CN106147253B - A kind of regeneration asphalt and preparation method thereof - Google Patents
A kind of regeneration asphalt and preparation method thereof Download PDFInfo
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- CN106147253B CN106147253B CN201510186434.XA CN201510186434A CN106147253B CN 106147253 B CN106147253 B CN 106147253B CN 201510186434 A CN201510186434 A CN 201510186434A CN 106147253 B CN106147253 B CN 106147253B
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Abstract
The invention discloses a kind of regeneration asphalts and preparation method thereof.The formula of the regeneration asphalt includes, in parts by weight：0.5~4.0 part of agent, 0.5~1.5 part of polyphosphoric acids, 0.5~1.5 part of stabilizer are prolonged in 100 parts of pitch of recycling, 20~40 parts of tapped oil, 10~25 parts of catalytic cracked oil pulp, 2.0~8.0 parts of thermoplastic elastomer, increasing.The regeneration asphalt performance of regeneration of this method especially suitable for the aged asphalt of waste asphalt pavement material recovery, gained meets the requirement of road asphalt technology, is used for the making of bituminous paving.
Description
Technical field
The present invention relates to a kind of regeneration asphalts and preparation method thereof, and the regeneration of pitch is especially recycled to waste asphalt pavement
Method.
Background technology
With the rapid development of highway communication cause, the construction of bituminous paving also rapidly increases, according to Chinese high speed design
Service life and practical military service shape, the highway built up successively after the nineties have been enter into it is big or middle repair the phase, every year there are about
12% Expressway Asphalt face needs repairing maintenance, and is increased with annual 15% speed.If will dig, milling Bituminous concrete surface mixes
It is discarded to close material, on the one hand causes environmental pollution, is on the other hand for the extremely deficient country of this high-quality asphalt of China
A kind of waste of resource, and new building stones are largely used, exploitation stone ore can also do great damage to ecological environment.To waste and old
Asphalt pavement material carries out regeneration, can reduce, save Master Cost and construction investment, while can reduce environment dirt again
Dye reduces energy consumption, sustainable development to society and preserves the ecological environment and is of great significance and is worth.
Asphalt material regeneration techniques make waste and old asphalt material restore every performance generally by addition regenerative agent.
CN201210411170.X provides a kind of bitumen regenerant and preparation method, 40%~65% catalytic cracked oil pulp is added 30%~
In 50% heavy oil, stirring at low speed reconcile 0.5~1.0 hour, add 1%~5% polymer and 1%~5% modifying agent high speed cut
Cutting dissipates 0.5~1.0 hour, is cooled to room temperature to obtain bitumen regenerant, disadvantage one be included heavy oil component colloid and
Asphalt content is higher, is unfavorable for infiltration and peptization of the regenerative agent in aged asphalt, and regeneration efficiency is relatively low, second is that including to change
The additive amounts such as property agent, that is, orthophosphoric acid, polyphosphoric acid, polyphosphoric acids are larger, and the presence of excess acid substance can make in slurry oil and heavy oil
In more active chemical constituent continue occur polycondensation reaction, become macromolecular asphalitine, keep regenerative agent performance unstable, it is anti-aging
Property and permeability be deteriorated, regeneration efficiency reduce.
Invention content
The present invention aiming at the deficiencies in the prior art, provides a kind of regeneration asphalt and preparation method thereof.This method
The regeneration asphalt performance of the regeneration of aged asphalt especially suitable for waste asphalt pavement material recovery, gained meets road asphalt
Technology requirement, is used for the making of bituminous paving.
Regeneration asphalt provided by the invention, formula include, in parts by weight：
Recycle 100 parts of pitch
20~40 parts of tapped oil
10~25 parts of catalytic cracked oil pulp
2.0~8.0 parts of thermoplastic elastomer, preferably 3.0~6.0 parts
0.5~4.0 part of agent, preferably 1.5~3.0 parts are prolonged in increasing
0.5~1.5 part of polyphosphoric acids, preferably 0.8~1.2 part
0.5~1.5 part of stabilizer, preferably 0.6~1.2 part.
In regeneration asphalt provided by the invention, it can also be added age resister, addition is 0~1.5 part, preferably 0.2
~1.0 parts.
In the present invention, tapped oil is the byproduct in process of oil production, is rich in aromatised fraction, preferably furfural treatment or phenol
Refined tapped oil, arene content 45wt% or more, saturation divide content to be less than 30wt%, and flash-point is not less than 220 DEG C.
In the present invention, catalytic cracked oil pulp is that aromatised fraction content is not less than 50wt%, and saturation divides content to be not more than 30wt%,
Flash-point is not less than 220 DEG C of catalytic cracked oil pulp.
In the present invention, thermoplastic elastomer is the copolymer of butadiene or isoprene and styrene block type, including benzene second
Alkene-butadiene-styrene block copolymer（SBS）, styrene-isoprene-styrene block copolymer（SIS）Or benzene second
Alkene-ethylene-butadiene-styrene block copolymer（SEBS）, optimization styrene butadiene styrene block copolymerization object（SBS）,
Because it is with good recoverable force and crack self-healing, SBS can be with line style or star structure, block ratio used in the present invention
PS/PB mass ratioes 30/70~40/60, molecular weight 8~300,000.
In the present invention, the butylbenzene that agent is the aobvious member production of butadiene-styrene rubber, such as commercially available SBR1500, SBR1502 and Shandong is prolonged in increasing
One or more mixing of rubber powder and SBR pitch modification agents.
In the present invention, the polyphosphoric acids（PPA）Middle P2O5Content >=80wt%, preferably P2O5The poly of content >=83wt%
Phosphoric acid, such as P2O5Content >=83wt% technical grades polyphosphoric acids and P2O5Content >=84wt% food-grade polyphosphoric acids.
In the present invention, the recycling pitch is generally by solvent extraction method and rotary evaporation method by waste asphalt road
Plane materiel material（RAP）The aged asphalt of recycling.
In the present invention, the stabilizer is long chain hydrocarbon groups trimethylene Diamines, preferably tallow base trimethylene diamines, hydrogenated tallow
One or more of base trimethylene diamines, lauryl trimethylene diamines, 12~octadecyl trimethylene diamines.
In the present invention, the age resister is commercially available age resister, such as irgasfos 168, antioxidant 2246 S, antioxidant
One or more of 2246-A, antioxidant 1010, antioxidant AW and antioxidant BLE etc..
The preparation method of the regeneration asphalt of the present invention, including：
（1）Tapped oil and catalytic cracked oil pulp heating melting, are uniformly mixed under agitation；
（2）By step（1）It is added in the recycling pitch of heating melting, is uniformly mixed in the mixture of gained；
（3）To step（2）Thermoplastic elastomer is added in the mixture of gained, increases and prolongs agent, after stirring swelling, poly phosphorus is added
Acid reacts after a certain period of time under the conditions of high speed shear, adds stabilizer, and after a certain period of time, regeneration asphalt is made in reaction.
In the method for the present invention, step（1）The heating temperature is 120~140 DEG C, 15~30min of incorporation time.
In the method for the present invention, step（2）Mixing condition be：145~160 DEG C of temperature, 15~30min of incorporation time.
The method of the present invention step（3）In, swelling temperature be 120~180 DEG C, preferably 145~160 DEG C, swelling time 40~
100min；It is as follows that the condition that polyphosphoric acids is reacted under the conditions of high speed shear is added：130~200 DEG C of reaction temperature, preferably
150~170 DEG C, 30~60min of reaction time；The reaction condition being added after stabilizer is as follows：130~160 DEG C of reaction temperature, instead
20~40min between seasonable.
Age resister can also be added in the method for the present invention, age resister can be in step（3）While stabilizer is added
Age resister is added, it can also be in step（3）Age resister is added after reaction, in 130~160 DEG C of condition of reaction temperature
10~20min of lower reaction.
The method of the present invention first mixes tapped oil and catalytic cracked oil pulp with recycling pitch, keeps filling of the pitch ground of aging soft
Change, restores asphalt performance, then after being mixed with thermoplastic rubber and butadiene-styrene rubber, under the action of polyphosphoric acids, each component is made to carry out
Compatible and crosslinking, while the part unstability light component polycondensation in tapped oil and catalytic cracked oil pulp being promoted to become to stablize colloid,
Long chain hydrocarbon groups diamines substance is added in due course, the unreacted polyphosphoric acids in part can be neutralized, avoids excessively being crosslinked and polycondensation is anti-
It answers, so that the pitch after regeneration has good comprehensive performance, meets the requirement of JTGF40-2004 polymer modified asphalt technologies,
Highly efficient regeneration is obtained by the aged asphalt of waste asphalt pavement material recovery to utilize.
The method of the present invention is simple, and raw material sources are extensive, and regeneration efficiency is high, is applicable in strong.
Specific implementation mode
For a better understanding of the present invention, carry out the technical solution that the present invention is further explained with reference to embodiment, these
Embodiment does not provide constraints to the present invention.Raw material used is as follows in the following examples and comparative examples：Recycling pitch is to use
The waste asphalt pavement material of solvent extraction and rotary evaporation method from recycling（RAP）The aged asphalt of middle recycling, property are shown in Table
1；Tapped oil is that Maoming Petrochemical furfural extract oil fragrance divides content 57.5wt%, saturation that content 17.2wt% open cups is divided to dodge
253 DEG C of point, catalytic cracked oil pulp Jingmen Effect of Catalysis In Petrochemistry cracking slurry oil, fragrance divide content 60.2wt%, saturation to divide content 21.5wt%,
225 DEG C of open cup flash point.Thermoplastic rubber is that Yanshan Petrochemical produces SBS1301, and increasing is prolonged agent and produced for China Petroleum Jilin Petrochemical company
SBR-1500；Polyphosphoric acids is the technical grade polyphosphoric acids of Hao Gang Chemical Co., Ltd.s of Shouguang City production, P2O5Content >=
84wt%；Stabilizer is -1,3 trimethylene diamines of N- tallows base of Guangzhou Bin Hao Chemical Co., Ltd.s production.Age resister is Nanjing
The antioxidant 2246 S of Datang chemical industry Co., Ltd.
Table 1 recycles the performance of pitch
| Project | Recycle pitch |
| Needle penetration (25 DEG C), 1/10mm | 25 |
| Softening point, DEG C | 63.8 |
| 60 DEG C of dynamic viscosities, Pa.s | 2880 |
| 5 DEG C of ductilities, cm | 0 |
Embodiment 1
Regeneration asphalt A, formula are in parts by weight, as follows：
Recycle 100 parts of pitch
20 parts of tapped oil
25 parts of catalytic slurry
3 parts of thermoplastic rubber
3 parts of agent is prolonged in increasing
1 part of PPA
1 part of stabilizer
1 part of age resister.
The preparation method of regeneration asphalt is as follows：
（1）Tapped oil and catalytic cracked oil pulp are heated to 130 DEG C, until melting trickling state, is proportionally added into retort
In, it is stirred 25min,
（2）150 DEG C of asphalt heating will be recycled, until molten condition, is added step（1）The mixture of gained, is stirred
20min；
（3) to step（2）Thermoplastic elastomer is added in the mixture of gained, increases and prolongs agent, after 150 DEG C of stirring swelling 60min,
Polyphosphoric acids is added at 160 DEG C and under the conditions of high speed shear after reaction 40min, is down to 145 DEG C and adds stabilizer and anti-aging
30min is reacted in agent, and regeneration asphalt is made, and performance is shown in Table 2, meets the requirement of JTG F40 technologies.
Embodiment 2
Regeneration asphalt B is prepared according to 1 preparation method of embodiment, each group distribution ratio is as follows by weight：
Recycle 100 parts of pitch
25 parts of tapped oil
20 parts of catalytic slurry
4 parts of thermoplastic rubber
2.5 parts of agent is prolonged in increasing
Crosslinking agent（PPA）0.8 part
0.8 part of stabilizer
0.8 part of age resister；
Regeneration asphalt performance is shown in Table 2, meets the requirement of JTG F40 technologies.
Embodiment 3
Regeneration asphalt C is prepared according to 1 preparation method of embodiment, each group distribution ratio is as follows by weight：
Recycle 100 parts of pitch
30 parts of tapped oil
15 parts of catalytic slurry
5 parts of thermoplastic rubber
2 parts of agent is prolonged in increasing
Crosslinking agent（PPA）1.0 part
1.0 parts of stabilizer
0.6 part of age resister.
Regeneration asphalt performance is shown in Table 2, meets the requirement of JTG F40 technologies.
Embodiment 4
Regeneration asphalt D is prepared according to 1 preparation method of embodiment, each group distribution ratio is as follows by weight：
Recycle 100 parts of pitch
35 parts of tapped oil
10 parts of catalytic slurry
6 parts of thermoplastic rubber
2 parts of agent is prolonged in increasing
Crosslinking agent（PPA）1.2 part
1.2 parts of stabilizer
0.4 part of age resister；
The preparation method of regeneration asphalt is as follows：
（1）Tapped oil and catalytic cracked oil pulp are heated to 135 DEG C, until melting trickling state, is proportionally added into retort
In, it is stirred 20min,
（2）155 DEG C of asphalt heating will be recycled, until molten condition, is added step（1）The mixture of gained, is stirred
20min；
（3) to step（2）Thermoplastic elastomer is added in the mixture of gained, increases and prolongs agent, after 155 DEG C of stirring swelling 60min,
Polyphosphoric acids is added at 165 DEG C and under the conditions of high speed shear after reaction 35min, is down to 150 DEG C and adds stabilizer and anti-aging
30min is reacted in agent, and regeneration asphalt is made, and performance is shown in Table 2, meets the requirement of JTG F40 technologies.
Embodiment 5
Regeneration asphalt E is prepared according to 1 preparation method of embodiment, each group distribution ratio is as follows by weight：
Recycle 100 parts of pitch
40 parts of tapped oil
15 parts of catalytic slurry
5 parts of thermoplastic rubber
3 parts of agent is prolonged in increasing
Crosslinking agent（PPA）1.0 part
0.8 part of stabilizer；
Regeneration asphalt performance is shown in Table 2, meets the requirement of JTG F40 technologies.
Comparative example 1
Comparative example 1 first prepares regenerative agent by the CN201210411170.X methods provided, then is mixed with recycling pitch
Regeneration asphalt DA, it is specific as follows：
By catalytic cracked oil pulp（Fragrance is divided into 52wt%）It is added to 135 DEG C of decompression residuum（Saturation is divided into 18wt%）In, it is low
Speed stirring 0.5 hour, is then added butadiene-styrene rubber（SBR）And polyphosphoric acids（Purity 84wt%）, high speed shear 0.5 hour, cooling
Regenerative agent is obtained to room temperature.Regenerative agent each component is by weight percentage：
Decompression residuum 35%
Catalytic cracked oil pulp 60%
SBR 3%
Polyphosphoric acids 2%；
It is added in 80% recycling pitch by weight by 20% regenerative agent, is stirred 1 hour at 150 DEG C and obtain regeneration asphalt,
Regeneration asphalt performance is shown in Table 2.
Comparative example 2
Tapped oil and catalytic cracked oil pulp are heated to 130 DEG C, until melting trickling state, is proportionally added into retort,
It is stirred 30min, thermoplastic elastomer is then added, increases and prolongs agent and polyphosphoric acids, under the conditions of high speed shear after reaction 40min,
It is down to 145 DEG C and adds stabilizer and age resister, react 30min, bitumen regenerant is made, regenerative agent each component is by weight
For：
30 parts of tapped oil
15 parts of catalytic slurry
5 parts of thermoplastic rubber
2 parts of agent is prolonged in increasing
Crosslinking agent（PPA）1.0 part
1.0 parts of stabilizer
0.6 part of age resister；
The bitumen regenerant of preparation is added in 100 parts of recycling pitch, being stirred to react 30min under the conditions of 150 DEG C obtains
To regeneration asphalt DB, regeneration asphalt performance is shown in Table 2.
Comparative example 3
Regeneration asphalt DC is prepared according to 3 preparation method of embodiment, the difference is that not adding stabilizer component, regeneration asphalt
2 can be shown in Table.
Comparative example 4
Regeneration asphalt DD is prepared according to 3 preparation method of embodiment, the difference is that polyphosphoric acids is substituted for orthophosphoric acid, is regenerated
Asphalt performance is shown in Table 2.
2 embodiment of table and comparative example regeneration asphalt property
| Project | Implement Example 1 | Implement Example 2 | Implement Example 3 | Implement Example 4 | Implement Example 5 | Compare Example 1 | Compare Example 2 | Compare Example 3 | Compare Example 4 | JTGF40 -2004 |
| Needle penetration（25 DEG C), 1/10mm | 66 | 65 | 65 | 64 | 66 | 68 | 67 | 62 | 66 | 60-80 |
| Softening point, DEG C | 64.8 | 66.7 | 68.6 | 71.2 | 69.6 | 47.0 | 61.2 | 74.5 | 60.2 | ≥55 |
| 135 DEG C of viscosity, Pa.s | 1.58 | 1.25 | 1.28 | 1.59 | 1.98 | 0.45 | 1.09 | 4.21 | 1.08 | ≤3.0 |
| 5 DEG C of ductilities, cm | 68 | 63 | 58 | 52 | 81 | 20 | 40 | 28 | 30 | ≥30 |
| 25 DEG C of elasticity are extensive It is multiple, % | 80 | 83 | 85 | 87 | 86 | 49 | 74 | 90 | 62 | ≥65 |
By table 2, statistics indicate that, regeneration asphalt performance of the present invention meets JTGF40-2004 polymer modified asphalt technologies and wants
It asks, the aged asphalt of waste asphalt pavement material recovery obtains highly efficient regeneration utilization.
Claims (18)
1. a kind of regeneration asphalt, formula include, in parts by weight：
Recycle 100 parts of pitch
20~40 parts of tapped oil
10~25 parts of catalytic cracked oil pulp
2.0~8.0 parts of thermoplastic elastomer
0.5~4.0 part of agent is prolonged in increasing
0.5~1.5 part of polyphosphoric acids
0.5~1.5 part of stabilizer
Wherein, the stabilizer is long chain hydrocarbon groups trimethylene Diamines.
2. regeneration asphalt described in accordance with the claim 1, it is characterised in that：The formula of the regeneration asphalt includes, in parts by weight：
Recycle 100 parts of pitch
20~40 parts of tapped oil
10~25 parts of catalytic cracked oil pulp
3.0~6.0 parts of thermoplastic elastomer
1.5~3.0 parts of agent is prolonged in increasing
0.8~1.2 part of polyphosphoric acids
0.6~1.2 part of stabilizer.
3. regeneration asphalt described in accordance with the claim 1, it is characterised in that：The tapped oil is furfural treatment or phenol treating
Tapped oil, wherein arene content are 45wt% or more, and saturation divides content to be less than 30wt%, and flash-point is not less than 220 DEG C；The catalysis
Cracking slurry oil is that aromatised fraction content is not less than 50wt%, and saturation divides content to be not more than 30wt%, and flash-point is not less than 220 DEG C of catalysis
Cracking slurry oil.
4. regeneration asphalt described in accordance with the claim 1, it is characterised in that：The thermoplastic elastomer is styrene-butadiene-
Styrene block copolymer, styrene-isoprene-styrene block copolymer or styrene ethylene butadiene-styrene
Block copolymer.
5. regeneration asphalt described in accordance with the claim 1, it is characterised in that：The thermoplastic elastomer is styrene-butadiene-
Styrene block copolymer, block ratio PS/PB mass ratioes 30/70~40/60, molecular weight 8~300,000.
6. regeneration asphalt described in accordance with the claim 1, it is characterised in that：The recycling pitch is by solvent extraction and rotation
The aged asphalt that the method for evaporation is recycled from waste asphalt pavement material.
7. regeneration asphalt described in accordance with the claim 1, it is characterised in that：It is butadiene-styrene rubber that agent is prolonged in the increasing；The poly
P in phosphoric acid2O5Content >=80wt%.
8. according to the regeneration asphalt described in claim 1 or 7, it is characterised in that：The stabilizer is tallow base trimethylene diamines, hydrogen
Change one or more of tallow base trimethylene diamines, 12~octadecyl trimethylene diamines.
9. according to the regeneration asphalt described in claim 1 or 7, it is characterised in that：The stabilizer is lauryl trimethylene diamines.
10. regeneration asphalt described in accordance with the claim 1, it is characterised in that：In the regeneration asphalt, containing age resister,
Its addition is 0.2~1.5 part.
11. regeneration asphalt according to claim 10, it is characterised in that：The age resister is irgasfos 168, antioxidant
One or more of 2246S, antioxidant 2246-A, antioxidant 1010, antioxidant AW and antioxidant BLE.
12. the preparation method of any regeneration asphalt of claim 1~11, including：
（1）Tapped oil and catalytic cracked oil pulp heating melting, are uniformly mixed under agitation；
（2）By step（1）The mixture of gained is added in the recycling pitch of heating melting, is uniformly mixed；
（3）To step（2）Thermoplastic elastomer is added in the mixture of gained, increases and prolongs agent, after stirring swelling, polyphosphoric acids is added and exists
It is reacted under the conditions of high speed shear after a certain period of time, adds stabilizer, after a certain period of time, regeneration asphalt is made in reaction.
13. according to the method for claim 12, it is characterised in that：Step（1）The heating temperature is 120~140 DEG C,
Incorporation time is 15~30min；Step（2）Mixing condition be：Temperature is 145~160 DEG C, and incorporation time is 15~30min.
14. according to the method for claim 12, it is characterised in that：Step（3）In, swelling temperature is 120~180 DEG C, molten
The swollen time is 40~100min；It is as follows that the condition that polyphosphoric acids is reacted under the conditions of high speed shear is added：Reaction temperature is
130~200 DEG C, the reaction time is 30~60min；The reaction condition being added after stabilizer is as follows：Reaction temperature is 130~160
DEG C, the reaction time is 20~40min.
15. according to the method for claim 14, it is characterised in that：Step（3）In, swelling temperature is 145~160 DEG C.
16. according to the method for claim 14, it is characterised in that：Step（3）In, polyphosphoric acids is added in high speed shear item
It is reacted under part, reaction temperature is 150~170 DEG C.
17. according to the method for claim 12, it is characterised in that：In step（3）It is added while stabilizer is added anti-ageing
Agent.
18. according to the method for claim 12, it is characterised in that：In step（3）Age resister is added after reaction,
10~20min is reacted under conditions of 130~160 DEG C of reaction temperature.
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| CN110551400A (en) * | 2018-06-01 | 2019-12-10 | 深圳海川新材料科技股份有限公司 | asphalt and preparation method thereof |
| CN111073318B (en) * | 2019-12-27 | 2022-08-09 | 北京东方雨虹防水技术股份有限公司 | Reclaimed rubber asphalt and preparation method thereof |
| CN114656793A (en) * | 2022-02-28 | 2022-06-24 | 甘肃省交通科学研究院集团有限公司 | PPA (polyphthalamide) -based compounded high-toughness SBS (styrene butadiene styrene) modified asphalt regenerant and preparation method thereof |
| CN115029012B (en) * | 2022-08-11 | 2022-11-04 | 北京工业大学 | Asphalt liquid anti-aging agent and preparation method and application thereof |
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| CN101629020A (en) * | 2009-08-10 | 2010-01-20 | 江苏省建筑科学研究院有限公司 | Special regenerant suitable for regenerating modified asphalt and prepared method thereof |
| CN103773011A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Asphalt regenerant and preparation method thereof |
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| JP4856500B2 (en) * | 2006-08-29 | 2012-01-18 | 昭和シェル石油株式会社 | Asphalt binder |
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| CN101629020A (en) * | 2009-08-10 | 2010-01-20 | 江苏省建筑科学研究院有限公司 | Special regenerant suitable for regenerating modified asphalt and prepared method thereof |
| CN103773011A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Asphalt regenerant and preparation method thereof |
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