CN115433465A - Anhydride modified asphalt and preparation method thereof - Google Patents
Anhydride modified asphalt and preparation method thereof Download PDFInfo
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- CN115433465A CN115433465A CN202110606313.1A CN202110606313A CN115433465A CN 115433465 A CN115433465 A CN 115433465A CN 202110606313 A CN202110606313 A CN 202110606313A CN 115433465 A CN115433465 A CN 115433465A
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- polyphosphoric acid
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- 239000010426 asphalt Substances 0.000 title claims abstract description 73
- 150000008064 anhydrides Chemical class 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 114
- 229920000137 polyphosphoric acid Polymers 0.000 claims abstract description 59
- 239000002893 slag Substances 0.000 claims abstract description 38
- 239000003208 petroleum Substances 0.000 claims abstract description 32
- 229920005989 resin Polymers 0.000 claims abstract description 32
- 239000011347 resin Substances 0.000 claims abstract description 32
- 230000009467 reduction Effects 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 150000008065 acid anhydrides Chemical class 0.000 claims abstract description 12
- 239000003607 modifier Substances 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 56
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 42
- 238000010008 shearing Methods 0.000 claims description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 239000012298 atmosphere Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000004321 preservation Methods 0.000 claims description 18
- 230000035484 reaction time Effects 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 16
- 230000001681 protective effect Effects 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 15
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 11
- 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 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000011261 inert gas Substances 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
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000000084 colloidal system Substances 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- 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 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 3
- CUXYLFPMQMFGPL-UHFFFAOYSA-N (9Z,11E,13E)-9,11,13-Octadecatrienoic acid Natural products CCCCC=CC=CC=CCCCCCCCC(O)=O CUXYLFPMQMFGPL-UHFFFAOYSA-N 0.000 claims description 2
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-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
- CUXYLFPMQMFGPL-SUTYWZMXSA-N all-trans-octadeca-9,11,13-trienoic acid Chemical compound CCCC\C=C\C=C\C=C\CCCCCCCC(O)=O CUXYLFPMQMFGPL-SUTYWZMXSA-N 0.000 claims description 2
- 230000008859 change Effects 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
- 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
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- 125000003118 aryl group Chemical group 0.000 claims 1
- 229930195733 hydrocarbon Natural products 0.000 claims 1
- 150000002430 hydrocarbons Chemical class 0.000 claims 1
- 239000011230 binding agent Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 230000004048 modification Effects 0.000 description 10
- 238000012986 modification Methods 0.000 description 10
- 239000012530 fluid Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 238000005553 drilling Methods 0.000 description 7
- 239000004593 Epoxy Substances 0.000 description 6
- 230000000087 stabilizing effect Effects 0.000 description 4
- 208000012839 conversion disease Diseases 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000000543 intermediate Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000005698 Diels-Alder reaction Methods 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000002897 diene group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002383 tung oil Substances 0.000 description 1
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
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/026—Working-up pitch, asphalt, bitumen by chemical means reaction with organic compounds
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses an anhydride modified asphalt and a preparation method thereof. The invention relates to anhydride modified asphalt, which comprises the following raw material components in parts by weight: poor slag reduction: 100 parts of a binder; acid anhydride modifier: 2 to 10 parts; polyphosphoric acid: 0.1 to 2 parts; initiator: 0.08 to 0.7 portion; and (3) modifying auxiliary agent: 1 to 15 parts; wherein the polyphosphoric acid comprises polyphosphoric acid I and polyphosphoric acid II; the modifying auxiliary agent comprises carbon five petroleum resin and carbon nine petroleum resin. The invention takes the difficult-to-treat inferior slag reduction as the raw material to obtain the acid anhydride modified asphalt with high anhydride conversion rate and good high-low temperature performance.
Description
Technical Field
The invention relates to a modified asphalt material and a preparation method thereof, in particular to anhydride modified asphalt and a preparation method thereof.
Background
The anhydrization modified asphalt is not only a novel modified asphalt material, but also can be used as an intermediate for preparing other special asphalt materials, such as asphalt water-based drilling fluid materials, high-quality epoxy asphalt, polymer modified asphalt with stable storage, electrode materials and the like.
The anhydrization modification is an important link for developing high-quality modified asphalt such as epoxy asphalt, polymer modified asphalt and the like. The modifier such as asphalt and epoxy resin has large difference in solubility parameter, density, dielectric constant and the like, belongs to a thermodynamic incompatible system, nonpolar asphalt is difficult to form a homogeneous phase with a polar modifier, the integral uniformity cannot be achieved, the overall relevant mechanical properties of the material are not completely released, and the polarity of the asphalt after anhydride modification is enhanced, so that the compatibility of the two is promoted. The asphalt drilling fluid system mainly uses oil base, but the oil base drilling fluid has certain defects in the aspects of cost and environmental protection, the water-based cationic drilling fluid is paid more and more attention, and the hydrophilic performance of the asphalt can be improved through the acid anhydride modification, so that a foundation is laid for developing asphalt water-based drilling fluid materials. However, bitumen belongs to a relatively inert system, has poor reactivity with acid anhydride and has low reaction conversion rate. The unreacted anhydride left in the asphalt can cause the mechanical property of the asphalt to be poor, the heated micromolecular anhydride is volatilized to be harmful to human bodies and the environment, the conversion rate is low, the anhydride consumption is increased, and the cost is increased. Therefore, the preparation of the high-conversion-rate anhydride asphalt is very significant.
With the increasing heaviness of crude oil, the yield of vacuum residue is gradually improved, the content of heavy metal, sulfur and the like in the residue are increased, the relative content of saturates and asphaltenes in the residue is increased, the relative content of aromatics and colloids is reduced, the association degree of asphaltenes is increased, the existing form is more complex, and the production difficulty of directly preparing high-grade asphalt from inferior residue is increased. Therefore, it would be a better choice for such increasingly inferior residua if they could be converted via anhydrification to intermediates for the production of new materials.
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 performing maleic anhydride modification on the matrix asphalt, although the compatibility is improved to a certain degree, the conversion rate in the maleic anhydride modification process is very low, and a large amount of acid mist can appear when the asphalt is heated to influence safety and 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 solves the problem of improving compatibility by maleic anhydride modification, and neutralizes and converts unreacted maleic anhydride monomers by adding organic alcohol substances, thereby preventing the pollution of volatilization of the maleic anhydride to the environment. However, the method has the defects of more reactions, difficult control of reaction process, low conversion rate of maleic anhydride monomers and influence on the strength of a later-period curing system due to excessive addition of organic alcohols.
In conclusion, grade A asphalt with better properties is selected when the asphalt is subjected to anhydrization modification by the method, the anhydrization modification method does not have universality on poor-quality residual oil, the overall anhydrization conversion rate of the method is not high, and the prepared anhydrized asphalt has poor low-temperature ductility.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an anhydride modified asphalt and a preparation method thereof. The invention takes the difficult-to-treat inferior slag reduction as the raw material to obtain the acid anhydride modified asphalt with high anhydride conversion rate and good high-low temperature performance.
The invention provides anhydride modified asphalt which comprises the following raw material components in parts by weight:
poor slag reduction: 100 parts of (A);
acid anhydride modifier: 2 to 10 parts, preferably 2 to 8 parts;
polyphosphoric acid: 0.1 to 2 parts, preferably 0.2 to 1.8 parts;
initiator: 0.08 to 0.7 part, preferably 0.15 to 0.7 part;
and (3) a modifying auxiliary agent: 1 to 15 parts, preferably 2 to 10 parts;
wherein the polyphosphoric acid comprises polyphosphoric acid I and polyphosphoric acid II; the modifying auxiliary agent comprises carbon five petroleum resin and carbon nine petroleum resin.
The properties of the poor slag reduction include: the flash point is 241 to 256 ℃, the sulfur content is 2.61 to 3.65wt%, and the saturation component accounts for 26.1 to 37.7 percent, the aroma component accounts for 20.2 to 34.5 percent, the colloid accounts for 18.3 to 24.8 percent, the asphaltene accounts for 21.3 to 30.1 percent, and the asphaltene accounts for 21.3 to 26.0 percent preferably according to mass fraction.
The inferior slag reduction also has the following properties: the carbon residue value is 21-29 wt%, the nitrogen content is 0.14-0.61 wt%, the total content of nickel and vanadium is 320-365 mu g/g, and the condensation index CI is 0.26-0.35.
The poor-quality slag reduction can be tower river slag reduction or other slag reduction meeting the properties, and the poor-quality slag reduction is a fraction with an initial boiling point of more than 425 ℃.
The polyphosphoric acid I is polyphosphoric acid with low phosphoric acid content, and the polyphosphoric acid II is polyphosphoric acid with high phosphoric acid content, wherein the polyphosphoric acid I accounts for 20-50% of the total mass of the polyphosphoric acid, and the polyphosphoric acid II accounts for 50-80% of the total mass of the polyphosphoric acid.
The low-phosphoric-acid-content polyphosphoric acid refers to phosphoric acid (as H) contained in polyphosphoric acid 3 PO 4 Calculated) is 105-125 percent, preferably 110-120 percent.
The high phosphoric acid content polyphosphoric acid refers to phosphoric acid (as H) contained in polyphosphoric acid 3 PO 4 Measured), the mass content is 130-145%, preferably 130-140%.
The initiator is one or more of dicumyl peroxide, tert-butyl hydroperoxide, benzoyl peroxide, sodium metabisulfite, azobisisobutyronitrile, azobisisoheptonitrile and cumene hydroperoxide.
The anhydride modifier is one or more of maleic anhydride, polyisobutylene succinic anhydride, methyl nadic anhydride, modified methyl nadic anhydride, dodecenyl succinic anhydride, eleostearic acid anhydride, polyazelaic anhydride, polyglutamic anhydride, polyazelaic anhydride or hydrolyzed polymaleic anhydride.
In the modifying auxiliary agent, the carbon five petroleum resin accounts for 70-90% of the total mass of the modifying auxiliary agent, and the carbon nine petroleum resin accounts for 10-30% of the total mass of the modifying auxiliary agent.
The average molecular weight of the carbon-penta petroleum resin is 300-2800, preferably 500-2000, the softening point is 60-110 ℃, preferably 65-102 ℃, the ash content is 0.01-0.06 wt%, and the acid value is 0.20-0.40 KOH/g, preferably 0.22-0.36 KOH/g.
The average number average molecular weight of the carbon-nine petroleum resin is 300 to 3000, preferably 1000 to 2900, the softening point is 60 to 140 ℃, preferably 85 to 132 ℃, the ash content is 0.01 to 0.05wt%, and the acid value is 0.19 to 0.37 KOH/g, preferably 0.19 to 0.33 KOH/g.
The invention also provides a preparation method of the anhydride modified asphalt, which comprises the following steps:
(1) Adding the poor slag reduction and the polyphosphoric acid II which are heated to a flowing state into a reaction kettle, heating to a reaction temperature, continuously stirring, reacting under a protective gas, and carrying out heat preservation treatment after the reaction is finished;
(2) Adding polyphosphoric acid I into the material obtained in the step (1), adding an anhydride modifier and an initiator after uniformly stirring, continuously stirring and heating to a reaction temperature, and reacting under a protective gas;
(3) Adding carbon five petroleum resin into the material obtained in the step (2), stirring, changing the temperature to the reaction temperature, and reacting under protective gas;
(4) And (4) adding carbon-nine petroleum resin into the material obtained in the step (3), carrying out high-speed shearing in an air atmosphere, and then stirring to obtain the final anhydride modified asphalt.
In the step (1), the reaction kettle is a high-pressure reaction kettle, and the initial temperature of the reaction kettle is adjusted to be 120 to 130 ℃.
In the step (1), the heating to the reaction temperature is heating to the reaction temperature by adopting temperature programming, the heating rate is 1 to 3 ℃/min, the reaction temperature is 140 to 180 ℃, and the preferable temperature is 145 to 160 ℃. The reaction time is 3 to 6 hours. The stirring speed is 600 to 800r/min.
In the step (1), the protective gas is inert gas and/or N 2 The amount of the protective gas is such that the pressure in the reaction vessel is maintained at 0.2 to 0.9MPa, preferably 0.4 to 0.8MPa. The heat preservation treatment condition is that the heat preservation is carried out for 10 to 1697 h at the temperature of 120 to 135 ℃.
And (2) adding polyphosphoric acid I, and preferably stirring for 30-50min at a stirring speed of 300-600r/min.
In the step (2), the protective gas is inert gas and/or N 2 . The amount of the protective gas is such that the pressure in the reaction kettle is maintained at 0.3 to 0.9MPa, preferably 0.5 to 0.9MPa. The continuous stirring speed is 600 to 800r/min. The heating to the reaction temperature is heating to the reaction temperature by adopting programmed heating, and the heating rate is 1 to 3 ℃/min. The reaction temperature is 160-180 ℃, and the reaction time is 6-8h.
In the step (3), the protective gas is inert gas and/or N 2 . The amount of the protective gas is such that the pressure in the reaction kettle is maintained at 0.3 to 0.9MPa, preferably 0.5 to 0.9MPa. The stirring speed is 600 to 800r/min. The temperature is changed to the reaction temperature by adopting a program, the temperature change rate is 1 to 3 ℃/min, the reaction temperature is 140 to 165 ℃, and the reaction time is 2 to 4h.
In the step (4), O is contained in the air atmosphere 2 The volume content is maintained at 20-40%.
In the step (4), the shearing rate is 3000-5000 r/min, preferably 3000-4500 r/min, the shearing time is 60-90min, and the required temperature during shearing is 120-180 ℃, preferably 140-160 ℃. The stirring time is 2 to 4 hours, and the stirring speed is 200 to 400r/min.
Compared with the prior art, the anhydride modified asphalt and the preparation method thereof have the following advantages:
(1) The invention adopts inferior slag reduction as a raw material, which is not suitable for producing high-grade road asphalt, such as the tower and river slag reduction with high asphaltene content, special form and extremely poor comprehensive performance. The method adopts the cooperation of the inferior slag reduction, the polyphosphoric acid I and II, the initiator, the anhydride modifier, the carbon five petroleum resin and the carbon nine petroleum resin to obtain the anhydride modified asphalt, has high anhydride conversion rate and excellent high and low temperature performance, can be used as an intermediate for preparing new materials such as epoxy asphalt, drilling fluid asphalt and the like, develops the use of the inferior slag reduction, and improves the added value of the epoxy asphalt, the drilling fluid asphalt and the like.
(2) The polyphosphoric acid I and the polyphosphoric acid II are added step by step, and different reaction conditions are adopted, so that the asphaltene cluster and the chain-shaped light component in the inferior slag reduction can be subjected to targeted adjustment. The component adjustment not only increases the reactive site and contact area of the acid anhydride and the asphalt, so that the Diels-Alder reaction between the acid anhydride and the asphalt is easier to carry out, but also greatly increases the polarity of the surface of the asphaltene, enhances the pi-pi charge transfer effect and the hydrogen bond acting force, and effectively increases the conversion rate of the anhydrization reaction.
(3) The invention also introduces a modification auxiliary agent, wherein the modification auxiliary agent mainly utilizes the diene structure of the carbon-five petroleum resin and is matched with the synergistic effect of the carbon-nine petroleum resin, so that unreacted micromolecular anhydride can be captured, the reaction conversion rate is improved, and the environmental pollution caused by the volatilization of the anhydride is avoided. And through the optimization and limitation of the two components of the modification auxiliary agent, the high-temperature stability and low-temperature ductility of the anhydride modified asphalt are improved, and a foundation is laid for the development of high-quality terminal functional materials.
(4) The method specially optimizes the conditions of the anhydride reaction, ensures the maximization of the reaction conversion rate, has poor properties of the selected raw materials, effectively reduces the production cost, has no volatilization of anhydride in the reaction process, and is harmless to human bodies and environment.
Detailed Description
The technical solution of the present invention is further described by the following examples, which are not intended to limit the scope of the present invention, and the percentages of the following are mass fractions.
In the invention, the conversion rate of the acid anhydride is measured by using a mode of ethanol extraction and sodium hydroxide standard solution titration, and the calculation formula of the conversion rate is as follows:
wherein, C NaOH Molar concentration (mol/L) of NaOH used for titration, V NaOH For the volume of NaOH solution consumed (L), m is taken as the sample mass (g), mtotal is the total mass of reaction products (g), MAH General assembly To add the total mass (g) of the anhydride modifier, MAH Volatilize Is the mass (g) of the anhydride reagent volatilized during the reaction.
Example 1
(1) Adding 100 parts of fluid slag-reducing Tahe (properties shown in Table 1) into a high-pressure reaction kettle at 120 deg.C, stirring, and adding 0.2 part of phosphoric acid (as H) 3 PO 4 Calculated) 135 percent of polyphosphoric acid II is slowly added into the reaction kettle (after the polyphosphoric acid II is added within 3 min), the temperature is increased to 145 ℃ according to the speed program of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is increased 2 Reacting in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5 MPa, and the reaction time is 4h; after the reaction is finished, the mixture is placed in a reaction kettle for heat preservation, the heat preservation temperature is 120 ℃, and the heat preservation time is 10 hours.
(2) 0.1 part of phosphoric acid (in terms of H) 3 PO 4 Calculated) 110 percent of polyphosphoric acid I is added into the slag-reduced tower river after the reaction in the step (1), after the mixture is stirred for 30min uniformly, 4 parts of maleic anhydride and 0.5 part of dicumyl peroxide are added, the temperature is raised to 175 ℃ according to the speed program of 2 ℃/min at the stirring speed of 650r/min, and after the temperature is raised, N is added 2 The reaction is carried out in the atmosphere, the pressure in the reaction kettle is maintained at 0.6 MPa, and the reaction time is 6h.
(3) Adding 1.5 parts of carbon-five petroleum resin (average molecular weight of 1500, ash content of 0.02% and acid value of 0.25 KOH/g) with softening point of 82 ℃ into the slag reduction tower after reaction in the step (2), changing the temperature to 150 ℃ according to the speed program of 2 ℃/min under the stirring speed of 600r/min, stabilizing the temperature, and adding N 2 The reaction is carried out in the atmosphere, the pressure in the reaction kettle is maintained at 0.8MPa, and the reaction time is 2h.
(4) Adding 0.5 part of carbon-nine petroleum resin (average molecular weight 2000, ash content 0.03% and acid value 0.29 KOH/g) with softening point 103 ℃ into the reduced slag of the tower river after the reaction in the step (3), and shearing at 140 ℃ for 60min at the shearing rate of 4000 r/min; stirring for 2h at 140 ℃ after shearing, wherein the stirring speed is 300r/min, and the shearing and stirring processes are performed in the presence of O 2 The volume content is 30 percent, and the acid anhydride is obtained after the stirring is stableFor specific properties of bitumen A1, see Table 2.
Example 2
(1) 100 parts of slag reduction tower river (properties shown in table 1) heated to a flowing state is added into a high-pressure reaction kettle at the temperature of 120 ℃ to be stirred, and 0.25 part of phosphoric acid (expressed as H) is added 3 PO 4 Calculated) 135 percent of polyphosphoric acid II is slowly added into the reaction kettle (after the polyphosphoric acid II is added within 3 min), the temperature is increased to 145 ℃ according to the speed program of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is increased 2 Carrying out reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5 MPa, and the reaction time is 6h; after the reaction is finished, the mixture is placed in a reaction kettle for heat preservation, the heat preservation temperature is 120 ℃, and the heat preservation time is 16 hours.
(2) 0.1 part of phosphoric acid (in terms of H) 3 PO 4 Calculated) 110 percent of polyphosphoric acid I is added into the tower river slag-reduced reaction obtained in the step (1), after stirring for 30min, 4.75 parts of tung oil acid anhydride and 0.6 part of dicumyl peroxide are added, the temperature is programmed to 175 ℃ according to the speed of 2 ℃/min under the stirring speed of 650r/min, and N is added after the temperature is increased 2 The reaction is carried out in the atmosphere, the pressure in the reaction kettle is maintained at 0.8MPa, and the reaction time is 6h.
(3) Adding 2 parts of carbon five petroleum resin (with the same properties as in example 1) with the softening point of 82 ℃ into the slag reduction tower obtained after the reaction in the step (2), changing the temperature to 150 ℃ according to the speed program of 2 ℃/min at the stirring speed of 600r/min, stabilizing the temperature, and adding the mixture into N 2 The reaction is carried out in the atmosphere, the pressure in the reaction kettle is maintained at 0.8MPa, and the reaction time is 2h.
(4) Adding 0.5 part of carbon-nine petroleum resin (the property is the same as that of example 1) with the softening point of 103 ℃ into the slag reduction of the tower river after the reaction in the step (3), and shearing at 140 ℃ for 60min at the shearing rate of 4000 r/min; stirring at 140 deg.C for 2.5h after shearing, with stirring rate of 300r/min, and shearing and stirring in O 2 The reaction is carried out under the environment with the volume content of 30 percent, and the anhydrized asphalt A2 is obtained after the stirring stabilization is finished, and the specific properties are shown in the table 2.
Example 3
(1) 100 portions of the slag reduction of the Tahe heated to a flowing state (properties are shown in Table 1) are addedStirring in a high-pressure reaction kettle at the temperature of 120 ℃, and adding 0.2 part of phosphoric acid (as H) 3 PO 4 Calculated) 135 percent of polyphosphoric acid II is slowly added into the reaction kettle (after the polyphosphoric acid II is added within 3 min), the temperature is increased to 145 ℃ according to the speed program of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is increased 2 Reacting in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5 MPa, and the reaction time is 4h; after the reaction is finished, the mixture is placed in a reaction kettle for heat preservation, the heat preservation temperature is 120 ℃, and the heat preservation time is 10 hours.
(2) 0.2 part of phosphoric acid (in terms of H) 3 PO 4 Calculated) 110 percent polyphosphoric acid I is added into the tower river slag-reduced slag reacted in the step (1), after stirring for 30min, 5 parts of maleic anhydride, 0.5 part of dicumyl peroxide and 0.1 part of azobisisobutyronitrile are added, the temperature is programmed to 180 ℃ at the stirring speed of 650r/min according to the speed of 2 ℃/min, and after the temperature is increased, N is added 2 The reaction is carried out in the atmosphere, the pressure in the reaction kettle is maintained at 0.6 MPa, and the reaction time is 6h.
(3) Adding 1.5 parts of carbon five petroleum resin (average molecular weight of 1650, ash content of 0.02% and acid value of 0.26 KOH/g) with softening point of 90 deg.C into the residue of the tower river obtained in step (2), changing temperature to 150 deg.C at stirring speed of 600r/min according to speed program of 2 deg.C/min, stabilizing temperature, and adding into N 2 The reaction is carried out in the atmosphere, the pressure in the reaction kettle is maintained at 0.8MPa, and the reaction time is 2h.
(4) Adding 0.5 part of carbon-nine petroleum resin (with average molecular weight of 2200, ash content of 0.03% and acid value of 0.24 KOH/g) with softening point of 112 ℃ into the slag-reduced tower river obtained after the reaction in the step (3), and shearing at 140 ℃ for 60min at a shearing rate of 4000 r/min; stirring for 2h at 140 ℃ after shearing, wherein the stirring speed is 300r/min, and the shearing and stirring processes are performed in the presence of O 2 The reaction is carried out under the environment with the volume content of 30 percent, and the anhydrized asphalt A3 is obtained after the stirring stabilization is finished, and the specific properties are shown in the table 2.
Example 4
(1) Adding 100 parts of fluid slag-reducing Tahe (properties shown in Table 1) into a high-pressure reaction kettle at 125 deg.C, stirring, and adding 0.4 part of phosphoric acid(with H) 3 PO 4 Calculated) 140 percent of polyphosphoric acid II is slowly added into the reaction kettle (the addition is finished within 5 min), the temperature is raised to 160 ℃ according to the speed program of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature rise is finished 2 Carrying out reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5 MPa, and the reaction time is 6h; after the reaction is finished, the mixture is placed in a reaction kettle for heat preservation, the heat preservation temperature is 120 ℃, and the heat preservation time is 16 hours.
(2) 0.3 part of phosphoric acid content (as H) 3 PO 4 Calculated) 110 percent polyphosphoric acid I is added into the tower river slag-reduced slag reacted in the step (1), after stirring for 30min, 4.75 parts of maleic anhydride, 0.5 part of dicumyl peroxide and 0.2 part of benzoyl peroxide are added, the temperature is raised to 175 ℃ according to the speed program of 2 ℃/min under the stirring speed of 700r/min, and after the temperature is raised, N is added 2 The reaction is carried out in the atmosphere, the pressure in the reaction kettle is maintained at 0.6 MPa, and the reaction time is 8h.
(3) Adding 3 parts of carbon-five petroleum resin (average molecular weight is 1500, ash content is 0.02%, acid value is 0.22 KOH/g) with softening point of 80 ℃ into the tower slag reduction after reaction in the step (2), changing the temperature to 150 ℃ according to the speed program of 2 ℃/min under the stirring speed of 600r/min, stabilizing the temperature, and adding N 2 The reaction is carried out in the atmosphere, the pressure in the reaction kettle is maintained at 0.8MPa, and the reaction time is 2h.
(4) Adding 0.5 part of carbon-nine petroleum resin (average molecular weight of 2050, ash content of 0.03% and acid value of 0.29 KOH/g) with softening point of 105 ℃ into the slag removed from the tower river after the reaction in the step (3), and shearing at 140 ℃ for 60min at the shearing rate of 4000 r/min; stirring for 4h at 140 ℃ after shearing, wherein the stirring speed is 300r/min, and the shearing and stirring processes are performed in the presence of O 2 The reaction is carried out under the environment with the volume content of 30 percent, and the anhydrized asphalt A4 is obtained after the stirring stabilization is finished, and the specific properties are shown in the table 2.
Comparative example 1
100 parts of slag reduction tower river (properties are shown in table 1) heated to a flowing state is added into a high-pressure reaction kettle at the temperature of 125 ℃ for stirring, 4 parts of maleic anhydride is added after the mixture is uniform, and the stirring speed is 650r/min, and the speed process is 2 ℃/minHeating to 175 ℃ sequentially, and heating to N 2 And (3) carrying out reaction in the atmosphere, maintaining the pressure in the reaction kettle at 0.6 MPa for 6h, and obtaining the anhydride asphalt B1 after the reaction is finished.
Comparative example 2
Adding 100 parts of tower river slag (properties shown in table 1) heated to a flowing state into a high-pressure reaction kettle at 125 ℃, stirring, adding 4 parts of maleic anhydride and 0.5 part of dicumyl peroxide after the mixture is uniform, raising the temperature to 175 ℃ according to a speed program of 2 ℃/min at a stirring speed of 650r/min, and after the temperature is raised, adding N 2 And (3) carrying out reaction in the atmosphere, maintaining the pressure in the reaction kettle at 0.6 MPa, and reacting for 6h to obtain the anhydride asphalt B2 after the reaction is finished.
Comparative example 3
Same as example 1, except that the phosphoric acid content (as H) of 0.2 part was not added during the preparation 3 PO 4 Calculated as H) of 135% of polyphosphoric acid II, 0.1 part of phosphoric acid 3 PO 4 Calculated) was 110% polyphosphoric acid I. The anhydrified asphalt obtained in this comparative example was B3.
Comparative example 4
The same as example 1 except that 1.5 parts of carbon five petroleum resin having a softening point of 82 ℃ and 0.5 part of carbon nine petroleum resin having a softening point of 103 ℃ were not introduced during the preparation. This comparative example gave an anhydrified bitumen of B4.
Comparative example 5
Same as example 1, except that 0.2 part of phosphoric acid (as H) was not added during the preparation 3 PO 4 Calculated as H) of 135% of polyphosphoric acid II, and a phosphoric acid content (calculated as H) 3 PO 4 Calculated) was changed to 0.3 part of polyphosphoric acid I of 110%. The anhydrified asphalt obtained in this comparative example was B5.
Comparative example 6
The same as example 1, except that 1.5 parts of carbon five petroleum resin with a softening point of 82 ℃ is not introduced in the preparation process, and the addition amount of the carbon nine petroleum resin is changed to 2.0 parts. The anhydrified asphalt obtained in this comparative example was B6.
Test example
The anhydride asphalts from the examples and comparative examples were tested for conversion and for criticality (according to road engineering asphalt and asphalt test protocol JTG E20-2011) and the relevant properties are shown in table 2.
TABLE 1 properties of slag reduction of Tahe used in examples and comparative examples
| Carbon residue value/wt% | 27.8 |
| Carbon content/wt% | 89.13 |
| Nitrogen content/wt% | 0.14 |
| Hydrogen content/wt% | 7.44 |
| Sulfur content/wt.% | 3.13 |
| Total content of nickel and vanadium/ug/g | 337 |
| Saturated fraction/%) | 30.17 |
| Fraction of aroma/%) | 28.11 |
| Gum/% of | 17.73 |
| Asphaltene/% | 23.99 |
| Condensation index CI | 0.31 |
| Colloid instability index Ic | 1.18 |
| Penetration at 25 deg.C/0.1 mm | 51 |
| Penetration index (five points) | 1.81 |
| 25 ℃ ductility/cm | 62.4 |
| Softening Point/. Degree C | 57.8 |
| Flash point/. Degree.C | 253 |
| Dynamic viscosity (60 ℃) Pa.s | 1680 |
TABLE 2 Properties of acid anhydride-modified asphalts obtained in examples and comparative examples
| Modified asphaltBlue number | Penetration/0.1 mm at 25 ℃ | Softening Point/. Degree C | 25 ℃ ductility/cm | Conversion rate% |
| A1 | 31 | 75.1 | 18.8 | 84.92 |
| A2 | 33 | 70.7 | 16.2 | 81.01 |
| A3 | 29 | 75.4 | 18.1 | 85.27 |
| A4 | 26 | 76.2 | 20.9 | 87.04 |
| B1 | 38 | 65.7 | 2.8 | 56.03 |
| B2 | 34 | 66.2 | 0 | 60.22 |
| B3 | 32 | 70.1 | 6.9 | 72.14 |
| B4 | 35 | 65.9 | 4.4 | 75.39 |
| B5 | 33 | 68.9 | 7.1 | 72.47 |
| B6 | 35 | 67.1 | 4.2 | 76.02 |
The scope of the present invention is not limited by the above-described embodiments, but is defined by the claims. Those skilled in the art can appropriately modify the embodiments without departing from the technical spirit and scope of the present invention, and the modified embodiments are also included in the scope of the present invention.
Claims (17)
1. The anhydride modified asphalt comprises the following raw material components in parts by weight:
poor slag reduction: 100 parts of (A);
acid anhydride modifier: 2 to 10 parts, preferably 2 to 8 parts;
polyphosphoric acid: 0.1 to 2 parts, preferably 0.2 to 1.8 parts;
initiator: 0.08 to 0.7 part, preferably 0.15 to 0.7 part;
and (3) a modifying auxiliary agent: 1 to 15 parts, preferably 2 to 10 parts;
wherein the polyphosphoric acid comprises polyphosphoric acid I and polyphosphoric acid II; the modifying auxiliary agent comprises carbon five petroleum resin and carbon nine petroleum resin.
2. The acid-denatured asphalt according to claim 1, wherein: the inferior slag reduction property comprises: the flash point is 241 to 256 ℃, the sulfur content is 2.61 to 3.65wt%, the saturation component accounts for 26.1 to 37.7 percent, the aromatic component accounts for 20.2 to 34.5 percent, the colloid accounts for 18.3 to 24.8 percent, the asphaltene accounts for 21.3 to 30.1 percent, and the asphaltene accounts for 21.3 to 26.0 percent.
3. The acid-denatured asphalt according to claim 2, wherein: the inferior slag reduction also has the following properties: the carbon residue value is 21-29 wt%, the nitrogen content is 0.14-0.61 wt%, the total content of nickel and vanadium is 320-365 mu g/g, and the condensation index CI is 0.26-0.35.
4. The anhydride-modified asphalt according to claim 1, wherein: the polyphosphoric acid I is polyphosphoric acid with low phosphoric acid content, and the polyphosphoric acid II is polyphosphoric acid with high phosphoric acid content, wherein the polyphosphoric acid I accounts for 20-50% of the total mass of the polyphosphoric acid, and the polyphosphoric acid II accounts for 50-80% of the total mass of the polyphosphoric acid.
5. The acid-denatured asphalt according to claim 4, wherein: the low-phosphoric-acid-content polyphosphoric acid refers to phosphoric acid contained in polyphosphoric acid and H 3 PO 4 The mass content is 105-125%, preferably 110-120%; the high phosphoric acid content polyphosphoric acid refers to polyphosphoric acid contained in polyphosphoric acidPhosphoric acid with H 3 PO 4 The mass content is 130-145%, preferably 130-140%.
6. The anhydride-modified asphalt according to claim 1, wherein: the initiator is one or more of dicumyl peroxide, tert-butyl hydroperoxide, benzoyl peroxide, sodium metabisulfite, azobisisobutyronitrile, azobisisoheptonitrile and cumene hydroperoxide.
7. The acid-denatured asphalt according to claim 1, wherein: the anhydride modifier is one or more of maleic anhydride, polyisobutylene succinic anhydride, methyl nadic anhydride, modified methyl nadic anhydride, dodecenyl succinic anhydride, eleostearic acid anhydride, polyazelaic anhydride, polyglutamic anhydride, polyazelaic anhydride or hydrolyzed polymaleic anhydride.
8. The acid-denatured asphalt according to claim 1, wherein: in the modifying auxiliary agent, the carbon five petroleum resin accounts for 70-90% of the total mass of the modifying auxiliary agent, and the carbon nine petroleum resin accounts for 10-30% of the total mass of the modifying auxiliary agent.
9. The process for producing an acid-denatured asphalt according to any of claims 1 to 8, characterized in that: the method comprises the following steps:
(1) Adding the inferior slag reduction and polyphosphoric acid II which are heated to a flowing state into a reaction kettle, heating to a reaction temperature, continuously stirring, reacting under a protective gas, and carrying out heat preservation treatment after the reaction is finished;
(2) Adding polyphosphoric acid I into the material obtained in the step (1), stirring uniformly, adding an anhydride modifier and an initiator, continuously stirring and heating to a reaction temperature, and reacting under a protective atmosphere;
(3) Adding hydrocarbon petroleum resin into the material obtained in the step (2), stirring, changing the temperature to the reaction temperature, and reacting under protective gas;
(4) And (4) adding carbon-nine petroleum resin into the material obtained in the step (3), carrying out high-speed shearing in an air atmosphere, and then stirring to obtain the final anhydride modified asphalt.
10. The method of claim 9, wherein: in the step (1), the reaction kettle is a high-pressure reaction kettle, and the initial temperature of the reaction kettle is adjusted to be 120-130 ℃.
11. A method according to claim 9 or 10, characterized by: in the step (1), the heating to the reaction temperature is heating to the reaction temperature by adopting temperature programming, the heating rate is 1 to 3 ℃/min, the reaction temperature is 140 to 180 ℃, and the reaction time is 3 to 6h.
12. A method according to claim 9 or 10, characterized by: in the step (1), the protective gas is inert gas and/or N 2 The amount of the protective gas enables the pressure in the reaction kettle to be maintained at 0.2 to 0.9MPa; the heat preservation treatment condition is that the heat preservation is carried out for 10 to 1697 h at the temperature of 120 to 135 ℃.
13. The method of claim 9, wherein: in the step (2) and the step (3), the protective gas is inert gas and/or N 2 (ii) a The amount of the protective gas ensures that the pressure in the reaction kettle is maintained to be 0.3 to 0.9MPa.
14. A method according to claim 9 or 13, characterized by: in the step (2), heating to the reaction temperature is heating to the reaction temperature by adopting programmed heating, and the heating rate is 1 to 3 ℃/min; the reaction temperature is 160-180 ℃, and the reaction time is 6-8h.
15. The method of claim 9, wherein: in the step (3), the temperature is changed to the reaction temperature by adopting a program, the temperature change rate is 1 to 3 ℃/min, the reaction temperature is 140 to 165 ℃, and the reaction time is 2 to 4h.
16. According to claimThe method of claim 9, wherein: in the step (4), O is contained in the air atmosphere 2 The volume content is maintained at 20-40%.
17. A method according to claim 9 or 16, characterized by: in the step (4), the shearing speed is 3000-5000 r/min, the shearing time is 60-90min, the temperature required during shearing is 120-180 ℃, the stirring time is 2-4h, and the stirring speed is 200-400r/min.
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| CN112210221A (en) * | 2019-07-10 | 2021-01-12 | 中国石油化工股份有限公司 | Epoxy asphalt material and preparation method thereof |
| CN112210222A (en) * | 2019-07-10 | 2021-01-12 | 中国石油化工股份有限公司 | Epoxy asphalt material for roads and bridges and preparation method thereof |
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| CN108165036A (en) * | 2018-01-16 | 2018-06-15 | 苏州拓博琳新材料科技有限公司 | A kind of modified asphalt composite of low temperature performance excellent and preparation method thereof |
| CN112210221A (en) * | 2019-07-10 | 2021-01-12 | 中国石油化工股份有限公司 | Epoxy asphalt material and preparation method thereof |
| CN112210222A (en) * | 2019-07-10 | 2021-01-12 | 中国石油化工股份有限公司 | Epoxy asphalt material for roads and bridges and preparation method thereof |
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