CN107245247A - Polyethylene modified asphalt based on carboxy-modified graphene oxide and preparation method thereof - Google Patents
Polyethylene modified asphalt based on carboxy-modified graphene oxide and preparation method thereof Download PDFInfo
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- CN107245247A CN107245247A CN201710358371.0A CN201710358371A CN107245247A CN 107245247 A CN107245247 A CN 107245247A CN 201710358371 A CN201710358371 A CN 201710358371A CN 107245247 A CN107245247 A CN 107245247A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
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Abstract
The invention provides a kind of polyethylene modified asphalt based on carboxy-modified graphene oxide and preparation method thereof, it includes the component of following parts by weight：100 parts of pitches, 0.5-3 parts of additives and 3-7 parts of modifying agent, its preparation method comprise the following steps：(1) pitch, is heated to the first temperature, is stirred after being subsequently added into modifying agent shearing, obtains modified pitch；(2) additive, is added in modified pitch to continue to shear, until additive is scattered in modified pitch, obtains the polyethylene modified asphalt based on carboxy-modified graphene oxide.Polyethylene modified asphalt is reacted using carboxy-modified graphene oxide in the raw material of the present invention so that the features such as asphalt has good adhesiveness, storage stability, high-temperature stability, high temperature Rut resistance and water stability；In addition, its preparation method is simple, technique relaxes, with low cost.
Description
Technical field
The invention belongs to road engineering technical field, and in particular to a kind of polyethylene based on carboxy-modified graphene oxide
Modified pitch and preparation method thereof.
Background technology
The developing rapidly to propose the performance of pitch of highway is deposited in higher and higher requirement, many high grade pavements
The problem of, it is necessary to draw attention.It is high temperature rut and problem on deformation first.The potential most serious of high temperature area bituminous paving
One of failure mode, is exactly oversize vehicle and heavy duty, the rut problem of overloading section of highway.The problem of in order to solve such, use
Polyethylene (PE) modified pitch is a kind of very effective method.
But there is the problem of poor adhesion and stability are poor in PE modified pitch.PE modifying agent in pitch must be refine to
Modified purpose is can be only achieved to a certain degree, and the addition of PE particles causes the viscosity and denseness of pitch to greatly improve, mobile performance
Significantly declined, therefore be difficult sufficiently to be wrapped up gathering materials.In addition, it is current from use for laboratory high-speed shearing machine to
Large-scale colloid mill is used in production, and domestic many manufacturers can produce, so the refinement dispersing apparatus of PE modifying agent is guaranteed.Ask
Topic be refined into a few micrometers PE can not hot storage for a long time, make stirring storage during PE particulates assemble collection combine
Cause to be modified failure.So PE, which can not keep microgranular naturally, is persistently dispersed among pitch i.e. shortage storage stability,
Poor storage stability forces PE modified pitch to be used while allocating.Want to must be hired by the large-scale of costliness using PE modified pitch
Thinning apparatus is simultaneously transported to job site, and the core of Austrian NOVOPHALT technologies namely relies on a kind of special movable type
Modifying agent refines dispersing apparatus to reach the purpose being used while allocating, and this puts into increase engineering, or even influence modified effect so that
The popularization and application of PE modified pitch are restricted.
Due to being limited by factors such as selections, PE modified pitch prepared by the above method is in adhesiveness and storage stability performance
It is upper still unsatisfactory.Adhesion property is not enough main reason is that add PE particles in PE modified pitch, causes pitch excessively
Sticky, therefore, it is difficult to wrapped in stone surface；Storage stability is not enough main reason is that PE particles can not be evenly
It is distributed among matrix pitch, can be isolated in long term storage so that PE modified effects declines to a great extent.Although there is patent to carry
Go out the method that job mix adds PE modifying agent, but this method causes site technique more complicated, and also quality is difficult to ensure.
The content of the invention
In view of the shortcomings of the prior art, primary and foremost purpose is to provide a kind of poly- based on carboxy-modified graphene oxide the present invention
Ethylene modified pitch.
Second object of the present invention is to provide a kind of polyethylene modified asphalt based on carboxy-modified graphene oxide
Preparation method.
To reach above-mentioned purpose, solution of the invention is：
A kind of polyethylene modified asphalt based on carboxy-modified graphene oxide, it includes the component of following parts by weight：
100 parts of pitch,
0.5-3.0 parts of additive,
3-7 parts of modifying agent.
Preferably, the one kind of pitch in Esso 70# pitches and SK70# pitches.
Preferably, modifying agent is low density polyethylene (LDPE) particle, and density is 0.915-0.940g/cm3, melt index is 1.5-
1.8g/10mim (230 DEG C, 2.16kg), mesh number is 7-18 mesh.
Preferably, additive is carboxy-modified graphene oxide.
A kind of preparation method according to the above-mentioned polyethylene modified asphalt based on carboxy-modified graphene oxide, it includes
Following steps：
(1) pitch, is heated to the first temperature, is stirred after being subsequently added into modifying agent shearing, obtains modified pitch；
(2) additive, is added in modified pitch to continue to shear, until additive is scattered in modified pitch, obtains base
In the polyethylene modified asphalt of carboxy-modified graphene oxide.
Preferably, in step (1), the first temperature is 170-180 DEG C.
Preferably, in step (1), shear rate is 3000 ± 500r/min, and shear time is 30 ± 5min.
Preferably, in step (1), mixing time is 30 ± 5min.
Preferably, in step (2), shear rate is 3000 ± 500r/min, and shear time is 20 ± 10min.
Due to using such scheme, the beneficial effects of the invention are as follows：
Polyethylene modified asphalt is reacted using carboxy-modified graphene oxide in the raw material of the present invention so that pitch
The features such as compound has good adhesiveness, storage stability, high-temperature stability, high temperature Rut resistance and water stability；Separately
Outside, its preparation method is simple, and technique relaxes, with low cost.
Embodiment
The invention provides a kind of polyethylene modified asphalt based on carboxy-modified graphene oxide and preparation method thereof.
<Polyethylene modified asphalt based on carboxy-modified graphene oxide>
A kind of polyethylene modified asphalt based on carboxy-modified graphene oxide, it includes the component of following parts by weight：
100 parts of pitch,
0.5-3 parts of additive,
3-7 parts of modifying agent.
Wherein, pitch can be selected from one kind in Esso 70# pitches and SK70# pitches.
Modifying agent is low density polyethylene (LDPE) particle, and density is 0.915-0.940g/cm3, melt index is 1.5-1.8g/
10mim (230 DEG C, 2.16kg), mesh number is 7-18 mesh.
The principle of PE modified pitch is, in pitch adding PE particles through certain technique, (particle size is 1.18-
After 2.36mm), PE particles in order to reduce surface free energy, some of pitch close component of structure can by PE particle absorptions,
In the presence of some light components, PE particles are swelled, and by such process, change the aggregated structure group of pitch
Into adding its viscosity；In addition, when adding PE particles in the pitch of melting, being dissolved after being heated, become by crystalline state and turn to amorphous
State, polyethylene is evenly distributed in the presence of mechanical agitation in pitch, while the wax point that polyethylene inner is penetrated into pitch
Son, volume is expanded and (is swelled), and originally regular Polyethylene Chain is extended, and is crystallized again after the cooling period, at this moment
Certain change can occur for polyethylene crystal.
Additive is carboxy-modified graphene oxide, and its structural formula is：
The present invention carboxy-modified graphene oxide be graphene through a kind of functionalization graphene obtained from peroxidating, on
Stating graphene oxide has the form crystal lattice of similar graphene, because functional group is the least a portion of carbon atom of substitution,
The crystalline element lattice of overall graphene are not destroyed, so above-mentioned graphene oxide still maintains the crystallinity of graphene
Matter, simply connects some functional groups on two-dimentional basal plane.Carboxy-modified graphene oxide is different from graphene, on its surface
Still exist in a large amount of oxygen-containing functional groups, plane containing-OH and-C-O-C, contain-COOH at its lamella edge, due to only on side
Edge carboxylated is without destroying middle carbon structure, therefore carboxylated graphene oxide has the stronger energy for participating in chemical reaction
Power.
Above-mentioned graphene oxide sheet surface and edge have a large amount of carboxyls, and the hydrogen on carboxyl has ionization tendency so that
Acidity is presented in carboxylic acid in aqueous, with good wettability and surface-active, so that can be in diluted alkaline water and pure
Disperse in water and form stable colloidal suspensions.But organic solvent is different from water, it can not be penetrated between graphene oxide layer
Space and destroy these hydrogen bonds and be allowed to peel off.The density of main group is reduced if reducing hydrogen bond by chemical functional groupization,
The intensity of interlayer hydrogen bond will be weakened, then can reduce the hydrophily of graphene oxide layer, so that it is in organic solvent
Peeling be possibly realized.The present invention is modified using organic isocyanate (cationic surfactant), so as to increase modification
The lipophile of graphene oxide, so as to promote the compatibility between modified graphene oxide and pitch, promotes modified graphite oxide
Alkene and pitch formation nanodispersion system.Therefore, carboxy-modified graphene oxide can generally there are boundary such as interfacial agent
Face, and reduce the energy between interface.On the one hand the compatibility of pitch and PE particles is promoted so that graphene oxide modified PE is modified
The storage stability of pitch is improved；On the other hand the viscosity of pitch can be reduced, so as to greatly improve PE modified pitch
Work workability so that PE modified pitch and the parcel that gathers materials are more complete, so as to improve the adhesiveness of PE modified asphalt mixtures.
In addition, graphene be it is most thin at present be but also most hard nano material, itself has very high intensity, can be with
Promote the coaction state between building stones, pitch and PE, the stress shape inside PE modified pitch can be changed from nanometer aspect
State, so as to improve the rutting resistance of PE modified asphalt mixtures.
<The preparation method of polyethylene modified asphalt based on carboxy-modified graphene oxide>
A kind of preparation method according to the above-mentioned polyethylene modified asphalt based on carboxy-modified graphene oxide, it includes
Following steps：
(1) pitch, is heated to the first temperature, is stirred after being subsequently added into modifying agent shearing, obtains modified pitch；
(2) additive, is added in modified pitch to continue to shear, until additive is scattered in modified pitch, obtains base
In the polyethylene modified asphalt of carboxy-modified graphene oxide.
Wherein, in step (1), the first temperature can be 170-180 DEG C, preferably 170 DEG C.
In step (1), shear rate can be 3000 ± 500r/min, preferably 3000r/min；Shear time can be with
For 30 ± 5min, preferably 30min.
In step (1), mixing time can be 30 ± 5min, preferably 30min.
In step (2), shear rate can be 3000 ± 500r/min, preferably 3000r/min；Shear time can be with
For 20 ± 10min, preferably 20min.
The present invention is first by PE particles and pitch high speed shear and stirring to obtain cementitious matter, then by modified graphene oxide
High speed shear is carried out with the particle modified pitches of PE and stirring completes scattered, and during mixing and stirring, modified graphene oxide can promote
The compatibility entered between pitch and PE particles, and from Nano grade to PE modified pitch carry out performance boost, improve adhesiveness and
Storage stability performance.
Below in conjunction with illustrated embodiment and comparative example, the present invention is further illustrated.
Embodiment 1：
The preparation method of the polyethylene modified asphalt based on carboxy-modified graphene oxide of the present embodiment includes following step
Suddenly：
(1) pitch, is heated to 170 DEG C of the first temperature, 5 parts of low density polyethylene (LDPE) particles are then added in above-mentioned pitch
Sheared, shear rate is 3000r/min, shear time is 30min, then stir 30min and obtain modified pitch；
(2), add 1 part of carboxy-modified graphene oxide in above-mentioned modified pitch to continue to shear, shear rate is
3000r/min, shear time is 20min, until carboxy-modified graphene oxide is dispersed in above-mentioned modified pitch, is obtained
Polyethylene modified asphalt based on carboxy-modified graphene oxide.
Wherein, in step (1), the first temperature is possible within 170-180 DEG C.
In step (1), shear rate is possible within 3000 ± 500r/min, shear time 30 ± 5min it
It is interior also possible.
In step (1), mixing time is possible within 30 ± 5min.
In step (2), shear rate is possible within 3000 ± 500r/min, and shear time is in 20 ± 10min
Within it is also possible.
Embodiment 2：
The preparation method of the polyethylene modified asphalt based on carboxy-modified graphene oxide of the present embodiment includes following step
Suddenly：
(1) pitch, is heated to 180 DEG C of the first temperature, 5 parts of low density polyethylene (LDPE) particles are then added in above-mentioned pitch
Sheared, shear rate is 3200r/min, shear time is 30min, then stir 30min and obtain modified pitch；
(2), add 1 part of carboxy-modified graphene oxide in above-mentioned modified pitch to continue to shear, shear rate is
3000r/min, shear time is 20min, until carboxy-modified graphene oxide is dispersed in above-mentioned modified pitch, is obtained
Polyethylene modified asphalt based on carboxy-modified graphene oxide.
Embodiment 3：
The preparation method of the polyethylene modified asphalt based on carboxy-modified graphene oxide of the present embodiment includes following step
Suddenly：
(1) pitch, is heated to 175 DEG C of the first temperature, 5 parts of low density polyethylene (LDPE) particles are then added in above-mentioned pitch
Sheared, shear rate is 3400r/min, shear time is 30min, then stir 30min and obtain modified pitch；
(2), add 1 part of carboxy-modified graphene oxide in above-mentioned modified pitch to continue to shear, shear rate is
3000r/min, shear time is 20min, until carboxy-modified graphene oxide is dispersed in above-mentioned modified pitch, is obtained
Polyethylene modified asphalt based on carboxy-modified graphene oxide.
Comparative example 1：
The preparation method of the common polythene modified pitch of this comparative example comprises the following steps：
Pitch is heated to 170 DEG C of the first temperature, 5 parts of low density polyethylene (LDPE) particles are then added in above-mentioned pitch is carried out
Shearing, shear rate is 3000r/min, and shear time is 30min, then stirs 30min and obtains common polythene modified pitch.
Comparative example 2：
The preparation method of the polyethylene modified asphalt based on modified graphene oxide of this comparative example comprises the following steps：
(1) pitch, is heated to 180 DEG C of the first temperature, 5 parts of low density polyethylene (LDPE) particles are then added in above-mentioned pitch
Sheared, shear rate is 3200r/min, shear time is 30min, then stir 30min and obtain modified pitch；
(2), add 1 part of modified graphene oxide in above-mentioned modified pitch to continue to shear, shear rate is 3000r/
Min, shear time is 20min, until modified graphene oxide is dispersed in above-mentioned modified pitch, is obtained based on modified oxygen
The polyethylene modified asphalt of graphite alkene.
Comparative example 3：
The preparation method of the polyethylene modified asphalt based on modified graphene oxide of this comparative example comprises the following steps：
(1) pitch, is heated to 175 DEG C of the first temperature, 5 parts of low density polyethylene (LDPE) particles are then added in above-mentioned pitch
Sheared, shear rate is 3400r/min, shear time is 30min, then stir 30min and obtain modified pitch；
(2), add 1 part of modified graphene oxide in above-mentioned modified pitch to continue to shear, shear rate is 3000r/
Min, shear time is 20min, until modified graphene oxide is dispersed in above-mentioned modified pitch, is obtained based on modified oxygen
The polyethylene modified asphalt of graphite alkene.
The forming method of above-described embodiment and the compound rut test piece of comparative example, marshal piece and compound according to
Chinese transportation portion《Highway engineering pitch and Asphalt Mixture Experiment code》Standard method as defined in JTJ052-2000 is carried out, its
The temperature of mixing and stirring of middle compound is 175 DEG C, and forming temperature is 175 DEG C, and rut test piece roller-compaction number of times is 12 times, and according in
Ministry of Communications of state《Highway engineering pitch and Asphalt Mixture Experiment code》Its pitch is tested in standard method as defined in JTJ052-2000
Compound wheel tracking test dynamic stability and asphalt Tensile Strength Ratio, test result such as table 1：
The performance test value of each embodiment of table 1 and comparative example
As can be seen from Table 1：The dynamic stability of the asphalt of embodiment is mixed apparently higher than the pitch of comparative example
Expect dynamic stability.By the comparison of embodiment 1 and comparative example 1 it can be found that same stages match somebody with somebody and asphalt content in the case of, oxidation
The raising effect for anti-rut behavior of the PE modified asphalt mixtures of graphene is substantially better than the effect of the anti-rut agents such as PE；
By embodiment 2, embodiment 3 and comparative example 2, comparative example 3 comparison it can be found that same stages match somebody with somebody and pitch consumption feelings
Under condition, it is far superior to merely using PE modified pitch using the anti-rut behavior of the PE modified asphalt mixtures of graphene oxide
Compound.It is possible thereby to illustrate, graphene oxide has obvious effect for improving the anti-rut behavior of PE modified asphalt mixtures
Really.Aoxidized by the comparison of embodiment 1 to embodiment 3 and comparative example 1 to the residual stability of comparative example 3 it can be found that using
The embodiment 1 that graphene is modified is to embodiment 3, and its residual stability has reached more than 80%, and graphene oxide is not used
Composite modified comparative example 1 is to comparative example 3, and its residual stability is universal in 50-60%, illustrates that graphene oxide is modified for PE
The raising of asphalt adhesion serves important function.
The above-mentioned description to embodiment is that this hair is understood that and used for the ease of those skilled in the art
It is bright.Those skilled in the art obviously can readily make various modifications to these embodiments, and described herein one
As principle be applied in other embodiment, without passing through performing creative labour.Therefore, the invention is not restricted to above-described embodiment.
Those skilled in the art do not depart from improvement that scope of the invention made and change all should be at these according to the principle of the present invention
Within the protection domain of invention.
Claims (9)
1. a kind of polyethylene modified asphalt based on carboxy-modified graphene oxide, it is characterised in that：It includes following parts by weight
Component：
100 parts of pitch,
0.5-3.0 parts of additive,
3-7 parts of modifying agent.
2. the polyethylene modified asphalt according to claim 1 based on carboxy-modified graphene oxide, it is characterised in that：Institute
State the one kind of pitch in Esso 70# pitches and SK70# pitches.
3. the polyethylene modified asphalt according to claim 1 based on carboxy-modified graphene oxide, it is characterised in that：Institute
Modifying agent is stated for low density polyethylene (LDPE) particle, density is 0.915-0.940g/cm3, melt index is 1.5-1.8g/10mim
(230 DEG C, 2.16kg), mesh number is 7-18 mesh.
4. the polyethylene modified asphalt according to claim 1 based on carboxy-modified graphene oxide, it is characterised in that：Institute
Additive is stated for carboxy-modified graphene oxide.
5. a kind of polyethylene modified asphalt based on carboxy-modified graphene oxide according to claim any one of 1-4
Preparation method, it is characterised in that：It comprises the following steps：
(1) pitch, is heated to the first temperature, is stirred after being subsequently added into modifying agent shearing, obtains modified pitch；
(2), add additive in the modified pitch to continue to shear, until the additive is scattered in the modified pitch
In, obtain the polyethylene modified asphalt based on carboxy-modified graphene oxide.
6. preparation method according to claim 5, it is characterised in that：In the step (1), the first temperature is 170-180
℃。
7. preparation method according to claim 5, it is characterised in that：In the step (1), shear rate be 3000 ±
500r/min, shear time is 30 ± 5min.
8. preparation method according to claim 5, it is characterised in that：In the step (1), mixing time be 30 ±
5min。
9. preparation method according to claim 5, it is characterised in that：In the step (2), shear rate be 3000 ±
500r/min, shear time is 20 ± 10min.
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| CN109943083A (en) * | 2019-02-20 | 2019-06-28 | 庄文琴 | A kind of preparation method of stretch-proof compound rubber asphalt mixture |
| CN111983321A (en) * | 2020-08-19 | 2020-11-24 | 南京林业大学 | Preparation and electric heating performance evaluation method of nano graphene oxide modified asphalt mixture |
| CN112521761A (en) * | 2020-11-06 | 2021-03-19 | 广州盛门新材料科技有限公司 | Graphene asphalt additive and preparation method thereof |
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Application publication date: 20171013 |