CN108587207A - High-performance graphene modified pitch and production method - Google Patents

High-performance graphene modified pitch and production method Download PDF

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Publication number
CN108587207A
CN108587207A CN201810502137.5A CN201810502137A CN108587207A CN 108587207 A CN108587207 A CN 108587207A CN 201810502137 A CN201810502137 A CN 201810502137A CN 108587207 A CN108587207 A CN 108587207A
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CN
China
Prior art keywords
graphene
quality
modified pitch
polyvinylpyrrolidone
pitch
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Pending
Application number
CN201810502137.5A
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Chinese (zh)
Inventor
周超
黄刚
张霞
袁小亚
李妍
杨涛
黄杨程
李力
孙玉恒
冯曼曼
贺俊玺
刘昭
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Chongqing Jiaotong University
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Chongqing Jiaotong University
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Priority to CN201810502137.5A priority Critical patent/CN108587207A/en
Publication of CN108587207A publication Critical patent/CN108587207A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

Abstract

The present invention proposes a kind of High-performance graphene modified pitch and production method, wherein High-performance graphene modified pitch is made of 70# matrix pitches, graphene and polyvinylpyrrolidone;The quality proportioning relationship of aforementioned three kinds of substances is:The quality of graphene is 12 ‰ ~ the 14 ‰ of 70# matrix pitch quality, and the quality of polyvinylpyrrolidone is the 0.8% ~ 1.0% of graphene quality.The method have the benefit that:It proposes one kind and being suitable for industrial High-performance graphene modified pitch and production method.

Description

High-performance graphene modified pitch and production method
Technical field
The present invention relates to a kind of nano material composite modified pitch technologies of preparing more particularly to a kind of High-performance graphene to change Property pitch and production method.
Background technology
Highway construction is to weigh the important indicator of the national economic development, and highway in China construction in recent years achieves huge hair Exhibition, ended for the end of the year 2014, and highway in China total kilometrage has broken through 4,450,000 kilometers, occupied the first in the world;In all highway constructions Cheng Zhong, bituminous paving occupy the overwhelming majority, due to factors such as volume of traffic increase, vehicle enlargement, vehicle heavy duty and the temperature difference Phenomena such as track, cracking occur in the presence of, bituminous paving happens occasionally, and causes Service Performance of Asphalt Pavement to decline, therefore traffic row More stringent requirements are proposed for performance and quality of the industry to bituminous paving, it is desirable to which the application and innovation for accelerating new material, new technology subtract The diseases such as few Protective Measures of Bitumen Pavement Initial Damage.
Currently, to bituminous paving improve benefit it is maximum be SBS modified pitch development;Practice have shown that in matrix pitch Middle addition SBS modifier can significantly improve high-temperature stability, anti-fatigue performance and the temperature sensitivity on road surface;But it is actually answering In, there are the preparation condition requirements high, storage unstable (easily layering, cohesion or isolation) of SBS modified pitch, to mix and stir construction relatively tired The problems such as difficult, cause the quality controllability of pitch and asphalt not good enough, influences the performance of bituminous paving to a certain degree.
Graphene is a kind of nano material with huge specific surface area and superpower surface-active, and experiment proves, in pitch Middle addition graphene can generate the physics of pitch, chemical property special effect, to improve asphalt performance comprehensively;But It is in actual production, graphene but can not directly to be added in pitch:Experiments have shown that the additive amount when graphene reaches one When determining degree, graphene will appear serious agglomeration traits, and graphene can not be uniformly dispersed in pitch, cause graphene can not Modified effect is played to pitch.
Invention content
To solve the problems in background technology, inventor uses a variety of surfactants and basic solvent (can be with pitch It is miscible or easily and separated from bitumen, to observe the dispersion effect of graphene) tested, having eventually found one kind can be by graphene Finely dispersed surfactant-polyvinylpyrrolidone, corresponding basic solvent are absolute ethyl alcohol;To determine pitch, table The optimum proportioning and optimum process condition of face activating agent and basic solvent, inventor have carried out following experiment:
Using Uniform ity Design Method, make graphene volume (ratio of graphene quality and 70# matrix pitch quality) 2 ‰ ~20 ‰ range, polyvinylpyrrolidone volume (ratio of polyvinylpyrrolidone quality and graphene quality) exist 1%~10% range, shear rate 2000~7000 revs/min of ranges, shear time 30min~ 180min ranges, shear temperature are in 110 DEG C~150 DEG C ranges;The factor level table of experimental design is as shown in table 1, Uniform designs table is as shown in table 2, and experiment arranges as shown in table 3;Table 1
Table 2
Table 3
Each time the performance indicator for testing obtained graphene modified pitch is as shown in table 4;
Table 4
Test data is analyzed using mathematical statistics software, obtained optimization material prescription is as shown in table 5;
Table 5
Graphene modified pitch is prepared according to optimization material prescription, the property of obtained graphene modified pitch and matrix pitch Energy index comparison is as shown in table 6;
Table 6
By table 6 as it can be seen that compared to matrix pitch, according to graphene modified pitch made from optimization material prescription, 5 DEG C disconnected Split can (anti-low-temperature cracking ability) improve 8.1 times, 64 DEG C of rut factors (high-temperature resistance) improve 1.4 times, creep restore Rate (delayed elasticity recovery capability) improves 1.3 times, and the performance of graphene modified pitch is obviously improved.
Then, the present invention has obtained following scheme:
A kind of High-performance graphene modified pitch, innovation are:The High-performance graphene modified pitch is by 70# matrix Pitch, graphene and polyvinylpyrrolidone composition;The quality proportioning relationship of aforementioned three kinds of substances is:The quality of graphene is 12 ‰~the 14 ‰ of 70# matrix pitch quality, the quality of polyvinylpyrrolidone are the 0.8%~1.0% of graphene quality.
It should be noted that:Optimize in material prescription, the quality of graphene is the 13 ‰ of 70# matrix pitch quality, poly- second The quality of alkene pyrrolidone is the 0.8% of graphene quality, and the corresponding data in aforementioned schemes is respectively 12 ‰~14 ‰ Hes 0.8%~1.0%;In view of there are weighing errors and operating loss in actual production, and in view of the convenience of practical operation Property, inventor has carried out reasonable expansion to the amount ranges of graphene and polyvinylpyrrolidone, and passes through other experiment It is verified, experiment proves, as long as the dosage of graphene and polyvinylpyrrolidone in the range of aforementioned schemes, can be made Obtain the High-performance graphene modified pitch of better performances.
To keep the performance indicator of High-performance graphene modified pitch more excellent, the invention also provides following preferred embodiments: The specific surface area of the graphene is 300~400m2The single layer rate of/g, graphene are more than 80%, and the phosphorus content of graphene is more than 98.9%.
A method of High-performance graphene modified pitch being prepared, innovation is:The method includes:
1) absolute ethyl alcohol to polyvinylpyrrolidone is added into polyvinylpyrrolidone to be completely dissolved, obtains mixing molten Liquid;
2) under air-tight state, the ultrasonic vibration carried out 1.5 hours to mixed solution is handled;
3) mixed solution is added in 70# matrix pitches, obtains mixture;Mixture is placed in 70 DEG C of environment, baking 6 ~8 hours;
4) mixture is sheared, obtains High-performance graphene modified pitch;3800~3900 revs/min of shear rate Clock, 110 DEG C of shear temperature, shear time 55 minutes;
In preceding method, the quality of graphene is 12 ‰~the 14 ‰ of 70# matrix pitch quality, polyvinylpyrrolidone Quality is the 0.8%~1.0% of graphene quality.
Graphene modified pitch is made using the present invention program, can effectively solve the graphene occurred in production process reunion Problem enables graphene to be evenly dispersed in pitch and plays corresponding modifying function, is particularly suitable for graphene and is modified drip Green a large amount of making.
The method have the benefit that:It proposes one kind and being suitable for industrial High-performance graphene modified pitch And production method.
Specific implementation mode
A kind of High-performance graphene modified pitch, innovation are:The High-performance graphene modified pitch is by 70# matrix Pitch, graphene and polyvinylpyrrolidone composition;The quality proportioning relationship of aforementioned three kinds of substances is:The quality of graphene is 12 ‰~the 14 ‰ of 70# matrix pitch quality, the quality of polyvinylpyrrolidone are the 0.8%~1.0% of graphene quality.
Further, the specific surface area of the graphene is 300~400m2The single layer rate of/g, graphene are more than 80%, stone The phosphorus content of black alkene is more than 98.9%.
A method of High-performance graphene modified pitch being prepared, innovation is:The method includes:
1) absolute ethyl alcohol to polyvinylpyrrolidone is added into polyvinylpyrrolidone to be completely dissolved, obtains mixing molten Liquid;
2) under air-tight state, the ultrasonic vibration carried out 1.5 hours to mixed solution is handled;
3) mixed solution is added in 70# matrix pitches, obtains mixture;Mixture is placed in 70 DEG C of environment, baking 6 ~8 hours;
4) mixture is sheared, obtains High-performance graphene modified pitch;3800~3900 revs/min of shear rate Clock, 110 DEG C of shear temperature, shear time 55 minutes;
The quality of the graphene is 12 ‰~the 14 ‰ of 70# matrix pitch quality, and the quality of polyvinylpyrrolidone is The 0.8%~1.0% of graphene quality.

Claims (3)

1. a kind of High-performance graphene modified pitch, it is characterised in that:The High-performance graphene modified pitch is dripped by 70# matrix Green, graphene and polyvinylpyrrolidone composition;The quality proportioning relationship of aforementioned three kinds of substances is:The quality of graphene is 70# The 12 ‰ of matrix pitch quality~14 ‰, the quality of polyvinylpyrrolidone are the 0.8%~1.0% of graphene quality.
2. High-performance graphene modified pitch according to claim 1, it is characterised in that:The specific surface area of the graphene For 300~400m2The single layer rate of/g, graphene are more than 80%, and the phosphorus content of graphene is more than 98.9%.
3. a kind of method preparing High-performance graphene modified pitch, it is characterised in that:The method includes:
1) absolute ethyl alcohol to polyvinylpyrrolidone is added into polyvinylpyrrolidone to be completely dissolved, obtains mixed solution;
2) under air-tight state, the ultrasonic vibration carried out 1.5 hours to mixed solution is handled;
3) mixed solution is added in 70# matrix pitches, obtains mixture;Mixture is placed in 70 DEG C of environment, baking 6~8 Hour;
4) mixture is sheared, obtains High-performance graphene modified pitch;3800~4000 revs/min of shear rate, cuts Cut 110 DEG C of temperature, shear time 55~60 minutes;
The quality of the graphene is 12 ‰~the 14 ‰ of 70# matrix pitch quality, and the quality of polyvinylpyrrolidone is graphite The 0.8%~1.0% of alkene quality.
CN201810502137.5A 2018-05-23 2018-05-23 High-performance graphene modified pitch and production method Pending CN108587207A (en)

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Application Number Priority Date Filing Date Title
CN201810502137.5A CN108587207A (en) 2018-05-23 2018-05-23 High-performance graphene modified pitch and production method

Publications (1)

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CN108587207A true CN108587207A (en) 2018-09-28

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109735126A (en) * 2019-01-16 2019-05-10 广西云亭烯技术有限公司 A kind of graphene asphalt modification dispersion liquid and preparation method thereof
CN110358314A (en) * 2019-07-05 2019-10-22 广西清鹿新材料科技有限责任公司 A kind of preparation method of graphene composite asphalt
CN110791110A (en) * 2019-11-07 2020-02-14 江苏路耐德公路养护技术有限公司 Asphalt adhesion promoter and preparation method thereof
CN113861706A (en) * 2021-10-18 2021-12-31 陕西理工大学 Modified asphalt containing nano material and application thereof
CN116333506A (en) * 2023-04-10 2023-06-27 重庆交通大学 Composite modified asphalt and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106995613A (en) * 2017-05-15 2017-08-01 柳州博泽科技有限公司 A kind of high-performance asphalt additive

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN106995613A (en) * 2017-05-15 2017-08-01 柳州博泽科技有限公司 A kind of high-performance asphalt additive

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HARIS BRCIC: ""Investigation of the rheological properties of asphalt binder containing graphene nanoplatelets"", 《MASTER THESIS, NORWEGIAN UNIVERSITY OF SCIENCE AND TECHNOLOGY, NORWAY》 *
魏伟等: "高浓度石墨烯水系分散液及其气液界面自组装膜", 《新型炭材料》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109735126A (en) * 2019-01-16 2019-05-10 广西云亭烯技术有限公司 A kind of graphene asphalt modification dispersion liquid and preparation method thereof
CN110358314A (en) * 2019-07-05 2019-10-22 广西清鹿新材料科技有限责任公司 A kind of preparation method of graphene composite asphalt
CN110791110A (en) * 2019-11-07 2020-02-14 江苏路耐德公路养护技术有限公司 Asphalt adhesion promoter and preparation method thereof
CN110791110B (en) * 2019-11-07 2021-07-06 江苏路耐德交通科技有限公司 Asphalt adhesion promoter and preparation method thereof
CN113861706A (en) * 2021-10-18 2021-12-31 陕西理工大学 Modified asphalt containing nano material and application thereof
CN116333506A (en) * 2023-04-10 2023-06-27 重庆交通大学 Composite modified asphalt and preparation method thereof

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Application publication date: 20180928