CN108264721A - The preparation method of high-viscosity bitumen modifier and modified pitch and asphalt containing the modifying agent - Google Patents
The preparation method of high-viscosity bitumen modifier and modified pitch and asphalt containing the modifying agent Download PDFInfo
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Abstract
Modified pitch and asphalt the present invention provides a kind of preparation method of high-viscosity bitumen modifier and containing the modifying agent, the high-viscosity bitumen modifier is used for asphalt modification, can meet the requirement of high viscosity, high-adhesiveness and high-low temperature resistant performance simultaneously.The preparation method of the high-viscosity bitumen modifier includes the following steps：(1) it is thermoplastic styrene butadiene rubber, ethylene octene polyolefin elastomer and maleic anhydride, initiator is uniform in high-speed mixer and mixing, graft reaction then occurs in double screw extruder and extruding pelletization prepares maleic anhydride modified master batch；(2) by the maleic anhydride modified master batch and butadiene-styrene rubber, tackifying resin and the crosslinking agent mixing in high mixer, dynamic vulcanization and extruding pelletization in double screw extruder is then added in, obtains the high-viscosity bitumen modifier.
Description
Technical field
The present invention relates to a kind of preparation method of high-viscosity bitumen modifier and the modified pitch containing the modifying agent and drips
Green mixture.
Background technology
Porous asphalt pavement there is noise reduction, permeable and ventilative, waterproof to float etc. special as a kind of macroporous pavement structure
Point can effectively reduce rainy day road surface accident, take place frequently in current urban waterlogging and country advocates build the big of " sponge city " energetically
It is particularly important under background.But general pitch lacks certain cohesive force to macroporous structure and influences performance, arranges in addition
Bituminous grout road surface also has that high and low temperature resistance is bad.And highly viscous modified pitch is polymerize by being introduced in pitch
Object etc. can provide the stronger adhesion strength of building stones and improve the performances such as high/low temperature and cause extensive concern.
SBS (thermoplastic styrene butadiene rubber) is used as most common polymer, is studied for asphalt modifier more.But its with
Bitumen compatibility is limited, and also to be improved as high-viscosity bitumen modifier tackifying ability, is difficult to meet the whole height in road surface in addition
Performance use demand.Chinese patent literature CN1657565A discloses a kind of asphalt modifier with high viscosity and preparation method thereof, by
SBS, Petropols and diatomite composition, although preparation method is simple, high-temperature storage characteristics are good, are difficult to take into account high/low temperature usability
Energy.Chinese patent literature CN101457009B discloses a kind of asphalt modifier with high viscosity and preparation method thereof, by SIS (benzene second
Alkene-isoprene-styrene block copolymer), coumarone indene resin and oleamide be prepared, although good with bitumen compatibility
And with good adhesiveness and high-temperature behavior, but the satisfaction of cryogenic property is not taken into account.Chinese patent literature
CN102268188B discloses a kind of high viscosity asphalt additive, preparation method and its application, by rubber powder and POE compounding masters
Agent, plasticizer, filler and stabilizer composition, can improve the performances such as softening point, the viscosity of pitch, but be not directed to road surface to a certain degree
The high performance use demand such as high-low temperature resistant.Although Yi Shang modification technology solves Bituminous stabilized to a certain extent, viscosity carries
The problems such as liter and high temperature resistant, but for meeting the high-performance requirement of viscosity, bitumen compatibility and high-low temperature resistant simultaneously, relate to
It is and less.
Invention content
Goal of the invention
It is an object of the present invention to provide a kind of preparation method of high-viscosity bitumen modifier, gained modifying agent is used for pitch
It is modified, the requirement of high viscosity, high-adhesiveness and high-low temperature resistant performance can be met simultaneously.
It is a further object to provide the modified drips of the high-viscosity bitumen modifier obtained containing above-mentioned preparation method
It is green.
Pitch it is a further object to provide the high-viscosity bitumen modifier obtained containing above-mentioned preparation method mixes
Close material.
Summary of the invention
According to the first aspect of the invention, the present invention provides a kind of preparation method of high-viscosity bitumen modifier, including
Following steps：
(1) thermoplastic styrene butadiene rubber, ethylene octene polyolefin elastomer and maleic anhydride, initiator are mixed in high mixer
It closes uniformly, graft reaction then occurs in double screw extruder and extruding pelletization prepares maleic anhydride modified master batch；
(2) by the maleic anhydride modified master batch and butadiene-styrene rubber, tackifying resin and the crosslinking agent mixing in high mixer, so
Dynamic vulcanization and extruding pelletization in double screw extruder are added in afterwards, obtain the high-viscosity bitumen modifier；
The quality group of the raw material becomes：
The thermoplastic styrene butadiene rubber (SBS) is known in the art common substance, is s-B-S
Triblock polymer；The butadiene-styrene rubber (SBR) is styrene and the random copolymer of butadiene, is equally known in the art
Common substance.In the present invention, when meaning is simple " butadiene-styrene rubber ", then refer to the random copolymerization of styrene and butadiene
Object when refering in particular to " thermoplastic styrene butadiene rubber ", then refers to the triblock polymer of s-B-S.
Preferably, the thermoplastic styrene butadiene rubber is the mixed of star-like thermoplastic styrene butadiene rubber and linear thermoplastic's butadiene-styrene rubber
Close object, and star-like thermoplastic styrene butadiene rubber account for thermoplastic styrene butadiene rubber gross mass 10%~40% (be, for example, 10%, 20%,
30%).
Preferably, the butadiene-styrene rubber in solution polymerized butadiene styrene rubber, emulsion polymerized styrene butadiene rubber and powder styrene butadiene rubber at least
It is a kind of.
Preferably, the tackifying resin is at least one of rosin resin, Petropols, terpene resin.
Preferably, the initiator is cumyl peroxide and/or azodiisobutyronitrile.
Preferably, the crosslinking agent is sulphur.
The design parameter of generation graft reaction and extruding pelletization in double screw extruder can be by people in the art
Member is through testing simple determine, it is preferred that wherein extruder screw draw ratio is 36: 1~48: 1, and extrusion temperature is from 120~190
DEG C, screw speed is 40~150rpm；
The design parameter of dynamic vulcanization and extruding pelletization can also be passed through by those skilled in the art in the double screw extruder
Experiment is simple to be determined, it is preferred that wherein extruder screw draw ratio is 36: 1~48: 1, and extrusion temperature is from 145~220 DEG C, spiral shell
Bar rotating speed is 40~300rpm.
According to the second aspect of the invention, the present invention also provides change containing the high-viscosity asphalt obtained by above-mentioned preparation method
Property agent modified pitch, the raw material composition of the modified pitch is comprising the high-viscosity bitumen modifier and pitch, the high viscous drip
Green content of modifier is the 1%~12% of asphalt quality.The pitch is preferably 70# and 90# pitches.
The preparation process of the modified pitch is as follows：(1) high-viscosity bitumen modifier is first added in 160~180 DEG C
Half an hour is stirred in 70# pitches；(2) it is small with 4000~5000rpm rates high-speed stirred 1 at 160~180 DEG C with high-speed shearing machine
When, it is to obtain the modified pitch then to develop half an hour.Wherein described 60 DEG C of dynamic viscosities of modified pitch are more than 20000Pa
s。
According to the third aspect of the present invention, the present invention also provides change containing the high-viscosity asphalt obtained by above-mentioned preparation method
Property agent asphalt, the raw material composition of the asphalt is comprising the high-viscosity bitumen modifier and pitch, the height
Viscosity bitumen modifier volume is the 1%~12% of asphalt quality.The pitch is preferably 70# and 90# pitches.
The preparation method of the asphalt can be optionally following one of which：
(1) can will gather materials, high-viscosity bitumen modifier, pitch, the direct mix of miberal powder obtain asphalt.
(2) can also high-viscosity bitumen modifier and pitch be first mixed with the modified pitch, then add in gather materials, ore deposit
Powder mix obtains asphalt.
The present invention passes through reactive extrursion and dynamic vulcanization technology system using raw materials such as SBS, POE, SBR, tackifying resin, MAH
Standby high-viscosity bitumen modifier.Wherein, SBS can take into account the raising of modified pitch and mixture high and low temperature resistance；POE and SBR
With excellent resistance to low temperature, the cost of POE is also relatively cheap in addition；The addition of star-shaped sbs, SBR and tackifying resin can be with
It is obviously improved the viscosity of system；Maleic anhydride reactive extrursion can make the upper polar group of SBS, POE polymer surfaces grafting, make it
It is promoted with the compatibility of pitch, increases system stability；Dynamic vulcanization is primarily to overcome the difficult processing of elastomer and rubber
Topic.There is excellent comprehensive performance using the modified pitch of the high-viscosity bitumen modifier of the invention prepared and asphalt,
Can meet porous asphalt pavement to high-viscosity asphalt, high-adhesiveness, high-low temperature resistant use demand.
Specific embodiment
With reference to embodiment, the technical solution that the present invention is further explained.
Each raw material information involved in following embodiment is as follows：Wherein, star-shaped sbs are 411 model of LG chemical companies of South Korea,
Type SBS is Yueyang petrochemical industry Co., Ltd YH-792 models；POE is 7447 model of DOW Chemical Co., Ltd；SBR is shown for Shandong
The poly- particle model of XY-GO15 breasts of first Chemical Industry Science Co., Ltd；Petropols are Jitian Chemical Co., Ltd. of Shenzhen, model
C5 Petropols for D0102；Purchased from Zhengzhou Sheng Yu chemical products Co., Ltd, model is respectively for rosin resin and terpene resin
FS-1 and T100；Maleic anhydride, cumyl peroxide, azodiisobutyronitrile are purchased from the auspicious Chemical Co., Ltd.s of Shanghai Feng, excellent
Grade, purity are more than 99%；Sulphur is purchased from Lianyun Harbour Lan Xing Industrial Technology Co., Ltd, and purity is more than 99%.
Used gathering materials is purchased from Nanjing Gao Jia road and bridge company limestone building stones, and the composition of wherein mixture is：
The 10-15mm building stones of 39wt%, the 5-10mm building stones of 44wt%, the 3-5mm building stones of 3%wt%, 11wt% 0-3mm building stones,
The miberal powder of 3wt%.Pitch used is Taizhou 70# pitches and 90# pitches, and softening point is respectively 47 DEG C and 45 DEG C, needle penetration (25
DEG C, 100g, 5s) it is respectively 71mm and 88mm.The test method of mixture is with reference to JTG E-20-2011 highway engineerings pitches and drip
Green test mixture regulation carries out.High-viscosity bitumen modifier associated test standards change with reference to JTT 860.2-2013 asphalts
Property additive second part：High viscosity additive regulation carries out.The compatibility of high-viscosity bitumen modifier and pitch is dripped according to modified
Apparent non-fusant is whether there is after blueness stirring to be judged, such as without apparent particle, shows that compatibility is good；It is otherwise opposite.
Embodiment 1
The raw material composition of the high-viscosity bitumen modifier is as follows：14 parts of type SBS, 6 parts of star-shaped sbs, ethylene-octene gather
30 parts of olefin elastomer (POE), 35 parts of butadiene-styrene rubber (SBR), 12.49 parts of Petropols, 0.5 part of maleic anhydride (MAH), peroxide
Change 0.01 part of diisopropylbenzene (DIPB), 2 parts of sulphur.
The preparation method of the high-viscosity bitumen modifier is as follows：(1) by SBS, POE, MAH, cumyl peroxide in height
It is uniformly mixed in mixed machine, then reactive extrursion is granulated in double screw extruder.Wherein extruder screw draw ratio is 40: 1, is squeezed
Go out temperature from 120 DEG C to 180 DEG C, screw speed 100rpm.(2) by first step reaction master batch and SBR, Petropols and sulphur
It is uniform in high-speed mixer and mixing, then in double screw extruder dynamic vulcanization extruding pelletization, obtain the high-viscosity bitumen modifier.
Wherein screw slenderness ratio is 36: 1, and extrusion temperature is from 155 DEG C to 200 DEG C, screw speed 250rpm.
Preparing for the modified pitch is as follows：(1) 6% above-mentioned high-viscosity bitumen modifier is first added in 180 DEG C of 70# to drip
Half an hour is stirred in blueness；(2) continue with 180 DEG C of high-speed shearing machine high-speed stirred 1 hour, then develop half an hour obtain it is described
Modified pitch.
Preparing for the asphalt is as follows：By the high-viscosity bitumen modifier, gather materials and mix in pot is first mixed at 180 DEG C
30s adds in pitch and continues mix 90s, is eventually adding miberal powder stirring 90s and obtains the asphalt.Wherein bitumen aggregate ratio is
4.4, high-viscosity bitumen modifier quality accounts for the 6% of pitch.
High-viscosity bitumen modifier, modified pitch and asphalt correlated performance described in 1 embodiment 1 of table
Embodiment 2
The raw material composition of the high-viscosity bitumen modifier is as follows：36 parts of type SBS, 4 parts of star-shaped sbs, ethylene-octene gather
25 parts of olefin elastomer (POE), 27.9 parts of butadiene-styrene rubber (SBR), 5 parts of rosin resin, 1 part of maleic anhydride (MAH), azo two are different
0.1 part of butyronitrile, 1 part of sulphur.
The preparation method of the high-viscosity bitumen modifier is as follows：(1) it is SBS, POE, MAH, azodiisobutyronitrile is mixed in height
It is uniformly mixed in machine, then reactive extrursion is granulated in double screw extruder.Wherein extruder screw draw ratio is 48: 1, is squeezed out
Temperature is from 130 DEG C to 185 DEG C, screw speed 50rpm.(2) first step reaction master batch is existed with SBR, rosin resin and sulphur
High-speed mixer and mixing is uniform, then in double screw extruder dynamic vulcanization extruding pelletization, obtains the high-viscosity bitumen modifier.Its
Middle extruder screw draw ratio is 40: 1, and extrusion temperature is from 145 DEG C to 210 DEG C, screw speed 100rpm.
Preparing for the modified pitch is as follows：(1) 8% above-mentioned high-viscosity bitumen modifier is first added in 170 DEG C of 90# to drip
Half an hour is stirred in blueness；(2) continue with 180 DEG C of high-speed shearing machine high-speed stirred 1 hour, then develop half an hour obtain it is described
Modified pitch.
Preparing for the asphalt is as follows：By the high-viscosity bitumen modifier, gather materials and mix in pot is first mixed at 170 DEG C
30s adds in pitch and continues mix 90s, is eventually adding miberal powder stirring 90s and obtains the asphalt.Wherein bitumen aggregate ratio is
4.3, the high-viscosity bitumen modifier quality accounts for the 8% of pitch.
High-viscosity bitumen modifier, modified pitch and asphalt correlated performance described in 2 embodiment 2 of table
Embodiment 3
The raw material composition of the high-viscosity bitumen modifier is as follows：22 parts of type SBS, 8 parts of star-shaped sbs, ethylene-octene gather
45 parts of olefin elastomer (POE), 15 parts of butadiene-styrene rubber (SBR), 6.2 parts of terpene resin, 3 parts of maleic anhydride (MAH), peroxidating two
0.3 part of isopropylbenzene, 0.5 part of sulphur.
The preparation method of the high-viscosity bitumen modifier is as follows：(1) by SBS, POE, MAH, cumyl peroxide in height
It is uniformly mixed in mixed machine, then reactive extrursion is granulated in double screw extruder.Wherein extruder screw draw ratio is 40: 1, is squeezed
Go out temperature from 140 DEG C to 180 DEG C, screw speed 40rpm.(2) by first step reaction master batch and SBR, terpene resin and sulphur
It is uniform in high-speed mixer and mixing, then in double screw extruder dynamic vulcanization extruding pelletization, obtain the high-viscosity bitumen modifier.
Wherein extruder screw draw ratio is 40: 1, and extrusion temperature is from 160 DEG C to 210 DEG C, screw speed 50rpm.
Preparing for the modified pitch is as follows：(1) 10% above-mentioned high-viscosity bitumen modifier is first added in 180 DEG C of 70#
It stirs half an hour (2) in pitch to continue to use 170 DEG C of high-speed shearing machine high-speed stirred 1 hour, it is to obtain height then to develop half an hour
Adhered modification pitch.
Preparing for the asphalt is as follows：By the high-viscosity bitumen modifier, gather materials and mix in pot is first mixed at 175 DEG C
30s adds in pitch and continues mix 90s, is eventually adding miberal powder stirring 90s and obtains the asphalt.Wherein bitumen aggregate ratio is
4.3, high-viscosity bitumen modifier quality accounts for the 10% of pitch.
High-viscosity bitumen modifier, modified pitch and asphalt correlated performance described in 3 embodiment 3 of table
Embodiment 4
The raw material composition of the high-viscosity bitumen modifier is as follows：35 parts of type SBS, 10 parts of star-shaped sbs, ethylene-octene gather
20 parts of olefin elastomer (POE), 15 parts of butadiene-styrene rubber (SBR), 13.7 parts of Petropols, 5 parts of maleic anhydride (MAH), peroxidating
0.3 part of diisopropylbenzene (DIPB), 1 part of sulphur.
The preparation method of the high-viscosity bitumen modifier is as follows：(1) by SBS, POE, MAH, cumyl peroxide in height
It is uniformly mixed in mixed machine, then reactive extrursion is granulated in double screw extruder.Wherein extruder screw draw ratio is 48: 1, is squeezed
Go out temperature from 150 DEG C to 200 DEG C, screw speed 100rpm.(2) by first step reaction master batch and SBR, Petropols and sulphur
It is uniform in high-speed mixer and mixing, then in double screw extruder dynamic vulcanization extruding pelletization, obtain the high-viscosity bitumen modifier.
Wherein extruder screw draw ratio is 36: 1, and extrusion temperature is from 165 DEG C to 220 DEG C, screw speed 40rpm.
Preparing for the modified pitch is as follows：(1) 10% above-mentioned high-viscosity bitumen modifier is first added in 180 DEG C of 90#
Half an hour is stirred in pitch；(2) continue to use 180 DEG C of high-speed shearing machine high-speed stirred 1 hour, it is to obtain institute then to develop half an hour
State modified pitch.
Preparing for the asphalt is as follows：By high-viscosity bitumen modifier, gather materials and mix 30s in pot first mixed at 180 DEG C,
It adds in pitch and continues mix 90s, be eventually adding miberal powder stirring 90s and obtain the asphalt.Wherein bitumen aggregate ratio is 4.2,
High adhered modification agent quality accounts for the 10% of pitch.
High-viscosity bitumen modifier, modified pitch and asphalt correlated performance described in 4 embodiment 4 of table
With reference to table 1-4, excellent part of the invention is：Asphalt modifier is good with bitumen compatibility, and modified pitch is almost
Without non-fusant；For modified pitch, meet condition from 60 DEG C of dynamic viscosities and excellent show that modified pitch has highly viscous spy
Point.From show with the adherency grade gathered materials modified pitch have excellent adhesive capacity；Ductility and low-temperature bending failure strain point
Do not show that modified pitch and mixture have good resistance to low temperature.The data such as softening point and dynamic stability show to be modified respectively
Pitch and mixture have good high temperature resistance；In short, the high-viscosity bitumen modifier of preparation of the embodiment of the present invention, modified drip
Green and asphalt various aspects of performance is more excellent, meets code requirement, can meet porous asphalt pavement high-low temperature resistant
Deng comprehensive performance requirement.
Claims (8)
1. a kind of preparation method of high-viscosity bitumen modifier, which is characterized in that include the following steps：
(1) it is thermoplastic styrene butadiene rubber, ethylene octene polyolefin elastomer and maleic anhydride, initiator is equal in high-speed mixer and mixing
It is even, graft reaction then occurs in double screw extruder and extruding pelletization prepares maleic anhydride modified master batch；
(2) by the maleic anhydride modified master batch and butadiene-styrene rubber, tackifying resin and the crosslinking agent mixing in high mixer, Ran Houjia
Enter dynamic vulcanization and extruding pelletization in double screw extruder, obtain the high-viscosity bitumen modifier；
The quality group of the raw material becomes：
2. the preparation method of high-viscosity bitumen modifier as described in claim 1, which is characterized in that the thermoplastic styrene butadiene rubber
For star-like thermoplastic styrene butadiene rubber and the mixture of linear thermoplastic's butadiene-styrene rubber, and star-like thermoplastic styrene butadiene rubber accounts for thermoplasticity
The 10%~40% of butadiene-styrene rubber gross mass.
3. the preparation method of high-viscosity bitumen modifier as described in claim 1, which is characterized in that the butadiene-styrene rubber is contains intermingle with
At least one of butadiene-styrene rubber, emulsion polymerized styrene butadiene rubber and powder styrene butadiene rubber.
4. the preparation method of high-viscosity bitumen modifier as described in claim 1, which is characterized in that the tackifying resin is rosin
At least one of resin, Petropols, terpene resin.
5. the preparation method of high-viscosity bitumen modifier as described in claim 1, which is characterized in that the initiator is peroxidating
Diisopropylbenzene (DIPB) and/or azodiisobutyronitrile.
6. the preparation method of high-viscosity bitumen modifier as described in claim 1, which is characterized in that the crosslinking agent is sulphur.
7. the modified pitch containing the high-viscosity bitumen modifier obtained by any one of the claim 1-6 preparation methods, special
Sign is that raw material composition includes the high-viscosity bitumen modifier and pitch, and the high-viscosity bitumen modifier volume is asphalitine
The 1%~12% of amount.
8. the asphalt containing the high-viscosity bitumen modifier obtained by any one of the claim 1-6 preparation methods,
It is characterized in that, raw material composition includes the high-viscosity bitumen modifier and pitch, and the high-viscosity bitumen modifier volume is pitch
The 1%~12% of quality.
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| CN113025070A (en) * | 2021-03-17 | 2021-06-25 | 山东京博石油化工有限公司 | Preparation method of high-viscosity modified asphalt |
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| CN114605846A (en) * | 2022-04-26 | 2022-06-10 | 河南蓝翎环科防水材料有限公司 | Super-durable high polymer modified asphalt waterproof coiled material and preparation method thereof |
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