CN113773663B - Asphalt containing modified nano graphene oxide and asphalt mixture - Google Patents
Asphalt containing modified nano graphene oxide and asphalt mixture Download PDFInfo
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- CN113773663B CN113773663B CN202111211324.6A CN202111211324A CN113773663B CN 113773663 B CN113773663 B CN 113773663B CN 202111211324 A CN202111211324 A CN 202111211324A CN 113773663 B CN113773663 B CN 113773663B
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- 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
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention relates to asphalt containing modified nano graphene oxide, which comprises matrix asphalt and modified nano graphene oxide accounting for 0.03-0.06% of the mass of the matrix asphalt, wherein the modified nano graphene oxide is prepared by mixing polyvinylpyrrolidone and nano graphene oxide powder in a mass ratio of 1: (5-6) mixing and preparing. According to the product provided by the invention, a certain amount of nano graphene oxide prepared by a specific method is added into conventional matrix asphalt, so that the comprehensive performance of the asphalt can be comprehensively improved, and the product is more suitable for being used in an extreme environment.
Description
Technical Field
The invention relates to the technical field of road engineering materials, in particular to asphalt containing modified nano graphene oxide and an asphalt mixture.
Background
With the development of economy and the increase of traffic demands, the traffic volume and the axle load of China increase year by year. Meanwhile, with the change of global climate, extreme weather events such as ultra-high temperature weather and sleet frost weather frequently occur in recent years. Asphalt pavements are mostly adopted in roads in China, but in the face of complex road conditions and natural environments, unmodified asphalt cannot bear increasing axle loads and severe weather environments, and the service life of the asphalt pavements is seriously influenced. Therefore, there is an urgent need to develop new asphalt materials to enhance the performance of road asphalt pavement to ensure longer service life under complicated and severe service conditions.
In the prior art, nano graphene oxide is adopted to improve the performance of asphalt. However, the nano graphene oxide has a very large specific surface area and a relatively high surface energy, so that spontaneous agglomeration often occurs, and the nano graphene oxide cannot be well dispersed in asphalt, so that the modification effect of the nano graphene oxide on the asphalt is greatly reduced. Although the method of heating asphalt to reduce viscosity, strong shear stirring or adding dispersant can be adopted to improve the dispersibility of the nano material in the asphalt, the effect is not significant.
At present, development of asphalt and asphalt mixture with excellent comprehensive performance and good use effect is urgently needed.
Disclosure of Invention
The first purpose of the invention is to provide asphalt containing modified nano graphene oxide. The asphalt provided by the invention has excellent comprehensive performance and has good effects on temperature sensitivity, viscosity, plasticity, ageing resistance and the like.
Specifically, the asphalt containing the modified nano graphene oxide provided by the invention comprises matrix asphalt and the modified nano graphene oxide accounting for 0.03-0.06% of the mass of the matrix asphalt.
In some embodiments of the invention, the mass of the modified nano graphene oxide accounts for 0.04-0.05% of the mass of the matrix asphalt.
In some embodiments of the invention, the base asphalt is base asphalt # 70. The modified nano graphene oxide provided by the invention can be well dispersed in the matrix asphalt, and especially can play an optimal synergistic effect with No. 70 matrix asphalt, so that the asphalt with excellent comprehensive performance is obtained.
The modified nano graphene oxide is prepared by the method comprising the following steps:
(1) Mixing and stirring graphite, concentrated sulfuric acid and phosphoric acid, slowly adding potassium permanganate, and stirring for reaction;
(2) Adding deionized water into the reaction liquid obtained in the step (1), adding a hydrogen peroxide solution for reaction, repeatedly washing and centrifuging the obtained reaction product to strip graphite oxide and form nano graphene oxide gel, and drying to obtain nano graphene oxide powder;
(3) Mixing a polyvinylpyrrolidone (PVP) water solution with the nano graphene oxide powder, wherein the mass ratio of the PVP to the nano graphene oxide powder is 1: (5-6), uniformly dispersing by ultrasonic, stirring for reaction, washing and drying.
In some embodiments of the present invention, the stirring reaction in step (1) is performed in an ice bath, a water bath at 30-50 ℃ and a water bath at 80-95 ℃ in this order. Under the conditions, the nano graphene oxide with proper and uniform particle size can be formed.
In some embodiments of the present invention, the repeated washing in step (2) is performed with an acidic aqueous solution, preferably an aqueous solution having a pH of 5.3 to 5.7. Under the conditions, the nano graphene oxide with proper and uniform particle size can be formed.
The invention limits the mass ratio of the polyvinylpyrrolidone in the polyvinylpyrrolidone aqueous solution in the step (3) to the nano graphene oxide powder to be 1: (5 to 6), more preferably 1:5.5. according to the invention, through optimizing the mass ratio of the polyvinylpyrrolidone to the nano graphene oxide powder, the polyvinylpyrrolidone modified nano graphene oxide powder can be dispersed in the matrix asphalt in the best state and dispersion degree and can perform a synergistic effect with the matrix asphalt, so that the optimal modification effect is generated on the matrix asphalt, especially the No. 70 matrix asphalt.
In some embodiments of the present invention, the stirring reaction in step (3) is performed at 32 to 38 ℃ at a pH of 7.6 to 8, and then at 25 to 30 ℃ at a pH of 6.8 to 7.2. According to the invention, by optimizing the conditions of the mixing reaction of polyvinylpyrrolidone and the nano graphene oxide powder, the particle size of the nano graphene oxide powder modified by polyvinylpyrrolidone in a specific proportion can be ensured to be more uniform and the property is more stable, so that the optimal modification effect on the matrix asphalt is generated.
In some embodiments of the present invention, the modified nano graphene oxide powder is prepared by a method comprising the following specific steps:
(1) Mixing 0.15 part of graphite, 34 parts of concentrated sulfuric acid and 3 parts of concentrated phosphoric acid, mechanically stirring for 10 minutes in an ice bath, slowly adding 0.9 part of potassium permanganate, keeping the temperature at 0 ℃, stirring and reacting for 2 hours in the ice bath, then stirring and reacting for 60 minutes in a water bath at 40 ℃, and then adjusting the temperature of the water bath to 95 ℃, stirring and reacting for 60 minutes;
(2) Suspending the reaction product obtained in the step (1) in water, adding 11 parts of hydrogen peroxide for reaction, repeatedly washing and centrifuging the reaction product for 5 times by using a water solution with the pH of 5.5, stripping graphite oxide in the washing process to form nano graphene oxide gel, and drying at 60 ℃ to obtain nano graphene oxide powder;
(3) Adding the nano graphene oxide powder obtained in the step (2) into a PVP (polyvinyl pyrrolidone) aqueous solution, wherein the mass ratio of the PVP to the nano graphene oxide powder is 1:5.5, obtaining a uniformly dispersed colloidal solution through ultrasonic dispersion, firstly carrying out stirring reaction under the conditions of 35 ℃ water bath and pH value of 7.8, then carrying out stirring reaction under the conditions of 28 ℃ water bath and pH value of 7.0, washing colloid obtained after the reaction is finished with deionized water and ethanol, and drying to obtain the modified nano graphene oxide powder.
In some embodiments of the invention, the modified asphalt containing the nano material is prepared by shearing, stirring and mixing the matrix asphalt and the nano graphene oxide at 120-140 ℃ and 2000-5000 r/min.
In a second aspect, the present invention provides an asphalt mixture, wherein the asphalt containing modified nano graphene oxide in the first aspect further contains a mineral mixture with a graded composition containing coarse aggregate, fine aggregate and filler.
The coarse aggregate can be selected from broken stones, broken gravels, screened gravels, slag and the like with grading and particle size meeting requirements; the fine aggregate can be natural sand, artificial sand, stone chips and the like with grading and grain size meeting requirements; the filler is generally mineral powder and the like, the filler plays a role in filling and improving the asphalt performance in the asphalt mixture, and the mineral powder can be obtained by grinding limestone or strong basic rock in the magma rock with gradation and grain size meeting requirements.
The mineral mixture in the asphalt mixture can be selected according to the actual requirements (such as weather conditions, traffic properties, construction conditions and the like) of asphalt pavement construction by referring to national standards and methods disclosed in the prior art.
In a third aspect, the invention protects the application of the asphalt containing the modified nano graphene oxide in the first aspect or the asphalt mixture in the second aspect in asphalt pavement construction.
Compared with the prior art, the asphalt containing the modified nano graphene oxide provided by the invention is added with a small amount of nano graphene oxide prepared by a specific method in the conventional matrix asphalt, so that the comprehensive performance of the asphalt can be comprehensively improved, and the temperature sensitivity, viscosity, plasticity and aging resistance of the asphalt are improved to different degrees, thereby being more suitable for being used in extreme environments.
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
Example 1
The embodiment provides an asphalt containing modified nano graphene oxide, which specifically comprises the following components: 100g of No. 70 matrix asphalt and 0.05g of modified nano graphene oxide;
the modified nano graphene oxide is prepared by the following method:
(1) Mixing 0.15g of graphite with 34g of concentrated sulfuric acid and 3g of concentrated phosphoric acid, mechanically stirring for 10 minutes in an ice bath, slowly adding 0.9g of potassium permanganate, keeping the temperature at 0 ℃, stirring and reacting for 2 hours in the ice bath, then stirring and reacting for 60 minutes in a water bath at 40 ℃, and then adjusting the temperature of the water bath to 95 ℃, and stirring and reacting for 60 minutes;
(2) Suspending the reaction product obtained in the step (1) in water, adding 11g of hydrogen peroxide for reaction, repeatedly washing and centrifuging the reaction product for 5 times by using a water solution with the pH value of 5.5, stripping graphite oxide in the washing process to form nano graphene oxide gel, and drying at 60 ℃ to obtain nano graphene oxide powder;
(3) Adding the nano graphene oxide powder obtained in the step (2) into a PVP (polyvinyl pyrrolidone) aqueous solution, wherein the mass ratio of the PVP to the nano graphene oxide powder is 1:5.5, obtaining a uniformly dispersed colloidal solution through ultrasonic dispersion, firstly carrying out stirring reaction under the conditions of 35 ℃ water bath and pH value of 7.8, then carrying out stirring reaction under the conditions of 28 ℃ water bath and pH value of 7.0, washing colloid obtained after the reaction is finished through deionized water and ethanol, and drying to obtain the modified nano graphene oxide powder.
Example 2
This example provides an asphalt containing modified nano graphene oxide, which is different from example 1 only in that: the dosage of the modified nano graphene oxide is 0.03g.
Example 3
This example provides an asphalt containing modified nano graphene oxide, which is different from example 1 only in that: the dosage of the modified nano graphene oxide is 0.06g.
Example 4
This example provides an asphalt containing modified nano graphene oxide, which is different from example 1 only in that: in the process of preparing the modified nano graphene oxide, the stirring reaction in the step (3) is only carried out in a water bath at 30 ℃ and under the condition of pH value of 7.5.
Comparative example 1
The comparative example provides an asphalt containing modified nano graphene oxide, which is different from example 1 only in that: in the process of preparing the modified nano graphene oxide, the mass ratio of the polyvinylpyrrolidone to the modified nano graphene oxide powder in the step (3) is 1:4.
comparative example 2
This comparative example provides an asphalt containing modified nano graphene oxide, which differs from example 1 only in that: polyvinylpyrrolidone (PVP) adopted during preparation of the modified nano graphene oxide is replaced by Cetyl Trimethyl Ammonium Bromide (CTAB).
Comparative example 3
This comparative example provides an asphalt containing modified nano graphene oxide, which differs from example 1 only in that: and replacing polyvinylpyrrolidone (PVP) adopted in the preparation of the modified nano graphene oxide with N, N-dimethyl formamide (DMF).
Examples of the experiments
The modified nano graphene oxide-containing asphalt prepared in the examples and comparative examples of the present invention was tested for softening point, ductility, penetration, and penetration ratio according to the relevant regulations of road engineering asphalt and asphalt mixture test protocol (JTJE 20-2011). Wherein:
the softening point is the temperature when the asphalt is converted from a solid state to a viscous state, reflects the temperature sensitivity of the asphalt and is detected by a ring and ball method.
The penetration degree reflects the ability of the asphalt to resist deformation under the action of external force or self-weight. The smaller the penetration, the more viscous the bitumen.
Ductility reflects the property that asphalt deforms without being damaged when external force is applied, maintains the deformed shape after the external force is removed, and also reflects the self-healing performance of the asphalt. Specifically, the sample was prepared into a standard 8-shaped test mold (minimum cross-sectional area in the middle 1 cm) 2 ) The length of the film at the time of stretch-breaking at a stretching speed of 5cm/min and at a temperature of 10 ℃ is the ductility. The greater the ductility, the more plastic the bitumen.
The penetration ratio after evaporation reflects the degree of performance stability of the asphalt due to aging resistance, and specifically refers to the percentage of the penetration of the asphalt after evaporation to the penetration ratio before evaporation. The greater the penetration ratio after evaporation, the better the atmospheric stability of the bitumen and the slower the ageing.
The test results are shown in table 1.
Table 1: results of Performance testing
From the above results, the parameters of the modified nano graphene oxide-containing asphalt provided by the invention, such as softening point, penetration degree, ductility and the like, all meet the related technical requirements of technical Specification for road asphalt pavement construction (JTGF 40-2004). Among these, the overall effect of the bitumen provided in example 1 is the best.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, it is intended that all such modifications and alterations be included within the scope of this invention as defined in the appended claims.
Claims (10)
1. The asphalt containing modified nano graphene oxide is characterized by comprising matrix asphalt and modified nano graphene oxide accounting for 0.03 to 0.06 percent of the mass of the matrix asphalt;
the modified nano graphene oxide is prepared by the following steps:
(1) Mixing and stirring graphite, concentrated sulfuric acid and concentrated phosphoric acid, slowly adding potassium permanganate, and stirring for reaction;
(2) Adding deionized water into the reaction liquid obtained in the step (1), adding a hydrogen peroxide solution for reaction, repeatedly washing and centrifuging the obtained reaction product to strip graphite oxide and form nano graphene oxide gel, and drying to obtain nano graphene oxide powder;
(3) Mixing a polyvinylpyrrolidone aqueous solution with the nano graphene oxide powder, wherein the mass ratio of the polyvinylpyrrolidone to the nano graphene oxide powder is 1: (5 to 6), uniformly dispersing by ultrasonic, stirring for reaction, washing, drying,
the stirring reaction in the step (3) is performed under the conditions of temperature of 32 to 38 ℃ and pH value of 7.6 to 8, and then under the conditions of temperature of 25 to 30 ℃ and pH value of 6.8 to 7.2.
2. The asphalt containing the modified nano graphene oxide according to claim 1, wherein the mass of the modified nano graphene oxide accounts for 0.04 to 0.05 percent of the mass of the matrix asphalt.
3. The asphalt containing modified nano graphene oxide according to claim 1, wherein the base asphalt is No. 70 base asphalt.
4. The asphalt containing the modified nano graphene oxide according to claim 1, wherein the stirring reaction in the step (1) is performed in an ice bath, a water bath at 30 to 50 ℃ and a water bath at 80 to 95 ℃ in this order.
5. The asphalt containing the modified nano graphene oxide according to claim 1, wherein the repeated washing in the step (2) is performed by using an acidic aqueous solution.
6. The asphalt containing modified nano graphene oxide according to claim 5, wherein the acidic aqueous solution is an aqueous solution with a pH value of 5.3 to 5.7.
7. The asphalt containing the modified nano graphene oxide according to claim 1, wherein the modified nano graphene oxide powder is prepared by a method comprising the following steps:
(1) Mixing 0.15 part of graphite, 34 parts of concentrated sulfuric acid and 3 parts of concentrated phosphoric acid, mechanically stirring for 10 minutes in an ice bath, slowly adding 0.9 part of potassium permanganate, keeping the temperature at 0 ℃, stirring and reacting for 2 hours in the ice bath, then stirring and reacting for 60 minutes in a water bath at 40 ℃, and then adjusting the temperature of the water bath to 95 ℃, stirring and reacting for 60 minutes;
(2) Suspending the reaction product obtained in the step (1) in water, adding 11 parts of hydrogen peroxide for reaction, repeatedly washing and centrifuging the reaction product for 5 times by using a water solution with the pH of 5.5, stripping graphite oxide in the washing process to form nano graphene oxide gel, and drying at 60 ℃ to obtain nano graphene oxide powder;
(3) Adding the nano graphene oxide powder obtained in the step (2) into a PVP aqueous solution, wherein the mass ratio of PVP to the nano graphene oxide powder is 1:5.5, obtaining a uniformly dispersed colloidal solution through ultrasonic dispersion, firstly carrying out stirring reaction under the conditions of 35 ℃ water bath and pH value of 7.8, then carrying out stirring reaction under the conditions of 28 ℃ water bath and pH value of 7.0, washing colloid obtained after the reaction is finished with deionized water and ethanol, and drying to obtain the modified nano graphene oxide powder.
8. The asphalt containing modified nano graphene oxide according to any one of claims 1 to 7, wherein the asphalt is prepared by shearing, stirring and mixing the matrix asphalt and the nano graphene oxide at a temperature of 120 to 140 ℃ and at a speed of 2000 to 5000 r/min.
9. An asphalt mixture, which is characterized by comprising the asphalt containing the modified nano graphene oxide according to any one of claims 1 to 8, and a mineral mixture which comprises coarse aggregate, fine aggregate and filler and is composed according to a gradation.
10. The asphalt containing the modified nano graphene oxide according to any one of claims 1 to 8 or the asphalt mixture according to claim 9 for use in asphalt pavement construction.
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| CN114316611A (en) * | 2021-10-20 | 2022-04-12 | 鄂尔多斯市路泰公路工程有限责任公司 | Composite modified asphalt based on epoxy resin rubber powder and mixture |
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| CN108117714A (en) * | 2017-12-22 | 2018-06-05 | 广西大学 | A kind of composite asphalt modifier based on modified graphene and its preparation method and application |
| CN109401349A (en) * | 2018-11-26 | 2019-03-01 | 长沙理工大学 | A kind of graphene oxide modified pitch and preparation method thereof |
| CN109651958A (en) * | 2018-12-29 | 2019-04-19 | 厦门十维科技有限公司 | The preparation method of radiation protection asphalt material based on graphene |
| CN109956466A (en) * | 2019-04-10 | 2019-07-02 | 湖南大学 | It is a kind of to have both direction and the graphene-based composite membrane of thickness direction high heat conductance and preparation method thereof in face |
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