kept still for 4 hours, samples of the upper and lower sections of the segregation tube are taken to prepare sheets, and fluorescent photographs are observed and taken under an Axioskop2plus type fluorescence microscope, so that the epoxy resin of the modified epoxy asphalt A11-A44 is found to have good compatibility in an asphalt phase, and the fluorescent photographs of the upper and lower sections of the modified epoxy asphalt A33 in FIG. 1 can be referred to, and the epoxy resin and the asphalt phase in the modified epoxy asphalt B11-B44 are obviously layered, for example, the fluorescent photographs of the upper and lower sections of the modified epoxy asphalt B22 in FIG. 2 and the fluorescent photograph of the modified epoxy asphalt B44 in.
Claims (19)
1. The modified epoxy asphalt comprises the following raw material components in parts by weight:
modified mixed asphalt: 100 parts of (A);
cyclodextrin: 1-8 parts, preferably 2-6 parts;
initiator: 0.1 to 0.9 part, preferably 0.2 to 0.6 part;
epoxy resin: 35-64 parts, preferably 40-55 parts;
accelerator (b): 0.04-0.6 part;
curing agent A: 5-20 parts of a solvent;
curing agent B: 20-45 parts.
2. The modified epoxy asphalt according to claim 1, characterized in that: the modified blended asphalt comprises the following components in parts by weight:
base asphalt I: 20-70 parts, preferably 30-65 parts;
matrix asphalt II: 30-80 parts, preferably 35-70 parts;
modifying agent: 0.03 to 0.5 part, preferably 0.05 to 0.4 part.
3. The modified epoxy asphalt according to claim 2, characterized in that: the modifier is polyphosphoric acid.
4. The modified epoxy asphalt according to claim 2, characterized in that: the matrix asphalt I: the aromatic asphalt comprises, by mass, 20-30% of saturated components, 25-35% of aromatic components, 30-45% of colloid and 0.1-2% of asphaltene; the matrix asphalt II: the aromatic asphalt comprises, by mass, 15-30% of saturated components, 20-40% of aromatic components, 10-20% of colloid and 15-30% of asphaltene.
5. The modified epoxy asphalt according to claim 1, characterized in that: the cyclodextrin is one or more of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin, and is preferably alpha-cyclodextrin and/or beta-cyclodextrin.
6. The modified epoxy asphalt according to claim 1, characterized in that: the initiator is one or more of dicumyl peroxide, tert-butyl hydroperoxide, benzoyl peroxide and sodium metabisulfite.
7. The modified epoxy asphalt according to claim 1, characterized in that: the epoxy resin is E-44 bisphenol A type epoxy resin and E-51 bisphenol A type epoxy resin, and preferably E-51 bisphenol A type epoxy resin.
8. The modified epoxy asphalt according to claim 1, characterized in that: the accelerant is one or more of DMP-30, triethylamine, triethanolamine, benzyltriethylammonium chloride, resorcinol and m-cresol.
9. The modified epoxy asphalt according to claim 1, characterized in that: the curing agent A is an amine curing agent selected from one or more of low molecular polyamide 651, m-phenylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, low molecular polyamide 650, diethylaminopropylamine, N-aminoethyl piperazine and isophorone diamine; the curing agent B is an anhydride curing agent selected from one or more of maleic anhydride, polyisobutylene succinic anhydride, methyl nadic anhydride, modified methyl nadic anhydride, dodecenyl succinic anhydride, methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, elaeostearic anhydride, polyazelaic anhydride, polyglutamic anhydride, polyazelaic anhydride or hydrolyzed polymaleic anhydride, and preferably one or more of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride and elaeostearic anhydride.
10. A process for producing a modified epoxy asphalt according to any one of claims 1 to 9, comprising the steps of:
(1) preparing modified blended asphalt;
(2) heating the modified blended asphalt prepared in the step (1) to a flowing state, pouring the heated modified blended asphalt into a high-pressure reaction kettle, adjusting the temperature in the kettle, stirring, adding cyclodextrin, carrying out programmed heating, and continuing stirring;
(3) adding an initiator into a high-pressure reaction kettle, stirring, and filling inert gas for reaction;
(4) and (4) shearing the material reacted in the step (3), mixing the sheared material with epoxy resin, a curing agent A, a curing agent B and an accelerator, and shearing to obtain the modified epoxy asphalt.
11. The method of claim 10, wherein: the method for preparing the modified blended asphalt in the step (1) comprises the following steps: preheating the base asphalt I and the base asphalt II to a flowing state, mixing, and stirring under a heating condition to obtain mixed asphalt; and then adding polyphosphoric acid, continuing heating and stirring to obtain the modified blended asphalt.
12. The method of claim 11, wherein: the heating temperature during the preparation of the mixed asphalt is 100-180 ℃, the preferred heating temperature is 120-160 ℃, the stirring time is 1-6 hours, the preferred stirring time is 3-6 hours, and the stirring speed is 200-500 r/min; after the polyphosphoric acid is added, the heating temperature is 120-170 ℃, the preferable temperature is 135-170 ℃, the stirring time is 4-10 hours, and the stirring speed is 300-600 r/min.
13. The method of claim 10, wherein: in the step (2), the temperature in the kettle is adjusted to be 100-120 ℃.
14. The method of claim 10, wherein: in the step (2), the cyclodextrin is added within 0.5-1.5 h, the temperature programming rate is 0.5-1 ℃/min, and the temperature programming rate is 130-160 ℃, preferably 135-150 ℃.
15. The method of claim 10, wherein: the stirring speed in the step (2) is 200-400 r/min, and the stirring time is 0.5-2.0 h; in the step (3), the stirring speed is 500-800 r/min.
16. The method of claim 10, wherein: in the step (3), the inert gas is N2The inert gas is filled in the reactor in an amount which enables the pressure in the reactor to be 0.2-0.8 MPa, preferably 0.4-0.8 MPa, and the reaction time is 3-9 h, preferably 5-8 h.
17. The method of claim 10, wherein: in the step (4), the conditions for shearing the material reacted in the step (3) are as follows: the shearing temperature is 120-160 ℃, the preferred shearing time is 30-200 min, the preferred shearing time is 50-160 min, and the shearing speed is 4000-7000 r/min.
18. The method of claim 10, wherein: in the step (4), all the added substances are preheated, wherein the epoxy resin, the curing agent A, the curing agent B and the accelerator are preheated at the preheating temperature of 50-75 ℃ and preferably 55-70 ℃, and the sheared modified blended asphalt is preheated at the preheating temperature of 105-130 ℃ and preferably 115-125 ℃.
19. The method of claim 10, wherein: in the step (4), the temperature of the mixed shearing is 110-120 ℃, the shearing time is 10-30 min, preferably 15-30 min, and the shearing speed is 3000-8000 r/min, preferably 5000-8000 r/min.
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