CN104559234A - Asphalt viscosity reducer and asphalt composition - Google Patents
Asphalt viscosity reducer and asphalt composition Download PDFInfo
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- CN104559234A CN104559234A CN201310496030.1A CN201310496030A CN104559234A CN 104559234 A CN104559234 A CN 104559234A CN 201310496030 A CN201310496030 A CN 201310496030A CN 104559234 A CN104559234 A CN 104559234A
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Abstract
The invention discloses asphalt viscosity reducer and asphalt composition. The asphalt viscosity reducer comprises the following components in percentage by weight: 5-30% of an additive A, 1-10% of an additive B, 1-10% of kaloamine and 50-93% of an additive C. The components are uniformly mixed in a proportion, then the asphalt viscosity reducer is obtained, and the asphalt viscosity reducer is mixed with matrix asphalt to obtain the asphalt composition. The asphalt viscosity reducer has a good viscosity reduction function on asphalt, and the asphalt composition with the asphalt viscosity reducer has low high-temperature viscosity, good lubrication performance and good viscosity and ductility at 60 DEG C, meanwhile has the needle penetration and softening point the same as those of the base asphalt, and has the advantages of low production cost, simple and convenient preparation method, wide application range and the like.
Description
Technical field
The present invention relates to a kind of asphalt viscosity reduction agent and use the bituminous composition of this viscosity-depression agent.
Background technology
The asphalt used in current road engineering is generally divided into two types according to mixing and stirring construction temperature: cold-mix asphalt compound CMA (Cold Mix Asphalt) and hot-mix asphalt mixture HMA (Hot Mix Asphalt).Cold-mix asphalt compound generally adopt emulsified bitumen or eu-bitumen and gather materials to mix and stir under normal temperature state, making, without the need to to gather materials and binder heats, can mass energy be saved like this.But cold-mix asphalt compound initial stage pavement performance is poor, be difficult to the requirement meeting the important engineering such as motorway, Heavy Traffic road.Hot-mix asphalt mixture be most widely used, a kind of compound that pavement performance is the best.But in hot-mix asphalt mixture production process, pitch and building stones need to mix and stir under 150 ~ 180 DEG C of hot conditionss.By building stones, asphalt heating to so high temperature, consume mass energy.A large amount of CO is created in addition in hot-mix asphalt mixture production process
2, flue dust and obnoxious flavour (CO, SO
2, NO
xdeng), not only pollute environment, and have impact on the healthy of staff.Meanwhile, mixing and stirring under hot conditions also result in the aging of pitch, reduces the pavement performance of asphalt.
For protection of the environment, save energy; the research of Warm-Mix Bitumen Mixture WMA (Warm Mix Asphalt) has been carried out in countries such as the middle and later periods nineties 20th century Europe and the U.S.; its objective is by reducing mixing and stirring and paving material of asphalt; reach the energy consumption reduced in Process of Pitch Mixture Production, reduce CO
2deng gas and dust discharge amount, ensure that Warm-Mix Bitumen Mixture has the pavement performance substantially identical with hot-mix asphalt mixture and construction workability simultaneously.
At present, warm mix asphalt technologies mainly contains three kinds of modes: one is in pitch, add a kind of additive that can reduce pitch 135 DEG C of viscosity in advance, chemically angle changes the viscosity-temperature curve of pitch, thus reduce pitch and building stones mix and stir temperature, but namely 60 DEG C of viscosity that this method also can reduce pitch usually reduce the high-temperature stability of compound; Two is the emulsified bitumens adopting solid content higher, and mix and stir with building stones at 80 ~ 120 DEG C of temperature, which is low compared with the temperature of hot asphalt about 30 ~ 50 DEG C; Three is when mixing compound, water and pitch are added simultaneously to mix and stir in tank, because the existence of water makes asphalt foaming, reaches viscosity reducing effect.If but the method amount of water is excessive, then can produce a large amount of water vapour or cause bumping, if the water yield is very few, then foaming effect is bad.
CN102311649A discloses a kind of asphalt viscosity reduction modifier and preparation method thereof.A certain proportion of activator, ammonium silicofluoride, creosote, polyethylene and stearic acid are put in reaction vessel by the method, are warming up to 250 DEG C, and abundant stirring reaction obtains asphalt viscosity reduction modifier.The method take creosote as medium, and at high temperature, ammonium silicofluoride and stearic acid react, generate a kind of new compound, this compound plays viscosity reduction effect to pitch, can reduce construction temperature, bituminous concrete compactness can be significantly improved simultaneously, improve the high-temperature behavior of pitch.But ammonium silicofluoride itself is poisonous, has strong and stimulating, high temperature easily decomposes and give off poisonous gas, and at high temperature reacts with stearic acid, releases poisonous corrosive fume.
CN102532920A discloses a kind of Warm mixed asphalt cement and preparation method thereof.The method is that a certain proportion of bituminous cements is heated to 130 ~ 160 DEG C, adds a certain proportion of rheology modifier, stirs; Again high molecular polymer is added mixed system in batches, shear, stir until polymer beads is evenly distributed on < 100 micrometer range, be slowly warming up to 170 ~ 180 DEG C, stirring reaction takes the dish out of the pot for 1 ~ 2 hour.The method can improve the high temperature rut of bituminous cements, low temperature stretch-proof and resistance to embrittlement performance, and has lower viscosity under 110 ~ 135 DEG C of conditions, can still have good mix, pave, compaction capacity under reduction construction temperature.But need when preparing Warm mixed asphalt cement repeatedly to feed in raw material, stir and heat up, and need stir for a long time for 1 ~ 2 hour when mix, be difficult in industrial production make polymer beads control at < 100 micrometer range, preparation method is complicated, production cost is high, needs carry out scrap build and change Production Flow Chart, and the production process cycle is longer, the needs that scene paves cannot be adapted to, be difficult to realize industry and amplify and application.
CN101781468A discloses a kind of modified asphalt viscosity decreasing agent and preparation method thereof.The method, after being dewatered at 100 ~ 120 DEG C by compatilizer, adds organic acid, tensio-active agent and synthesis paraffin, in temperature be blended in the screw extrusion press of 80 ~ 100 DEG C, extrude, granulation, cooling obtain asphalt viscosity reduction agent.This viscosity-depression agent can reduce modifying asphalt 175 DEG C of viscosity; Synthesis paraffin in this viscosity-depression agent belongs to non-elastic material, easily brittle failure under cryogenic, thus cause the low temperature stretch-proof of asphalt and resistance to embrittlement degradation, and organic wax of most of low melting point is while reduction asphalt high-temperature viscosity, also reduce 60 DEG C of viscosity, reduce anti-rut behavior.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of asphalt viscosity reduction agent and bituminous composition.Asphalt viscosity reduction agent of the present invention has good viscosity reduction effect to pitch, the bituminous composition adding viscosity-depression agent of the present invention has lower high temperature viscosity and good oilness, 60 DEG C of higher viscosity and ductility, there is the penetration degree suitable with matrix pitch and softening temperature simultaneously, there is production cost low, the advantages such as preparation method is easy and have wide range of applications.
Asphalt viscosity reduction agent of the present invention, by weight percentage, comprises following component:
Additive A: 5wt% ~ 30wt%;
Additive B: 1wt% ~ 10wt%;
Carlow amine: 1wt% ~ 10wt%;
Addition of C: 50wt% ~ 93wt%;
Asphalt viscosity reduction agent of the present invention, preferably composition comprises by weight percentage:
Additive A: 10wt% ~ 20wt%;
Additive B: 2wt% ~ 5wt%;
Carlow amine: 2wt% ~ 5wt%
Addition of C: 70wt% ~ 86wt%;
Described additive A, fusing point is between 60 ~ 130 DEG C, comprise: one or more in polyethylene wax, Microcrystalline Wax, montanin wax, sasobit, sulphur, stearic acid, arachic acid, Lignoceric acid etc. and derivative thereof, preferably polyethylene wax and/or stearic acid.
Described additive B is high molecular component, comprise in polyethylene oxide-propylene oxide, resol, polyacrylic ester, aminoresin, polyethers, polyvinyl alcohol and partial esterification thereof or acetalation product one or more, optimization polypropylene acid esters and/or aminoresin, molecular weight all 1000 ~ 30000, preferably 2000 ~ 20000.
Described addition of C is low-molecular-weight component, comprise fatty acid distribution of coconut oil diglycollic amide, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, alkylol amide Soxylat A 25-7, Block polyoxyethylene-polyethenoxy ether, alkyl polyglycoside, polyvalent alcohol stearate, Span, fatty acid ethylene oxide condensate, castor oil polyoxyethylene ether, one or more in polyoxyethylene glycol dioleic acid ester and Spans series and the esterification of Tweens series and etherification product, preferred fat polyoxyethylenated alcohol, one or more in alkylol amide Soxylat A 25-7 and fatty acid distribution of coconut oil diglycollic amide, its molecular weight is all below 1000.
In asphalt viscosity reduction agent of the present invention, can need to add organic additive according to practical application, comprise ethyl diazoacetate, Cellmic C 121, N, N-dinitrosopentamethlyene tetramine and Diisopropyl azodicarboxylate etc.
In asphalt viscosity reduction agent of the present invention, also can need to add other properties-correcting agent according to practical application, as antistripping agent, antiaging agent, antioxidant, dispersion agent, stablizer, polymer modifiers etc.
The preparation method of asphalt viscosity reduction agent of the present invention, comprises following content: by proportioning, additive A, additive B, Carlow amine and addition of C are added reaction vessel respectively, mix, make asphalt viscosity reduction agent; Wherein mixing temperature is 60 ~ 130 DEG C, by higher than or close to the fusing point of use binder component or softening temperature, mixing time is 20 ~ 30 minutes, and mixing process adopts conventional mechanical stirring.
Bituminous composition of the present invention, comprises matrix pitch and above-mentioned asphalt viscosity reduction agent, and with matrix pitch weight for benchmark, viscosity-depression agent is the 0.1wt% ~ 5wt% of matrix pitch, is preferably 0.5wt% ~ 3wt%.
In bituminous composition of the present invention, described matrix pitch is one or more in straight-run pitch, oxidized bitumen and solvent deoiling pitch, and its penetration degree is 60 ~ 120 1/10mm.
The preparation method of bituminous composition of the present invention, comprises following content: add in matrix pitch by proportioning by above-mentioned asphalt viscosity reduction agent, mix, obtain bituminous composition; Wherein mixing temperature is 130 ~ 150 DEG C, and mixing time is 30 ~ 60 minutes; Mixing process adopts general mechanical stirring mode, also can adopt ultrasonic, the technique means such as microwave or high-shear.
The application of bituminous composition of the present invention in urban road laying, maintenance and building, particularly has broad application prospects in the compound of road bitumen mixes and stirs.
The application of bituminous composition of the present invention in asphalt, comprises following content: mix and stir temperature when building stones reach, and adds uniform mixing in bituminous composition to compound.
Bituminous composition of the present invention compares with traditional hot asphalt, has the following advantages:
(1) in bituminous composition of the present invention, each component is 120 ~ 165 DEG C time, there is good consistency and mobility, more obvious viscosity reduction effect is all had to matrix pitch, four kinds of component synergies, dispersion effect is good, good stability, significantly " lubrication " effect can be played, effectively can improve the construction workability of asphalt.
(2) in bituminous composition of the present invention, the synergy of each component also produces following beneficial effect: when additive A independently exists under cryogenic, be present in pitch with not homogeneous phase crystalline state, larger with the physico-chemical property difference of matrix pitch, consistency is bad, while reduction asphalt high-temperature viscosity, also reduce its 60 DEG C of viscosity, reduce anti-rut behavior.When adding additive B (high molecular component) and addition of C (low-molecular-weight component), the mobility good due to it and consistency, can be dispersed by heterogeneous crystallization during stirring, macromole in additive B and pitch is by this lubrication crystal grain parcel and be mutually wound around, form the more stable colloidal dispersion with spacial framework, improve its 60 DEG C of viscosity, improve high temperature rutting resistance.Carlow amine and other three kinds of components act synergistically, and can play solubilising, stable, viscosity reduction and lubricant effect, and Carlow amine contribute to the bonding force increasing pitch and building stones.
(3) bituminous composition of the present invention, there is lower high temperature viscosity and better oilness, therefore can reduce the mixing and stirring of asphalt, pave and compacting temperature, it mixes and stirs temperature can reduce by 15 ~ 30 DEG C than hot asphalt, reduce energy consumption about 30%, a large amount of minimizing is mixed and stirred and smog in construction process and discharge of poisonous waste, reduces harm and environmental pollution.
(4) bituminous composition of the present invention, while effectively reducing high temperature viscosity, 60 DEG C of higher viscosity can be kept, the cohesive force of building stones, stone flour and pitch can be increased well, improve the stripper-resistance of compound, effectively can prevent the Rutting damage of bituminous pavement under heavy traffic and Heavy Traffic condition.
(5) bituminous composition of the present invention, has higher ductility compared with matrix pitch, and plasticity is good, and good stability is not emanated, and effectively improves anti-cold cracking and the chronic fatigue performance of asphalt.
(6) bituminous composition of the present invention, has the penetration degree suitable with hot asphalt and softening temperature, and ageing property improves simultaneously, effective prolonging service life of pavement.Apply this warm-mixed asphalt and prepare asphalt, when mixing and stirring and mold temperature obviously reduces by 15 ~ 30 DEG C relative to hot-mix asphalt mixture, its compound properties is suitable with hot asphalt.
(7) bituminous composition of the present invention, raw material is simple, and production cost is low, and preparation method is easy, only need simple mechanical stirring, little to the pungency of human body, environmental friendliness, environmental protection, when being applied to asphalt, without the need to adding warm-mixing agent in addition, without the need to carrying out scrap build and changing Production Flow Chart in industrial production, being suitable for industry and amplifying and application.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but therefore do not limit the present invention.
Embodiment 1
Asphalt viscosity reduction agent raw materials quality per-cent is:
Polyethylene wax: 6.5wt%;
Aminoresin: 2wt%;
Carlow amine: 3.7wt%%;
Fatty acid distribution of coconut oil diglycollic amide: 87.8wt%;
By proportioning, polyethylene wax, aminoresin, Carlow amine and fatty acid distribution of coconut oil diglycollic amide are added reaction vessel respectively, stir and be warming up to 105 DEG C, churning time is 30min, makes asphalt viscosity reduction agent; By weight percentage, added in matrix pitch by the 0.5wt% of matrix pitch, mixing temperature is 147 DEG C, and churning time is 50min, obtains bituminous composition.
Embodiment 2
Asphalt viscosity reduction agent raw materials quality per-cent is:
Microcrystalline Wax: 14.2wt%;
Polyacrylic ester: 3.6wt%;
Carlow amine: 1.5wt%%;
Polyoxyethylene carboxylate: 80.7wt%;
By proportioning, Microcrystalline Wax, polyacrylic ester, Carlow amine and polyoxyethylene carboxylate are added reaction vessel respectively, stir and be warming up to 85 DEG C, churning time is 20min, makes asphalt viscosity reduction agent; By weight percentage, added in matrix pitch by the 3wt% of matrix pitch, mixing temperature is 140 DEG C, and churning time is 45min, obtains bituminous composition.
Embodiment 3
Asphalt viscosity reduction agent raw materials quality per-cent is:
Stearic acid: 26wt%;
Resol: 4.3wt%;
Carlow amine: 2.5wt%%;
Alkylphenol polyoxyethylene: 67.2wt%;
By proportioning, stearic acid, resol, Carlow amine and alkylphenol polyoxyethylene are added reaction vessel respectively, stir and be warming up to 100 DEG C, churning time is 25min, makes asphalt viscosity reduction agent; By weight percentage, added in matrix pitch by the 4.5wt% of matrix pitch, mixing temperature is 135 DEG C, and churning time is 35min, obtains bituminous composition.
Comparative example 1
Asphalt viscosity reduction agent raw materials quality per-cent is:
Resol: 4wt%;
Carlow amine: 4.5wt%%;
Alkylol amide Soxylat A 25-7: 91.5wt%;
By proportioning, resol, Carlow amine and alkylol amide Soxylat A 25-7 are added reaction vessel respectively, stir and be warming up to 95 DEG C, churning time is 25min, makes asphalt viscosity reduction agent; By weight percentage, added in matrix pitch by the 4wt% of matrix pitch, mixing temperature is 142 DEG C, and churning time is 40min, obtains bituminous composition.
Comparative example 2
Asphalt viscosity reduction agent raw materials quality per-cent is:
Sulphur: 17.4wt%;
Carlow amine: 1.5wt%%;
Span: 81.1wt%;
By proportioning, sulphur, Carlow amine and Span are added reaction vessel respectively, stir and be warming up to 72 DEG C, churning time is 30min, makes asphalt viscosity reduction agent; By weight percentage, added in matrix pitch by the 2wt% of matrix pitch, mixing temperature is 145 DEG C, and churning time is 45min, obtains bituminous composition.
Embodiment 4
According to the method that " standard specification for construction and acceptance of highway asphalt pavement " (JTG F40-2004) specifies, the bituminous composition in embodiment 1,2,3 and comparative example 1,2 is carried out compound and mixes and stirs, be prepared into compound test specimen A, B, C, D, E.This test bitumen aggregate ratio (bituminous composition accounts for the percentage ratio of mixture quality) is 5.2%, and bituminous composition and No. 70 asphaltic nature test results are in table 1, and mixture performance evaluation result is in table 2.
Table 1 bituminous composition and No. 70 asphaltic natures.
| Project | No. 70 pitches | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| 25 DEG C of penetration degree/0.1mm | 73 | 74 | 79 | 77 | 95 | 104 |
| Softening temperature/DEG C | 48.3 | 46.2 | 46.0 | 46.9 | 44.7 | 42.5 |
| 10 DEG C of ductility/cm | 76 | 122 | 131 | 135 | 123 | >150 |
| 60 DEG C of viscosity/Pas | 220.2 | 193.0 | 198.1 | 185.4 | 124.0 | 116.8 |
| Segregation character | ||||||
| Softening point difference (48h)/DEG C | 0.2 | 0.3 | 0.3 | 0.3 | 1.1 | 0.6 |
| Rotary viscosity/mPas | ||||||
| 120℃ | 1034.0 | 762.0 | 783.0 | 807.5 | 783.0 | 760.5 |
| 135℃ | 450.0 | 335.0 | 347.5 | 326.0 | 360.5 | 339.0 |
| 150℃ | 228.5 | 152.0 | 160.5 | 150.0 | 156.0 | 148.5 |
| 165℃ | 128.0 | 93.0 | 94.0 | 91.0 | 101.5 | 90.5 |
| After TFOT | ||||||
| Quality change/% | +0.046 | -0.606 | -0.518 | -0.703 | -0.454 | -0.937 |
| Penetration ratio/% | 64 | 81 | 83 | 86 | 73 | 88 |
| 10 DEG C of ductility/cm | 8.5 | 68 | 75 | 62 | 59 | 37 |
| Softening temperature | 51.8 | 48.6 | 48.2 | 48.0 | 46.2 | 44.9 |
Table 2 bituminous composition mixture performance test result.
| Project | Mix and stir temperature/DEG C | Mold temperature/DEG C | Stability/kN | Residual stability ratio (%) | Retained strength ratio (%) | Dynamic stability (secondary/mm) |
| Heat is mixed | 150 | 140 | 10.8 | 88.4 | 84.9 | 1450 |
| A | 130 | 110 | 9.3 | 85.1 | 83.2 | 1309 |
| B | 130 | 110 | 9.4 | 86.2 | 80.7 | 1211 |
| C | 130 | 115 | 10.0 | 89.0 | 85.9 | 1274 |
| D | 130 | 110 | 8.4 | 83.5 | 77.3 | 833 |
| E | 130 | 110 | 8.2 | 78.3 | 79.1 | 906 |
| Technological standard * | -- | -- | ≥8 | ≥80 | ≥75 | ≥1000 |
Testing data shows, the bituminous composition adding asphalt viscosity reduction agent of the present invention has lower high temperature viscosity, effectively can reduce the mixing and stirring of asphalt, pave and compacting temperature; Bituminous composition of the present invention can keep 60 DEG C of higher viscosity, have higher ductility and the penetration degree suitable compared with No. 70 pitch and softening temperature, and after its film, ageing property also improves simultaneously.Apply this bituminous composition and prepare asphalt, can be implemented in mix and stir and mold temperature obviously reduces by 20 ~ 30 DEG C relative to hot-mix asphalt mixture when, property indices all meets the requirement of " standard specification for construction and acceptance of highway asphalt pavement " (JTG F40-2004).
Claims (13)
1. an asphalt viscosity reduction agent, is characterized in that: by weight percentage, comprises following component:
Additive A: 5wt% ~ 30wt%;
Additive B: 1wt% ~ 10wt%;
Carlow amine: 1wt% ~ 10wt%;
Addition of C: 50wt% ~ 93wt%;
Wherein, described additive A, fusing point, between 60 ~ 130 DEG C, comprises one or more in polyethylene wax, Microcrystalline Wax, montanin wax, sasobit, sulphur, stearic acid, arachic acid or Lignoceric acid and derivative thereof;
Described additive B is high molecular component, comprises one or more in polyethylene oxide-propylene oxide, resol, polyacrylic ester, aminoresin, polyethers, polyvinyl alcohol and partial esterification thereof or acetalation product;
Described addition of C is low-molecular-weight component, comprises one or more in the esterification and etherification product that fatty acid distribution of coconut oil diglycollic amide, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, alkylol amide Soxylat A 25-7, Block polyoxyethylene-polyethenoxy ether, alkyl polyglycoside, polyvalent alcohol stearate, Span, fatty acid ethylene oxide condensate, castor oil polyoxyethylene ether, polyoxyethylene glycol dioleic acid ester and Spans are serial and Tweens is serial.
2. according to asphalt viscosity reduction agent according to claim 1, it is characterized in that: preferably composition comprises by weight percentage:
Additive A: 10wt% ~ 20wt%;
Additive B: 2wt% ~ 5wt%;
Carlow amine: 2wt% ~ 5wt%;
Addition of C: 70wt% ~ 86wt%.
3. according to the asphalt viscosity reduction agent described in claim 1 or 2, it is characterized in that: described additive A is polyethylene wax and/or stearic acid.
4. according to the asphalt viscosity reduction agent described in claim 1 or 2, it is characterized in that: described additive B is high molecular component is polyacrylic ester and/or aminoresin.
5., according to the asphalt viscosity reduction agent described in claim 1 or 2, it is characterized in that: described addition of C to be low-molecular-weight component be in fatty alcohol-polyoxyethylene ether, alkylol amide Soxylat A 25-7 and fatty acid distribution of coconut oil diglycollic amide one or more.
6. according to the asphalt viscosity reduction agent described in claim 1 or 2, it is characterized in that: in asphalt viscosity reduction agent, add organic additive, comprise one or more in ethyl diazoacetate, Cellmic C 121, N, N-dinitrosopentamethlyene tetramine and Diisopropyl azodicarboxylate.
7. a preparation method for the asphalt viscosity reduction agent described in claim 1 or 2, is characterized in that comprising following content: by proportioning, additive A, additive B, Carlow amine and addition of C are added reaction vessel respectively, mix, make asphalt viscosity reduction agent.
8. in accordance with the method for claim 7, it is characterized in that: mixing temperature is 60 ~ 130 DEG C, mixing time is 20 ~ 30 minutes, and mixing process adopts conventional mechanical stirring.
9. by a bituminous composition for the preparation of the asphalt viscosity reduction agent described in claim 1 or 2, it is characterized in that: comprise matrix pitch and asphalt viscosity reduction agent, with matrix pitch weight for benchmark, viscosity-depression agent is the 0.1wt% ~ 5wt% of matrix pitch.
10. according to bituminous composition according to claim 9, it is characterized in that: described matrix pitch is one or more in straight-run pitch, oxidized bitumen and solvent deoiling pitch, and its penetration degree is 60 ~ 120 1/10mm.
The preparation method of 11. 1 kinds of bituminous compositions according to claim 9, comprises following content: add in matrix pitch by proportioning by asphalt viscosity reduction agent, mix, obtain bituminous composition.
12. in accordance with the method for claim 11, it is characterized in that: mixing temperature is 130 ~ 150 DEG C, and mixing time is 30 ~ 60 minutes; Mixing process adopts the one or more combination in mechanical stirring, ultrasonic, microwave or high-shear technique means.
The application in urban road laying, maintenance and building of 13. 1 kinds of bituminous compositions according to claim 9.
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