CN105255204A - High-ductility modified asphalt and preparation method thereof - Google Patents
High-ductility modified asphalt and preparation method thereof Download PDFInfo
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- CN105255204A CN105255204A CN201510656858.8A CN201510656858A CN105255204A CN 105255204 A CN105255204 A CN 105255204A CN 201510656858 A CN201510656858 A CN 201510656858A CN 105255204 A CN105255204 A CN 105255204A
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Abstract
The invention discloses high-ductility modified asphalt. The high-ductility modified asphalt is prepared from, by weight, 92%-96% of matrix asphalt, 3%-6% of linear terminal hydroxylation SBS, 0%-3% of compatilizer and 0.1%-0.4% of stabilizer. The invention further discloses a preparation method of the modified asphalt. The modified asphalt is high in ductility, good in crack resistance, wide in using temperature range, good in storage stability, capable of obviously improving the low-temperature cracking and fatigue resistance of a road surface and widening the application range, and beneficial to industrial production.
Description
Technical field
The present invention relates to a kind of modifying asphalt, particularly relate to a kind of high ductility modifying asphalt.Meanwhile, the invention still further relates to the preparation method of this modifying asphalt.
Background technology
Modern road traffic axle load, flow is large, and tire pressure is high, and also therefore road pavement quality proposes requirements at the higher level, and plain asphalt has been difficult to adapt to day by day harsh environment and technical requirements.This is because plain asphalt exists unsurmountable characteristic, such as low temperature embrittlement, and temperature sensitivity is large, and high temperature trickles, and can not adapt to the requirement of high highway.So people wish the performance improving or improve some aspect of pitch by adding some other material.Polymer modified asphalt is most widely used, wherein, styrene-butadiene-styrene block copolymer (SBS) is due to the structure of its uniqueness, have rubber and plastics two kinds of performances concurrently, there is under normal temperature the elasticity of rubber, under high temperature, can plastic material be become, the anti-cold cracking property of pitch can be improved, the high-temperature stability of pitch can be improved again, promoted rapidly in modifying asphalt.
Polymer modified asphalt performance will reach best, polymkeric substance must be made to can be uniformly dispersed and be dissolved in matrix pitch, forms homogeneous system.But SBS is a kind of superpolymer, and be non-polar polymer, with the poor compatibility of the matrix pitch of polarity, cause modifying asphalt can be separated in the process such as high-temperature storage, transport, result makes asphalt performance be deteriorated, and low-temperature ductility reduces, easy to crack, temperature sensitivity is high, and then has influence on the quality of pitch and normal use.Therefore, SBS modifying asphalt still has some limitations, and needs the consistency improving SBS and pitch, improves modifying asphalt low-temperature ductility, could solve modifying asphalt like this at cold cracking, the phenomenon of embrittlement, its anti-fatigue performance is improved.
Because pitch is polar material, according to similar dissolve mutually theory, between polar material and polar material, consistency can be better.In order to improve SBS and bitumen compatibility, utilizing chemical modification in SBS, introduce polar group and being developed fast.As CN1365986A adopts chemical graft process forming section polar group on SBS, improve and bitumen compatibility, for the acid anhydrides series of compound mainly containing double bond of grafting.But this method destroys the complete molecular chain structure of SBS, makes the performance of self of SBS be subject to certain impact; And this polarity S BS is obtained by the reaction of macromole secondary grafting, complex process, production cost is high, is difficult to scale operation.CN101041708A discloses a kind of SBS(SBS-N of terminal amido) preparation method, and use it for modifying asphalt, this method prepares the integrity that official's energy SBS can not destroy the molecular chain of SBS itself, the original synthesis technique of SBS is not changed yet, and obviously can improve pitch segregation, improve stability in storage, but SBS-N improves DeGrain to raising low-temperature ductility, low-temperature ductility lower (<19cm), and ductility also not mentioned after TFOT.
In sum, be badly in need of one at present and have high ductility at low temperatures, fatigue resistance is good, has again the modifying asphalt of good hot storage stability simultaneously.
Summary of the invention
One of the object of the invention is to provide a kind of high ductility modifying asphalt, with linear terminal end hydroxylation SBS(SBS-OH) as modifier modification pitch, SBS-OH is with certain polarity, improve the consistency with matrix pitch, fully demonstrate the performance of SBS, modifying asphalt low-temperature ductility is improved, fatigue resistance improves, simultaneously hot storage stability is good, and obtaining can high temperature resistant low-temperature-resistant again, and can meet or exceed the modifying asphalt of the JTGF40-2004 code requirement of the Ministry of Communications's promulgation.
Two of object of the present invention is to provide the preparation method of above-mentioned high ductility modifying asphalt.
First object of the present invention is achieved through the following technical solutions: a kind of high ductility modifying asphalt, comprises the component of following mass percent:
Matrix pitch 92-96%
Linear terminal end hydroxylation SBS3-6%
Compatilizer 0-3%
Stablizer 0.1-0.4%.
The low-temperature ductility of described high ductility modifying asphalt is that after 24-38cm, TFOT, ductility is 15-27cm.
Described matrix pitch is adopted as road 70# matrix pitch.
The molecular-weight average of described linear terminal end hydroxyl SBS (SBS-OH) is 8-14 ten thousand, not oil-filled, inlay character S/B=3/7.
The preparation method of described SBS-OH is: with vinylbenzene, and divinyl is raw material monomer, and hexanaphthene is solvent, organolithium is initiator, four furan hydrogen are muttered (THF) for activator, adopts three sections of feed way synthesis SBS; After the 3rd section of reaction, add propylene oxide and carry out end-blocking, stop with ethanol after polymerization, then add anti-aging agent and mix, desolvation obtains SBS-OH.
Described compatilizer is furfural extract oil.
Described stablizer is sulfide, as the BHS-2A of Beijing Research Institute of Petro-Chemical Engineering.
Second object of the present invention is achieved through the following technical solutions: the preparation method of high ductility modifying asphalt, comprises the following steps:
(1) get matrix pitch, be heated to melting;
(2) add compatilizer and linear terminal end hydroxyl SBS, stir premix, then high speed shear 20-30min;
(3) add stablizer high speed shear 8-12min again, then stir and grow 4-5h, namely obtain high ductility modifying asphalt.
The stir speed (S.S.) 150-250r/min of the stirring premix in described step (2), does time as 0.5-2h in advance, and premix temperature is 180-190 DEG C.
The shearing rate of the high speed shear in described step (2) and (3) is 2500r/min, and shear temperature is 170-180 DEG C.
Stir speed (S.S.) 90 ~ 120r/min that stirring in described step (3) is grown, developmental temperature is 170-180 DEG C.
advantage of the present invention:
(1) end group of the SBS-OH that the present invention is used is with-OH group, there is polarity, network structure can be formed with the polar group in pitch or physical adsorption or chemical covalent bonds, thus in pitch, form even, stable space three-dimensional reticulated structure system, the consistency of SBS-OH and pitch is improved, improves the low-temperature performance of modifying asphalt.
(2) ductility (5 DEG C) of SBS-OH modifying asphalt that prepared by the present invention is greater than 24cm, reach 35cm, after TFOT, ductility is greater than 15cm, all 100,000 with SBS(molecular-weight average under the same terms) improve 33.5% and 21.1% respectively compared with modifying asphalt, there is good low-temperature performance and snappiness, the anti-cold cracking property on road surface can be significantly improved.
(3) SBS-OH modifying asphalt provided by the invention meets national standard, have that ductility is large, splitting resistance is high, use temperature wide ranges, also there is good preservation stability, cold cracking and the anti-fatigue ability on road surface can be improved significantly, broadened application scope, is beneficial to the suitability for industrialized production of modifying asphalt.
Embodiment
In following examples 1 ~ 4 and comparative example 1 ~ 4, for the road 70# matrix pitch of Maoming Petrochemical, the invention will be further elaborated, and its performance index are in table 1.Compatilizer is provided by Maoming Petrochemical for furfural extract oil, and the preparation of its performance is in table 2.Stablizer is sulfide BHS-2A, and by Beijing, Research Institute of Petro-Chemical Engineering provides, and the preparation of its performance is in table 3.
Described stablizer is BHS-2A, and by Beijing, Research Institute of Petro-Chemical Engineering provides, and fundamental property is in table 3.
And SBS adopts the preparation of anionoid polymerization three-step approach and obtains in embodiment 1 ~ 4: be polymerized in 10L anionoid polymerization still; employing high pressure nitrogen is protected; pressure 0.4MPa, vinylbenzene and divinyl mass ratio (inlay character S/B) are 3:7, and monomer mass percentage ratio is 15%.The vinylbenzene of hexanaphthene, metering and a small amount of tetrahydrofuran (THF) (THF) are added in polymeric kettle, heating, it is broken assorted to add n-Butyl Lithium at a certain temperature, when reaction system by colourless to faint yellow constant time, reaction system impurity is removed, and the amount of the n-Butyl Lithium consumed is broken assorted amount.Then cause at adding rapidly the n-Butyl Lithium (effective lithium) 60 DEG C of initiating amount according to the relative molecular mass of design, adopt three sections of feed way synthesis SBS; After the 3rd section of reaction, add a certain amount of propylene oxide and carry out end-blocking, stop with excessive ethanol after polymerization, add anti-aging agent 2,6 ditertiary butyl p cresol (antioxidant 264), polymers soln water vapour boils glue desolventizing and obtains SBS-OH.The mol ratio of THF and effective lithium is 0.3, and the mol ratio of propylene oxide and effective lithium is 1.2:1.The mol ratio of terminator ethanol and effective lithium is 1:1.The consumption of anti-aging agent is 0.6% of polymerization end product quality.
The initiating amount of effective lithium and initiator n-Butyl Lithium, can according to the number-average molecular weight (M of the SBS of expection gained
n) and the total monomer consumption of vinylbenzene and divinyl determine, namely adopt following formula
icarry out calculating and obtaining:
Formula
i: V
initiator=(m/M
n)/C
Wherein, V
initiatorfor the volume of initiator; M is vinylbenzene and divinylic monomer quality; M
nfor designing the average molecular weight of SBS; C is the volumetric molar concentration of initiator.
embodiment 1
Batching: the mass percent of each component is respectively: matrix pitch 94.5%, SBS-OH4.3%; Furfural extract oil 1%, BHS-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS-OH is 80,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS-OH, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 4).
comparative example 1
Batching: the mass percent of each component is respectively: matrix pitch 94.5%, SBS4.3%; Furfural extract oil 1%, BHT-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS is 80,000.
Get 70# matrix pitch, be heated to 185 ± 5 DEG C of meltings; Then furfural extract oil and SBS is added, premix 1h under 200r/min, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 4).
embodiment 2
Batching: the mass percent of each component is respectively: matrix pitch 94.5%, SBS-OH4.3%; Furfural extract oil 1%, BHT-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS-OH is 100,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS-OH, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 4).
comparative example 2
Batching: the mass percent of each component is respectively: matrix pitch 94.5%, SBS4.3%; Furfural extract oil 1%, BHS-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS is 100,000.
Get 70# matrix pitch and be heated to 180 ± 5 DEG C of meltings; Then add furfural extract oil and SBS, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 4)
embodiment 3
Batching: the mass percent of each component is respectively: matrix pitch 94.5%, SBS-OH4.3%; Furfural extract oil 1%, BHT-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS-OH is 120,000.
Get 70# matrix pitch, be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS-OH, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 4).
comparative example 3
Batching: the mass percent of each component is respectively: matrix pitch 94.5%, SBS4.3%; Furfural extract oil 1%; BHS-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS is 120,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 4).
embodiment 4
Batching: the mass percent of each component is respectively: matrix pitch 94.5%, SBS-OH4.3%; Furfural extract oil 1%, BHS-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS-OH is 140,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS-OH, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 4).
comparative example 4
Batching: the mass percent of each component is respectively: matrix pitch 94.5%, SBS4.3%; Furfural extract oil 1%, BHS-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS is 140,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 4).
Date comprision from table 4 is obviously found out, the low-temperature ductility (5 DEG C) of the SBS-OH modifying asphalt prepared by embodiments of the invention 1 ~ 4 is all greater than 30cm, and after TFOT, ductility is greater than 15cm, compared with conventional SBS modified asphalt, ductility significantly improves, and softening temperature improves.When SBS-OH molecular-weight average is 100,000 (embodiment 2), the performance ductility of modifying asphalt reaches 35cm, and after TFOT, ductility reaches 25.2cm, softening temperature 74.3 DEG C, segregation softening point difference 2.3 DEG C, is less than 2.5 DEG C of road traffic regulation, and the performance of its modifying asphalt is best.
embodiment 5
Batching: the mass percent of each component is respectively: matrix pitch 95.3%, SBS-OH3.5%; Furfural extract oil 1%, BHS-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS-OH is 100,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS-OH, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 5h under 100r/min, namely obtains modifying asphalt (character is in table 5).
embodiment 6
Batching: the mass percent of each component is respectively: matrix pitch 94.3%, SBS-OH3.5%; Furfural extract oil 2%, BHS-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS-OH is 100,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS-OH, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4h under 100r/min, namely obtains modifying asphalt (character is in table 5).
embodiment 7
Batching: the mass percent of each component is respectively: matrix pitch 93%, SBS-OH5%; Furfural extract oil 1.7%, BHS-2A0.3%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS-OH is 100,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS-OH, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 5).
embodiment 8
Batching: the mass percent of each component is respectively: matrix pitch 96%, SBS-OH3%; Furfural extract oil 0.8%, BHS-2A0.2%; Wherein matrix pitch is 70# matrix pitch; The molecular-weight average of linear SBS-OH is 100,000.
Get 70# matrix pitch and be heated to 185 ± 5 DEG C of meltings; Then add furfural extract oil and SBS-OH, under 200r/min, stir premix 1h, high speed shear 25min at 175 ± 5 DEG C, shearing rate 2500r/min; After adding stablizer (BHS-2A), continue high speed shear 10min, then at 175 ± 5 DEG C, stir speed (S.S.) is grow 4.5h under 100r/min, namely obtains modifying asphalt (character is in table 5).
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character, the above embodiment of the present invention all can only be thought explanation of the present invention instead of restriction, if matrix pitch is except with except road 70# matrix pitch, other road bitumens can also be adopted.Therefore every above embodiment is done according to substantial technological of the present invention any trickle amendment, equivalent variations and modification, all belong in protection scope of the present invention.
Claims (10)
1. a high ductility modifying asphalt, is characterized in that, comprises the component of following mass percent:
Matrix pitch 92-96%
Linear terminal end hydroxylation SBS3-6%
Compatilizer 0-3%
Stablizer 0.1-0.4%.
2. high ductility modifying asphalt according to claim 1, is characterized in that, described matrix pitch adopts road 70# matrix pitch.
3. high ductility modifying asphalt according to claim 1, is characterized in that, the molecular-weight average of described linear terminal end hydroxyl SBS is 8-14 ten thousand, not oil-filled, inlay character S/B=3/7.
4. high ductility modifying asphalt according to claim 1, is characterized in that, described compatilizer is furfural extract oil.
5. high ductility modifying asphalt according to claim 1, is characterized in that, described stablizer is sulfide.
6. the high ductility modifying asphalt according to any one of claim 1-5, is characterized in that, the low-temperature ductility of described modifying asphalt is that after 24-38cm, TFOT, ductility is 15-27cm.
7. the preparation method of the high ductility modifying asphalt described in any one of claim 1-6, is characterized in that, comprise the following steps:
(1) get matrix pitch, be heated to melting;
(2) add compatilizer and linear terminal end hydroxyl SBS, stir premix, then high speed shear 20-30min;
(3) add stablizer high speed shear 8-12min again, then stir and grow 4-5h, namely obtain high ductility modifying asphalt.
8. the preparation method of high ductility modifying asphalt according to claim 7, is characterized in that, the stir speed (S.S.) 150-250r/min of the stirring premix in described step (2) does time as 0.5-2h in advance, and premix temperature is 180-190 DEG C.
9. the preparation method of high ductility modifying asphalt according to claim 7, is characterized in that, the shearing rate of the high speed shear in described step (2) and (3) is 2500r/min, and shear temperature is 170-180 DEG C.
10. the preparation method of high ductility modifying asphalt according to claim 7, is characterized in that, stir speed (S.S.) 90 ~ 120r/min that the stirring in described step (3) is grown, developmental temperature 170-180 DEG C.
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| CN110484008A (en) * | 2019-08-29 | 2019-11-22 | 中海沥青股份有限公司 | A method of improving ductility after No. 50 petroleum road asphalts dry |
| CN112745691A (en) * | 2019-10-30 | 2021-05-04 | 中国石油化工股份有限公司 | Modified asphalt with stable thermal storage prepared from two end group polarized SBS |
| CN112745692A (en) * | 2019-10-30 | 2021-05-04 | 中国石油化工股份有限公司 | End-hydroxylated SBS/graphene composite modified asphalt and preparation method thereof |
| CN112745691B (en) * | 2019-10-30 | 2022-06-14 | 中国石油化工股份有限公司 | Modified asphalt with stable thermal storage prepared from two end group polarized SBS |
| CN116120837A (en) * | 2023-01-05 | 2023-05-16 | 江苏凯伦建材股份有限公司 | Modified asphalt coating, preparation method thereof and waterproof material |
| CN116120837B (en) * | 2023-01-05 | 2023-12-08 | 江苏凯伦建材股份有限公司 | Modified asphalt coating, preparation method thereof and waterproof material |
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