CN110358314A - A kind of preparation method of graphene composite asphalt - Google Patents
A kind of preparation method of graphene composite asphalt Download PDFInfo
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- CN110358314A CN110358314A CN201910601761.5A CN201910601761A CN110358314A CN 110358314 A CN110358314 A CN 110358314A CN 201910601761 A CN201910601761 A CN 201910601761A CN 110358314 A CN110358314 A CN 110358314A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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Abstract
The present invention discloses a kind of preparation method of graphene composite asphalt, comprising the following steps: A, prepares graphene alcohol dispersion liquid: the graphene powder comprising surfactant being mixed with dehydrated alcohol, ultrasonic disperse is carried out, obtains graphene alcohol dispersion liquid；B, graphene composite asphalt product is prepared: by pitch heating melting, the pitch of graphene alcohol dispersion liquid and molten condition made from step A is mixed in the ratio of 1-2.5:10-14,50-80min is stirred, graphene composite asphalt mixture is obtained, up to graphene composite asphalt product after drying.Graphene and pitch of the invention faster and can be mixed more fully, simple process, shorten the production cycle, and the softening point and viscosity of modified pitch are all improved.
Description
Technical field
The invention belongs to chemical field, specially a kind of preparation method of graphene composite asphalt.
Background technique
Since the property of pitch raw material limits, always there are various defects in pitch, for example high temperature is soft in use
There is different degrees of aging in different bad borders in change, cold cracking, pit slot etc..The excellent properties of carbon based nano-material can
So that the property of pitch is improved.
However, when carbon based nano-material is added in matrix pitch, due to meeting when carbon based nano-material is added to a certain amount of
There is agglomeration, it is therefore necessary to carry out decentralized processing.During decentralized processing, the selection of decentralized medium is particularly important, existing
Have in technology and is mixed using additive SBS and carbon based nano-material with matrix pitch, it is not only at high cost, and also the process time is long.
In the modification of carbon based nano-material, if the carbon based nano-material added in matrix pitch is more, it can make
Product cost is excessively high, uneconomical；If the carbon based nano-material of addition is less, the carbon based nano-material in pitch can not fill
Divide and play a role, ideal modified effect is not achieved.
Summary of the invention
The present invention, aiming to the above problems, provides a kind of preparation methods of graphene composite asphalt, do dispersion with dehydrated alcohol and are situated between
Matter prepares dispersion liquid, and then graphene alcohol dispersion liquid is added in matrix pitch, enable the two faster and more fully
Mixing, simple process shorten the production cycle, and the softening point and viscosity of modified pitch are all improved.
In order to achieve the above objectives, technical scheme is as follows:
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, it prepares graphene alcohol dispersion liquid: the graphene powder comprising surfactant being mixed with dehydrated alcohol, is surpassed
Sound dispersion, obtains graphene alcohol dispersion liquid；
B, it prepares graphene composite asphalt product: pitch heating melting by graphene alcohol dispersion liquid made from step A and melts
The pitch for melting state is mixed in the ratio of 1-2.5:10-14, is stirred 50-80min, is obtained graphene composite asphalt mixture, does
Up to graphene composite asphalt product after dry.
Further, the preparation method of the graphene powder comprising surfactant is the following steps are included: by graphite
Alkene powder is mixed with neopelex, polyvinylpyrrolidone and water, is carried out decentralized processing, is obtained graphene mixing slurry
Material obtains the graphene powder comprising surfactant after dry.
Further, the mass percentage composition of the graphene mixed slurry are as follows: neopelex 0.5 ‰-
2%, polyvinylpyrrolidone 0.5 ‰ -2%, graphene 1%-5%, remaining is water.
Further, the method for the decentralized processing is one of ultrasonic disperse, homogeneous, shearing, grinding or one kind
Above combination；
The time of the ultrasonic disperse is 0.2-0.4h, and the time of homogeneous is 4-6.5h, and the time of shearing is 0.5-2h, grinding
Time be 5-7h.
Further, the temperature of the drying is 130-180 DEG C, and the dry time is 20-28 h.
Further, the partial size of the graphite composite powder comprising surfactant is 5-140 μm.
Further, the graphene powder in the step A comprising surfactant accounts for the matter of graphene alcohol dispersion liquid
Amount degree is 0.03%-0.2%.
Further, the time of ultrasonic disperse is 50-100 min in the step A.
Further, the whipping temp in the step B is 100-200 DEG C.
Further, temperature dry in the step B is 50-80 DEG C, and the dry time is 5-10 h.
The invention has the benefit that
Inventor has found by numerous studies, dehydrated alcohol can more preferable dispersed graphite alkene powder, after dehydrated alcohol disperses
Graphene and pitch compound tense, initial viscosity is relatively low, is easy to stir evenly.
The present invention is poly- using anionic surfactant sodium dodecylbenzene sulfonate (SDBS) and nonionic surfactant
Vinylpyrrolidone (PVP) combination is used as surfactant, and the graphene powder comprising surfactant prepared is dripping
There are very outstanding uniform and stable disperse properties in blueness, can effectively substitute expensive CNT, Al2O3Etc. prior arts dispersing agent
Material.
Using with heterocycle structure anionic surfactant and anionic surfactant matched combined as surface
Activating agent can form more stable π-π interaction with graphene, while alkane long-chain is existed by negative electron exchange adsorption
Graphene surface overcomes the Van der Waals force between graphene sheet layer, forms steric hindrance and electrostatic steric effect overcomes graphene
Agglomeration traits, and the hydrophilic group on heterocycle can improve the hydrophily at graphene interface, and pass through electrostatic repulsion forces and space
Steric hindrance realizes the uniform and stable dispersion of graphene in pitch, so as to improve the agglomeration traits of graphene in pitch.
Moreover, inventor also found after study, pitch made of prepared by the method graphene alcohol dispersion liquid,
With very outstanding softening point and viscosity, as described in Example 16, the stone that mass fraction is 0.05% is added in No. 10 pitches
Its softening point of black alkene has reached 105.2 DEG C, increases 7.2 DEG C than original 98 DEG C；And for No. 70 pitches, in graphene
Its softening point has reached 59.6 DEG C when being added to 0.20%, improves for 51.8 DEG C of softening point than being not added with graphene originally
7.8 degree Celsius；For No. 10 pitches, viscosity value reaches when adding 0.05% graphene, viscosity is at 150 DEG C
7340mPa.s；For No. 70 pitches, viscosity when viscosity when adding the graphene that mass fraction is 0.20% is at 100 DEG C reaches
4660mPa.s is arrived.
Graphene alcohol dispersion liquid of the present invention has carried out ultrasonic disperse, inventor has found that relative to other dispersions
Means, ultrasound can increase the hydrophily of graphene, promote its stable dispersion in pitch.
The present invention is first surface-treated with neopelex, polyvinylpyrrolidone, carries out functionalized modification, then
Decentralized medium is done with dehydrated alcohol and prepares graphene dispersing solution, and then graphene alcohol dispersion liquid is added in matrix pitch, is made
Obtaining graphene can faster and more fully mix with pitch, and simple process shortens the production cycle, the softening of modified pitch
Point and viscosity are all improved.
Detailed description of the invention
Fig. 1 is the softening point data of the graphene comprising surfactant and No. 10 Asphalt compositions；
Fig. 2 is the softening point data of the graphene comprising surfactant and No. 70 Asphalt compositions；
Fig. 3 is the viscosity data of the graphene comprising surfactant and No. 10 Asphalt compositions；
Fig. 4 is the viscosity data of the graphene comprising surfactant and No. 70 Asphalt compositions.
Specific embodiment
Below by specific embodiment, the present invention is described in detail.
Embodiment 1
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene powder, neopelex, polyvinyl pyrrole
The mixing of alkanone water, then carries out 12 min of ultrasonic disperse, grinds 5 h, obtains graphene mixed slurry, wherein graphene mixing
The mass percentage composition of slurry are as follows: neopelex 0.5 ‰, polyvinylpyrrolidone 0.5 ‰, graphene 1%,
Yu Weishui；Graphene mixed slurry obtains the graphene comprising surfactant that partial size is 5 μm after drying 20 h at 130 DEG C
Powder；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 50 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.03%；
C, graphene composite asphalt product is prepared: by pitch heating melting, by graphene alcohol dispersion liquid made from 1kg step B
It is mixed with the pitch of 10kg molten condition, 50 min is stirred at 100 DEG C, obtain graphene composite asphalt mixture, graphene
Mix asphalt mixture dries 5 h at 50 DEG C to get graphene composite asphalt product.
Embodiment 2
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene powder and neopelex, polyethylene pyrrole
Pyrrolidone, water mixing, then carry out 14 min of ultrasonic disperse, 6.5 h of homogeneous obtains graphene mixed slurry, wherein graphene
The mass percentage composition of mixed slurry are as follows: neopelex 0.8 ‰, polyvinylpyrrolidone 0.8 ‰, graphene
1.5%, remaining is water；Graphene mixed slurry obtains partial size after drying 21 h at 140 DEG C as 10 μm comprising surfactant
Graphene powder；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 55 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.05%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.2kg step B
Liquid is mixed with the pitch of 10.3kg molten condition, and 52 min are stirred at 110 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 6 h at 52 DEG C to get graphene composite asphalt product.
Embodiment 3
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene powder and neopelex, polyethylene pyrrole
Pyrrolidone, water mixing, then carry out 15 min of ultrasonic disperse, 6 h of homogeneous, shear 30 min, grind 5.5 h, obtain graphene
Mixed slurry, wherein the mass percentage composition of graphene mixed slurry are as follows: neopelex 0.1%, polyethylene pyrrole
Pyrrolidone 0. 1%, graphene 2%, remaining is water；It is 20 μm that graphene mixed slurry, which dries at 150 DEG C and obtains partial size after 22 h,
The graphene powder comprising surfactant；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 60 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.08%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.5 kg step B
Liquid is mixed with the pitch of 11kg molten condition, and 55 min are stirred at 120 DEG C, obtains graphene composite asphalt mixture, graphite
Alkene mix asphalt mixture dries 7 h at 55 DEG C to get graphene composite asphalt product.
Embodiment 4
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 17 min of ultrasonic disperse, shear 50 min, grind 6 h, obtain graphene mixed slurry, wherein
The mass percentage composition of graphene mixed slurry are as follows: neopelex 0.3%, polyvinylpyrrolidone 0.3%, graphite
Alkene 2.5%, remaining is water；Graphene mixed slurry obtains partial size after drying 23 h at 155 DEG C as 30 μm comprising surface-active
The graphene powder of agent；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 65 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.1%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.2kg step B
Liquid is mixed with the pitch of 11.4kg molten condition, and 58 min are stirred at 130 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 8 h at 58 DEG C to get graphene composite asphalt product.
Embodiment 5
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by black alkene and neopelex, polyvinylpyrrolidone,
Water mixing, then carries out 4 h of homogeneous, shears 1 h, grinds 6.8 h, obtains graphene mixed slurry, wherein graphene mixing slurry
The mass percentage composition of material are as follows: neopelex 0.5%, polyvinylpyrrolidone 0.5%, graphene 3%, remaining is
Water；Graphene mixed slurry obtains the Graphene powder comprising surfactant that partial size is 40 μm after drying 24 h at 160 DEG C
Body；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 70 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.12%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.5kg step B
Liquid is mixed with the pitch of 12kg molten condition, and 60 min are stirred at 140 DEG C, obtains graphene composite asphalt mixture, graphite
Alkene mix asphalt mixture dries 9 h at 60 DEG C to get graphene composite asphalt product.
Embodiment 6
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 20 min of ultrasonic disperse, 1 h of homogeneous, shear 65 min, obtain graphene mixed slurry, wherein
The mass percentage composition of graphene mixed slurry are as follows: neopelex 0.7%, polyvinylpyrrolidone 0.7%, graphite
Alkene 3.5%, remaining is water；Graphene mixed slurry obtains partial size after drying 25 h at 162 DEG C as 50 μm comprising surface-active
The graphene powder of agent；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 75 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.14%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.6kg step B
Liquid is mixed with the pitch of 12.3kg molten condition, and 62 min are stirred at 150 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 10 h at 62 DEG C to get graphene composite asphalt product.
Embodiment 7
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 6.5 h of homogeneous, shear 1.2 h, obtain graphene mixed slurry, wherein graphene mixed slurry
Mass percentage composition are as follows: neopelex 0.9%, polyvinylpyrrolidone 0.9%, graphene 4%, remaining is water；
Graphene mixed slurry obtains the graphene powder comprising surfactant that partial size is 60 μm after drying 26 h at 164 DEG C；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 80 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.15%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.8kg step B
Liquid is mixed with the pitch of 12.4kg molten condition, and 64 min are stirred at 160 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 8 h at 65 DEG C to get graphene composite asphalt product.
Embodiment 8
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 18 min of ultrasonic disperse, 4.8 h of homogeneous, shear 1.5 h, grind 7 h, obtain graphene mixing slurry
Material, wherein the mass percentage composition of graphene mixed slurry are as follows: neopelex 1%, polyvinylpyrrolidone 1%,
Graphene 4.5%, remaining is water；Graphene mixed slurry obtains partial size after drying 27 h at 165 DEG C as 70 μm comprising surface
The graphene powder of activating agent；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 85 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.16%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.8kg step B
Liquid is mixed with the pitch of 12.6kg molten condition, and 66 min are stirred at 170 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 5 h at 64 DEG C to get graphene composite asphalt product.
Embodiment 9
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 24 min of ultrasonic disperse, obtain graphene mixed slurry, wherein the quality of graphene mixed slurry
Percentage composition are as follows: neopelex 1.2%, polyvinylpyrrolidone 1.2%, graphene 5%, remaining is water；Graphene
Mixed slurry obtains the graphene powder comprising surfactant that partial size is 80 μm after drying 28 h at 166 DEG C；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 90 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.18%；
C, graphene composite asphalt product is prepared: by pitch heating melting, by graphene alcohol dispersion liquid made from 2kg step B
It is mixed with the pitch of 12kg molten condition, 68 min is stirred at 180 DEG C, obtain graphene composite asphalt mixture, graphene
Mix asphalt mixture dries 6 h at 65 DEG C to get graphene composite asphalt product.
Embodiment 10
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 5.8 h of grinding, obtain graphene mixed slurry, wherein the quality percentage of graphene mixed slurry
Than composition are as follows: neopelex 1.4%, polyvinylpyrrolidone 1.4%, graphene 4.5%, remaining is water；Graphene is mixed
It closes after slurry dries 23 h at 166.5 DEG C and obtains the graphene powder comprising surfactant that partial size is 90 μm；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 95 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.2%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.9kg step B
Liquid is mixed with the pitch of 11.3kg molten condition, and 70 min are stirred at 190 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 7 h at 68 DEG C to get graphene composite asphalt product.
Embodiment 11
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 5 h of homogeneous, grind 6.4 h, obtain graphene mixed slurry, wherein graphene mixed slurry
Mass percentage composition are as follows: neopelex 1.6%, polyvinylpyrrolidone 1.6%, graphene 4%, remaining is water；Stone
Black alkene mixed slurry obtains the graphene powder comprising surfactant that partial size is 100 μm after drying 24 h at 167 DEG C；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 100 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.03%；
C, prepare graphene composite asphalt product: by pitch at 200 DEG C heating melting, by graphene made from 1.2kg step B
Alcohol dispersion liquid is mixed with the pitch of 10.8kg molten condition, and 72 min are stirred at 200 DEG C, and it is mixed to obtain graphene composite asphalt
Object is closed, graphene mix asphalt mixture dries 8 h at 70 DEG C to get graphene composite asphalt product.
Embodiment 12
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 2 h of shearing, grind 6.5 h, obtain graphene mixed slurry, wherein graphene mixed slurry
Mass percentage composition are as follows: neopelex 1.8%, polyvinylpyrrolidone 1.8%, graphene 3.5%, remaining is water；
Graphene mixed slurry obtains the graphene powder comprising surfactant that partial size is 110 μm after drying 25 h at 164 DEG C；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 88 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.05%；
B, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.3kg step B
Liquid is mixed with the pitch of 10.8kg molten condition, and 70 min are stirred at 195 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 9 h at 75 DEG C to get graphene composite asphalt product.
Embodiment 13
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene and neopelex, polyvinylpyrrolidine
Ketone, water mixing, then carry out 19 min of ultrasonic disperse, grind 5.8 h, obtain graphene mixed slurry, wherein graphene mixing
The mass percentage composition of slurry are as follows: neopelex 2%, polyvinylpyrrolidone 2%, graphene 5%, remaining is water；
Graphene mixed slurry obtains the graphene powder comprising surfactant that partial size is 120 μm after drying 26 h at 168 DEG C；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 78 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.08%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 1.4kg step B
Liquid is mixed with the pitch of 10.6kg molten condition, and 76 min are stirred at 155 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 10 h at 78 DEG C to get graphene composite asphalt product.
Embodiment 14
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene powder and neopelex, polyethylene pyrrole
Pyrrolidone, water mixing, then carry out 23 min of ultrasonic disperse, grind 6.2 h, obtain graphene mixed slurry, wherein graphene
The mass percentage composition of mixed slurry are as follows: neopelex 1%, polyvinylpyrrolidone 1%, graphene 1%, remaining
For water；Graphene mixed slurry obtains the graphene comprising surfactant that partial size is 130 μm after drying 27 h at 170 DEG C
Powder；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 80 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.1%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 2.1kg step A
Liquid is mixed with the pitch of 12.4kg molten condition, and 50 min are stirred at 100 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 5 h at 50 DEG C to get graphene composite asphalt product.
Embodiment 15
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene powder and neopelex, polyethylene pyrrole
Pyrrolidone, water mixing, then carry out ultrasonic disperse 17min, grind 6.4 h, obtain graphene mixed slurry, wherein graphene
The mass percentage composition of mixed slurry are as follows: neopelex 1.7%, polyvinylpyrrolidone 1.8%, graphene 3%,
Remaining is water；Graphene mixed slurry obtains the stone comprising surfactant that partial size is 135 μm after drying 20 h at 172 DEG C
Black alkene powder；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 90 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.12%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 2.1kg step A
Liquid is mixed with the pitch of 12.6kg molten condition, and 80 min are stirred at 120 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 6 h at 60 DEG C to get graphene composite asphalt product.
Embodiment 16
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene powder and neopelex, polyethylene pyrrole
Pyrrolidone, water mixing, then carry out 12 min of ultrasonic disperse, grind 6 h, shear 1 h, obtain graphene mixed slurry, wherein
The mass percentage composition of graphene mixed slurry are as follows: neopelex 1%, polyvinylpyrrolidone 1%, graphene
2%, remaining is water；Graphene mixed slurry obtains partial size after drying 22 h at 178 DEG C as 140 μm comprising surfactant
Graphene powder；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 88 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.18%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 2.3kg step A
Liquid is mixed with the pitch of 13.6kg molten condition, and 80 min are stirred at 140 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 7 h at 65 DEG C to get graphene composite asphalt product.
Embodiment 17
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene powder and neopelex, polyethylene pyrrole
Pyrrolidone, water mixing, then carry out 21 min of ultrasonic disperse, 4 h of homogeneous, grind 6 h, obtain graphene mixed slurry, wherein
The mass percentage composition of graphene mixed slurry are as follows: neopelex 1%, polyvinylpyrrolidone 2%, graphene
1%, remaining is water；Graphene mixed slurry obtains partial size after drying 20 h at 180 DEG C as 100 μm comprising surfactant
Graphene powder；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 70 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.2%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 2.5kg step A
Liquid is mixed with the pitch of 14kg molten condition, and 80 min are stirred at 160 DEG C, obtains graphene composite asphalt mixture, graphite
Alkene mix asphalt mixture dries 8 h at 70 DEG C to get graphene composite asphalt product.
Embodiment 18
The preparation method of graphene composite asphalt of the invention, comprising the following steps:
A, preparation includes the graphene powder of surfactant: by graphene powder and neopelex, polyethylene pyrrole
Pyrrolidone, water mixing, then carry out 23 min of ultrasonic disperse, grind 5 h, obtain graphene mixed slurry, wherein graphene is mixed
Close the mass percentage composition of slurry are as follows: neopelex 2%, polyvinylpyrrolidone 2%, graphene 4%, remaining is
Water；Graphene mixed slurry obtains the Graphene powder comprising surfactant that partial size is 110 μm after drying 25 h at 145 DEG C
Body；
B, it prepares graphene alcohol dispersion liquid: will include the graphene powder and dehydrated alcohol of surfactant made from step A
Mixing carries out 80 min ultrasonic disperses, obtains graphene alcohol dispersion liquid；Wherein, comprising the graphene powder of surfactant
The mass percentage content for accounting for graphene alcohol dispersion liquid is 0.08%；
C, it prepares graphene composite asphalt product: pitch heating melting disperses graphene ethyl alcohol made from 2.4kg step A
Liquid is mixed with the pitch of 13.5kg molten condition, and 80 min are stirred at 200 DEG C, obtains graphene composite asphalt mixture, stone
Black alkene mix asphalt mixture dries 10 h at 80 DEG C to get graphene composite asphalt product.
19 graphene composite asphalt performance measurement of embodiment
One, graphene composite asphalt softening point measurement
Using the softening point of asphalt softening point tester measurement bitumen samples.
Application method:
(1) bitumen samples are melted using oil bath pan；
(2) copper ring is slightly heated, is put on metal plate, bitumen samples will have been melted and poured into copper ring, be until filling copper ring
Only；
(3) when copper ring temperature drops to room temperature, copper ring is clamped with ring, sample blade scrapes off copper ring and overflows the sample of coming, makes
The upper surface and copper ring edge of its bitumen samples are to it；
(4) copper ring for being placed with bitumen samples is put into the circular hole on metal frame middle plate, loads onto locator and standard small ball,
Then metal is placed in the beaker for filling standard solution, any part should not all have bubble, then be inserted into thermometer, make
It is flushed below mercury ball lower end and copper ring；
(5) beaker is put on asbestos gauge, starts the heating that uniformly heats up by initial temperature temperature and heating rate as defined in table, surpasses
The experiment of regulation heating rate is crossed to cancel；
(6) thermometer is read immediately when bitumen samples are sagging as the temperature rises and gradually, just contacted metal frame lower plywood
Temperature takes the arithmetic mean of instantaneous value of two ring sample softening temperatures, the softening point as sample.
This softening point measurement carries out two groups of experiments altogether.
1. it is compound as laboratory sample to select No. 10 pitches to carry out according to following 5 kinds of processing modes:
1. sample 1: blank control, i.e. not No. 10 pitches of containing graphene；
2. sample 2: the graphene composite asphalt product being prepared according to the preparation method of embodiment 1 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.03%；
3. sample 3: the graphene composite asphalt product being prepared according to the preparation method of embodiment 2 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.05%；
4. sample 4: the graphene composite asphalt product being prepared according to the preparation method of embodiment 3 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.08%；
5. sample 5: the graphene composite asphalt product being prepared according to the preparation method of embodiment 4 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.1%.
Test results are shown in figure 1.
2. it is compound as laboratory sample to select No. 70 pitches to carry out according to following 4 kinds of processing modes:
1. sample 1: blank control, i.e. not No. 70 pitches of containing graphene；
2. sample 2: the graphene composite asphalt product being prepared according to the preparation method of embodiment 2 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.05%；
3. sample 3: the graphene composite asphalt product being prepared according to the preparation method of embodiment 4 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.1%；
4. sample 4: the graphene composite asphalt product being prepared according to the preparation method of embodiment 10 is comprising surface
The mass percentage content that the graphene of activating agent accounts for graphene alcohol dispersion liquid is 0.2%.
Test results are shown in figure 2.
By Fig. 1 and Fig. 2 it is found that being added in the graphene of different quality in No. 10 pitches, addition mass fraction is 0.05%
Its softening point of graphene highest in each group, reach 105.2 DEG C, increase 7.2 DEG C than original 98 DEG C；And No. 70 are dripped
For blueness, when graphene is added to 0.20%, its softening point highest, has reached 59.6 DEG C, than being not added with the soft of graphene originally
Change and improves 7.8 degrees Celsius for 51.8 DEG C of point.The raising of softening point shows that the high temperature of pitch can be strengthened by adding graphene
Stability.
Two, graphene composite asphalt viscosimetric analysis
Using the viscous drag and hydrodynamic viscosity of NDJ-1 rotary viscosimeter measurement pitch.
Application method:
(1) power supply for connecting viscosity determinator, is arranged temperature；
(2) sample cylinder and rotor are put into togerther constant temperature 90 minutes in instrument；
(3) pitch is added and is melted, is put into the good sample cylinder of constant temperature, pitch is filled with without too full, and liquid level is slightly higher than rotor
Upper cone is just good；
(4) sample cylinder for being filled with pitch is put into Viscometry instrument with fixture；
(5) suitable rotor is selected, rotor is hung on analyzer, the measuring head of viscosimeter is reduced, rotor is inserted into sample cylinder
In；
(6) viscosity determinator is run, observe data, each setting at a temperature of, record three group number-readings, respectively per minute note
Record is primary；
(7) different temperature is arranged to continue to test, totally 10 groups of temperature setting.
This viscosimetric analysis carries out two groups of experiments altogether.
1. it is compound as laboratory sample to select No. 10 pitches to carry out according to following 5 kinds of methods:
1. sample 1: blank control, i.e. not No. 10 pitches of containing graphene；
2. sample 2: the graphene composite asphalt product being prepared according to the preparation method of embodiment 1 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.03%；
3. sample 3: the graphene composite asphalt product being prepared according to the preparation method of embodiment 2 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.05%；
4. sample 4: the graphene composite asphalt product being prepared according to the preparation method of embodiment 3 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.08%；
5. sample 5: the graphene composite asphalt product being prepared according to the preparation method of embodiment 4 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.1%.
Test results are shown in figure 3.
2. it is compound as laboratory sample to select No. 70 pitches to carry out according to following 4 kinds of processing modes:
1. sample 1: blank control, i.e. not No. 70 pitches of containing graphene；
2. sample 2: the graphene composite asphalt product being prepared according to the preparation method of embodiment 2 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.05%；
3. sample 3: the graphene composite asphalt product being prepared according to the preparation method of embodiment 4 is comprising surface is living
Property agent graphene account for graphene alcohol dispersion liquid mass percentage content be 0.1%；
4. sample 4: the graphene composite asphalt product being prepared according to the preparation method of embodiment 10 is comprising surface
The mass percentage content that the graphene of activating agent accounts for graphene alcohol dispersion liquid is 0.2%.
Test results are shown in figure 4.
As can be seen from figs. 3 and 4 viscosity is higher when adding 0.05% graphene for No. 10 pitches, the viscosity at 150 DEG C
Numerical value is 7340mPa.s, and the index of viscosity reduces as the temperature rises；For No. 70 pitches, when addition mass fraction is
Viscosity when 0.20% graphene reaches highest in each group experiment, and the viscosity at 100 DEG C is 4660mPa.s, and viscosity is with temperature
The raising of degree and reduce.As it can be seen that the addition of graphene can promote the viscosity of pitch.
Claims (10)
1. a kind of preparation method of graphene composite asphalt, which comprises the following steps:
A, it prepares graphene alcohol dispersion liquid: the graphene powder comprising surfactant being mixed with dehydrated alcohol, is surpassed
Sound dispersion, obtains graphene alcohol dispersion liquid；
B, it prepares graphene composite asphalt product: pitch heating melting by graphene alcohol dispersion liquid made from step A and melts
The pitch for melting state is mixed in the ratio of 1-2.5:10-14, is stirred 50-80min, is obtained graphene composite asphalt mixture, does
Up to graphene composite asphalt product after dry.
2. the preparation method of graphene composite asphalt according to claim 1, it is characterised in that:
The preparation method of the graphene powder comprising surfactant is the following steps are included: by graphene powder and 12
Sodium alkyl benzene sulfonate, polyvinylpyrrolidone and water mixing, carry out decentralized processing, obtain graphene mixed slurry, obtain after dry
To the graphene powder comprising surfactant.
3. the preparation method of graphene composite asphalt according to claim 2, it is characterised in that: the graphene mixing
The mass percentage composition of slurry are as follows: neopelex 0.5 ‰ -2%, polyvinylpyrrolidone 0.5 ‰ -2%, graphene
1%-5%, remaining is water.
4. the preparation method of graphene composite asphalt according to claim 2, it is characterised in that: the decentralized processing
Method is one of ultrasonic disperse, homogeneous, shearing, grinding or more than one combination；
The time of the ultrasonic disperse is 0.2-0.4h, and the time of homogeneous is 4-6.5h, and the time of shearing is 0.5-2h, is ground
The time of mill is 5-7 hours.
5. the preparation method of graphene composite asphalt according to claim 2, it is characterised in that: the temperature of the drying
It is 130-180 DEG C, the dry time is 20-28 h.
6. the preparation method of graphene composite asphalt according to claim 2, it is characterised in that: described is living comprising surface
Property agent graphite composite powder partial size be 5-140 μm.
7. the preparation method of graphene composite asphalt according to claim 1, it is characterised in that: wrapped in the step A
The mass percentage content that graphene powder containing surfactant accounts for graphene alcohol dispersion liquid is 0.03%-0.2%.
8. the preparation method of graphene composite asphalt according to claim 1, it is characterised in that: surpass in the step A
The time of sound dispersion is 50-100min.
9. the preparation method of graphene composite asphalt according to claim 1, it is characterised in that: in the step B
Whipping temp is 100-200 DEG C.
10. the preparation method of graphene composite asphalt according to claim 1, it is characterised in that: done in the step B
Dry temperature is 50-80 DEG C, and the dry time is 5-10 h.
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