CN113860309B - Aerogel foam with mute function, preparation method thereof and tire - Google Patents

Aerogel foam with mute function, preparation method thereof and tire Download PDF

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CN113860309B
CN113860309B CN202111267007.6A CN202111267007A CN113860309B CN 113860309 B CN113860309 B CN 113860309B CN 202111267007 A CN202111267007 A CN 202111267007A CN 113860309 B CN113860309 B CN 113860309B
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mxene
graphene oxide
dispersion liquid
precipitate
aerogel foam
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CN113860309A (en
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刘瑞
闫平
马浩源
王伟
任衍峰
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Sailun Jinyu Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/90Carbides
    • C01B32/914Carbides of single elements
    • C01B32/921Titanium carbide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091Preparation of aerogels, e.g. xerogels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B60VEHICLES IN GENERAL
    • B60CVEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
    • B60C1/00Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
    • B60C1/0008Compositions of the inner liner
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/90Carbides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/90Carbides
    • C01B32/914Carbides of single elements
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02TCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00Road transport of goods or passengers
    • Y02T10/80Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
    • Y02T10/86Optimisation of rolling resistance, e.g. weight reduction 

Abstract

The invention provides aerogel foam with a mute function, a preparation method thereof and a tire. The preparation method comprises the following steps: step S1, mixing an MXene dispersion liquid and a graphene oxide dispersion liquid to form a mixed dispersion liquid; s2, freeze-drying the mixed dispersion liquid to obtain MXene doped graphene oxide; and S3, carrying out a reduction reaction on the MXene doped graphene oxide to obtain aerogel foam with a mute function. The graphene aerogel foam with good flexibility and a three-dimensional continuous porous network structure and MXene doping can be prepared by using the preparation method, and the graphene aerogel foam material has a good absorption effect on cavity noise.

Description

Aerogel foam with mute function, preparation method thereof and tire
Technical Field
The invention relates to the technical field of tire manufacturing, in particular to aerogel foam with a mute function, a preparation method of the aerogel foam and a tire.
Background
With the rapid development of the automobile industry in the world today, automobiles have become an indispensable important transportation means in daily life and industrial and agricultural production of people, the higher the requirements of people on automobiles have become, the more important the comfort has become, and the noise of automobiles is directly related to the riding comfort of passengers.
Automobile noise, i.e., when an automobile is traveling on a road, internal combustion engines, horns, tires, etc., all emit a large amount of sounds that are disliked by humans. In recent years, urban motor vehicles are growing rapidly, and the environment pollution phenomenon caused by traffic noise is also increasingly prominent. Experts consider that the greatest hazard of automobiles to environmental protection is noise pollution. The automotive noise problem includes two aspects: in-vehicle noise and out-of-vehicle noise. The former affects passengers in the vehicle and the latter affects the environment outside the vehicle. The automobile noise is the source of urban traffic noise, environmental protection departments of all countries are very important to see, the allowable standard of the automobile noise is formulated, and the standard is gradually modified and improved along with time.
The main means for controlling the noise of the automobile is to solve the problems of noise sources, noise transmission paths and the like. Four main sources of automobile noise are: noise of the power transmission system, aerodynamic noise, tire noise and air conditioner and automobile accessory noise. In the past decades, technicians in the automotive industry have focused on studying mechanical and aerodynamic noise, such as driveline and automotive streamline windage, and have been reduced to a considerable extent by various noise reduction measures. In recent years, however, it has been found by studying tire/road noise abroad that tire/road noise is a major source of automobile noise when the vehicle speed exceeds 50 to 60 km/h. When a vehicle is traveling on a highway or a high-grade road, a major source of driving noise is tire/road noise. The faster the vehicle speed, the greater the load, the higher the energy level of the tire noise, and the greater the proportion of the tire noise in the running noise of the automobile. Therefore, for automobiles, particularly for environmentally friendly automobiles (non-internal combustion engine locomotives, such as electric vehicles) which are not driven by gasoline and diesel engines, which have been vigorously developed in recent years, the reduction of tire noise will be a major problem.
The most important noise affecting the comfort of passengers is cavity noise of tires, the cavity noise frequency of all tires has an obvious single peak or split peak between 200 and 250Hz, the cavity noise is cavity resonance caused by the excitation of the road surface and the tires in the running process of the tires, and the cavity noise is caused in a vehicle by the transmission of a chassis and a vehicle body part.
Therefore, how to reduce the noise of the cavity is a key to reduce the noise of the tire.
Disclosure of Invention
The invention mainly aims to provide aerogel foam with a silencing function, a preparation method thereof and a tire, so as to reduce tire noise, improve riding comfort of passengers and reduce noise pollution to the environment.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing aerogel foam having a mute function, comprising the steps of: step S1, mixing an MXene dispersion liquid and a graphene oxide dispersion liquid to form a mixed dispersion liquid; s2, freeze-drying the mixed dispersion liquid to obtain MXene doped graphene oxide; and S3, carrying out a reduction reaction on the MXene doped graphene oxide to obtain aerogel foam with a mute function.
Further, the concentration of the MXene in the MXene dispersion liquid is 30-50 mg/ml; the concentration of the graphene oxide in the graphene oxide dispersion liquid is 80-120 mg/ml; preferably, the volume ratio of the MXene dispersion liquid to the graphene oxide dispersion liquid is 1:1-3.
Further, in step S1, the MXene dispersion liquid and the graphene oxide dispersion liquid are mixed by means of ultrasonic dispersion to form a mixed dispersion liquid; preferably, the ultrasonic power in the ultrasonic dispersion process is 80-100 Hz, and the ultrasonic duration is 15-20 min.
Further, step S1 includes: step S11, adding powdery MAX into hydrofluoric acid solution, stirring and mixing, and centrifugally separating to obtain a first precipitate; centrifugal washing is carried out on the first precipitate by adopting deionized water washing, so as to obtain a second precipitate; adding the second precipitate into deionized water, shaking and mixing, centrifuging and separating, and collecting supernatant to obtain MXene dispersion; step S12, adding the expanded graphite powder into sulfuric acid solution, and stirring in an ice bath environment to obtain a premix; adding potassium permanganate into the pre-mixed solution under the stirring state for reaction to form a pre-reaction solution; adding hydrogen peroxide solution into the pre-reaction solution for reaction, then adding hydrochloric acid solution, and centrifugally separating to obtain a third precipitate; adding the third precipitate into deionized water, centrifugally separating, and washing with deionized water to obtain a fourth precipitate; dialyzing the fourth precipitate by using a dialysis bag to obtain graphene oxide dispersion liquid; step S13, mixing the MXene dispersion liquid and the graphene oxide dispersion liquid to form a mixed dispersion liquid; preferably, the concentration of the hydrofluoric acid solution is 45 to 49wt%; preferably, the concentration of the sulfuric acid solution is 95-98 wt%; preferably, the concentration of the hydrogen peroxide solution is 25 to 30wt%; preferably, the concentration of the hydrochloric acid solution is 1 to 1.5mol/L.
Further characterized in that MAX is Ti 3 AlC 2 、Ti 2 AlC、Nb 2 AlC、V 2 AlC or Mo 2 TiAlC 2 One or more of (a) is preferably Ti 3 AlC 2
Further, the particle size of the powdery MAX is 2-6 μm.
Further, in step S3, the temperature of the reduction reaction is 400 to 600 ℃.
According to another aspect of the present invention, there is also provided an aerogel foam having a mute function, which is prepared by the above preparation method.
According to still another aspect of the present invention, there is also provided a tire including an inner liner, characterized in that the aerogel foam having a mute function as described above is adhered to an inner surface of the inner liner.
Further, the thickness of the aerogel foam with the mute function is 8-15 mm; preferably, the aerogel foam having a silencing function is adhered by a binder selected from one or more of PA gum and EVA gum.
The graphene aerogel foam with good flexibility and a three-dimensional continuous porous network structure and MXene doping can be prepared by using the preparation method, and the graphene aerogel foam material has a good absorption effect on cavity noise.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIGS. 1 and 2 show SEM plan views at various magnifications of an aerogel foam having a muting function prepared according to example 1 of the present invention; and
fig. 3 shows an SEM cross-section of aerogel foam with a muting function prepared according to example 1 of the present invention.
Detailed Description
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present invention will be described in detail with reference to examples.
In order to reduce tire noise, improve riding comfort of passengers and reduce noise pollution to the environment, the invention provides a preparation method of aerogel foam with a silencing function, which comprises the following steps: step S1, mixing an MXene dispersion liquid and a graphene oxide dispersion liquid to form a mixed dispersion liquid; s2, freeze-drying the mixed dispersion liquid to obtain MXene doped graphene oxide; and S3, carrying out a reduction reaction on the MXene doped graphene oxide to obtain aerogel foam with a mute function.
In the preparation method, the mixed dispersion liquid formed by mixing the MXene dispersion liquid and the graphene oxide dispersion liquid is freeze-dried, so that the uniformity of dispersing and doping of the MXene in the graphene oxide can be better maintained. And then reducing to form the graphene aerogel foam which has good flexibility and a three-dimensional continuous porous network structure and is doped with MXene. The material has good absorption effect on cavity noise, and can be adhered to the inside of a tire to carry out silencing treatment on the cavity noise generated in running of a vehicle when the material is used, and the noise is restrained at the source generated by the tire noise, so that the effects of absorbing the noise and improving riding comfort are achieved.
Specifically, compared with the traditional foam material, the graphene aerogel foam has a three-dimensional continuous porous network structure, and has a rich composite void structure formed by micro-sized macropores and nano-sized mesopores, and has high specific surface area, high porosity and good elasticity. As the lightest material in the world, the graphene aerogel belongs to a solid material, and has very low surface density of only 0.16 mg and less than one fifth of air density, so the graphene aerogel can be used as a mute foam for a tire without increasing weight for the tire, and good fuel saving comfort is ensured. The graphene has very high intrinsic heat conductivity, and the heat conductivity is very excellent due to the performance, so that the safety performance of the tire running after excessive friction heat generation can be ensured. Graphene aerogel foam is an open cell foam for acoustic treatment that can effectively absorb sound, acoustic energy is transferred from the surface of the foam to the interior, absorption, reflection, vibration occur to cause acoustic energy to be lost, and energy is dissipated in the form of heat.
However, the air flow resistance of porous materials is primarily determined by the internal structure of the material, including pore size, porosity, and the area ratio of the baffles. Generally for open or semi-open structures, the smaller the pore size, the smaller the porosity, the larger the barrier area ratio, and the greater the material thickness, the greater the flow resistance of the sample. The open-cell structure of the pure graphene aerogel foam and the size of the holes thereof are large, and other barriers are not arranged in the pure graphene aerogel foam, so that the flow resistance and the tortuosity coefficient of the pure graphene aerogel foam are low. The self-assembled Mxene of the graphene aerogel foam doped with the MXene prepared by the method can randomly and completely or partially cover holes of a graphene aerogel foam skeleton, so that the transmission of sound waves in air is blocked to a certain extent, and meanwhile, the porosity of a material is slightly reduced due to the incorporation of the MXene, so that the flow resistance is improved. The added MXene also makes the material not pass through, the path of sound waves propagating inside is more tortuous, and the material tortuosity coefficient is increased. Therefore, compared with pure graphene aerogel foam, the MXene doped graphene aerogel foam prepared by the method has higher flow resistance and higher tortuosity coefficient. In addition, for the MXene doped graphene aerogel foam, the incorporated MXene separates the flaked graphene oxide and also connects the graphene backbone, converting the fully open and closed cell structures themselves into semi-open cell structures. Therefore, the flow resistance and the tortuosity coefficient of the graphene aerogel foam obtained by doping the MXene are remarkably improved compared with those of the pure graphene aerogel foam.
For both graphene and MXene, their specific surface areas are very large. Therefore, the addition of MXene to the graphene aerogel foam matrix can bring greater interfacial damping to the system. At the same time, carbon materials are good thermal conductors. Overall, when sound waves enter the interior of the material, the whole structure starts to vibrate, and the different mechanical properties of graphene and MXene make the vibration modes of the graphene and MXene different, and simultaneously cause friction and dissipation of sound energy. Specifically, due to the incorporation of MXene, a number of flaky MXene are covered at the surface and edge breaks of graphene, and when sound waves enter the interior of the material, this flaky MXene structure with a very large specific surface area generates a large amount of interactions and friction with air sound waves, converting sound wave energy into heat energy to a large extent.
In summary, the MXene doped graphene aerogel foam prepared by the method has high flow resistance, high tortuosity coefficient and strong interface damping, is favorable for the dissipation and absorption of sound by materials, has light weight, good heat conduction performance and good flexibility, and is very suitable for being applied to tires.
In order to make the doping amount of the MXene more suitable, the mute effect of the graphene aerogel foam is fully improved, and other properties such as light weight, heat conduction, flexibility and the like are combined, and in a preferred embodiment, the concentration of the MXene in the MXene dispersion liquid is 30-50 mg/ml; the concentration of the graphene oxide in the graphene oxide dispersion liquid is 80-120 mg/ml; preferably, the volume ratio of the MXene dispersion liquid to the graphene oxide dispersion liquid is 1:1-3. The concentration and the volume ratio of each dispersion liquid are controlled within the above ranges, so that the comprehensive performance of the graphene aerogel foam can be further improved.
In a preferred embodiment, in step S1, the MXene dispersion and the graphene oxide dispersion are mixed by means of ultrasonic dispersion to form a mixed dispersion; preferably, the ultrasonic power in the ultrasonic dispersion process is 80-100 Hz, and the ultrasonic duration is 15-20 min. The ultrasonic dispersion mode is adopted for mixing, so that the dispersion of the MXene and the graphene oxide is facilitated, and the MXene is more uniformly doped in the layer structure and the pore structure of the graphene oxide.
As described above, the MXene is doped mainly to increase the flow resistance, the tortuosity coefficient and the interface damping of the graphene aerogel foam, so a good dispersion doping effect will be more beneficial to the improvement of these properties. In a preferred embodiment, step S1 comprises:
step S11, adding powdery MAX into hydrofluoric acid solution, stirring and mixing, and centrifugally separating to obtain a first precipitate; centrifugal washing is carried out on the first precipitate by adopting deionized water washing, so as to obtain a second precipitate; adding the second precipitate into deionized water, shaking and mixing, centrifuging and separating, and collecting supernatant to obtain MXene dispersion;
step S12, adding the expanded graphite powder into sulfuric acid solution, and stirring in an ice bath environment to obtain a premix; adding potassium permanganate into the pre-mixed solution under the stirring state for reaction to form a pre-reaction solution; adding hydrogen peroxide solution into the pre-reaction solution for reaction, then adding hydrochloric acid solution, and centrifugally separating to obtain a third precipitate; adding the third precipitate into deionized water, centrifugally separating, and washing with deionized water to obtain a fourth precipitate; dialyzing the fourth precipitate by using a dialysis bag to obtain graphene oxide dispersion liquid;
step S13, mixing the MXene dispersion liquid and the graphene oxide dispersion liquid to form a mixed dispersion liquid.
Through the steps, the MXene in the MXene dispersion liquid and the graphene oxide in the graphene oxide dispersion liquid have a more stable dispersion effect, so that the performance of the final aerogel foam is further improved. Specifically, hydrofluoric acid is adopted to remove metal phases in powdery MAX phase to form MXene, after residual acid is further removed by water washing, MXene in supernatant obtained by centrifugal separation is more stable in dispersion, smaller in size and more beneficial to subsequent doping of graphene oxide. By adopting the process to prepare the graphene oxide, on one hand, stable dispersion liquid can be formed, and on the other hand, the graphene oxide has a better pore structure, and aerogel foam with a more proper pore structure can be formed after reduction. More preferably, the concentration of the hydrofluoric acid solution is 45 to 49wt%; preferably, the concentration of the sulfuric acid solution is 95-98 wt%; preferably, the concentration of the hydrogen peroxide solution is 25 to 30wt%; preferably, the concentration of the hydrochloric acid solution is 1 to 1.5mol/L. The solvents of the solutions are referred to herein as water.
In the actual production process, the MXene dispersion liquid and the graphene oxide dispersion liquid are preferably produced in the following manner:
MXene dispersion: adding powdery MAX into hydrofluoric acid solution, wherein each gram of MAX corresponds to 20-30 ml of hydrofluoric acid solution, stirring for 12-36 hours at 25-45 ℃, and centrifugally separating to obtain a first precipitate; centrifugal washing is carried out on the first precipitate by adopting deionized water washing until the pH value of supernatant fluid is 6-7, so as to obtain a second precipitate; adding the second precipitate into deionized water, shaking and mixing for 3-10 min, centrifuging and collecting supernatant to obtain MXene dispersion.
Graphene oxide dispersion: adding the expanded graphite powder into a sulfuric acid solution, wherein each gram of expanded graphite corresponds to 100-500 ml of the sulfuric acid solution, and mechanically stirring under an ice bath environment to obtain a premix; adding potassium permanganate into the premix under the mechanical stirring state for reaction, wherein the weight ratio of the potassium permanganate to the expanded graphite is 4-10:1-5, the reaction is carried out in a water bath environment at 30-50 ℃ for 10-60 min, then dropwise adding deionized water into the mixture, and stirring the mixture for 12-36 h to form a pre-reaction solution, wherein the volume ratio of the added deionized water to sulfuric acid solution is 1-3:5; dropwise adding hydrogen peroxide solution into the pre-reaction solution for reaction, wherein the volume ratio of the added hydrogen peroxide solution to the sulfuric acid solution is 5-10:500, then adding hydrochloric acid solution, the volume ratio of the hydrochloric acid solution to the sulfuric acid solution is 10-15:100, and performing centrifugal separation to obtain a third precipitate; adding the third precipitate into deionized water, centrifugally separating, and washing with deionized water to obtain a fourth precipitate; and (3) dialyzing the fourth precipitate by using a dialysis bag to obtain graphene oxide dispersion liquid, wherein the dialysis time is 10-15 days.
In a specific preparation process, after the dispersion is obtained, the concentration can be adjusted to a desired range by adding deionized water.
In order to further enhance the overall properties of the MXene-doped graphene aerogel foam, in a preferred embodiment, MAX is Ti 3 AlC 2 、Ti 2 AlC、Nb 2 AlC、V 2 AlC orMo 2 TiAlC 2 One or more of (a) is preferably Ti 3 AlC 2 . More preferably, the particle size of the powdery MAX is 2-6 μm. The above MAX materials are all commercially available.
The freeze drying is beneficial to improving the doping dispersion uniformity of the MXene, and is also beneficial to improving the three-dimensional pore structure of the graphene aerogel foam, so that the material has a better mute function. In a specific operation, the freeze-drying time is preferably 10 to 30 hours.
In order to sufficiently reduce graphene oxide to graphene, in a preferred embodiment, the temperature of the reduction reaction in step S3 is 400 to 600 ℃, preferably 500 ℃.
According to another aspect of the present invention, there is also provided an aerogel foam having a mute function, which is prepared by the above preparation method. The graphene aerogel foam with good flexibility and a three-dimensional continuous porous network structure and MXene doping can be prepared by using the preparation method, and the graphene aerogel foam material has a good absorption effect on cavity noise.
According to still another aspect of the present invention, there is also provided a tire including an inner liner, characterized in that the aerogel foam having a mute function as described above is adhered to an inner surface of the inner liner. The tire generally comprises, from the outside to the inside, a tread, cap ply, belt, carcass, innerliner, and the side portions generally have sidewalls, apex and bead wires, which are conventional structures in the art and will not be described in detail herein. The aerogel foam is adhered to the inside of the lining layer, so that the noise of the tire can be remarkably reduced, the riding comfort of passengers is improved, and the noise pollution to the environment is reduced. And the aerogel foam is light in weight and good in heat conductivity, and can not influence other performances of the tire after being applied. Because the deformation of the sidewall is larger in the tire running process, the aerogel foam is adhered to the inside of the inner liner, and the deformation is relatively smaller, so that the tire is more stable.
Preferably, the thickness of the aerogel foam with the silencing function is 8-15 mm; preferably, the aerogel foam having a silencing function is adhered by a binder selected from one or more of PA gum and EVA gum.
The present application is described in further detail below in conjunction with specific embodiments, which should not be construed as limiting the scope of the claims.
Example 1
Preparation of MXene Dispersion:
1. 1g MAX powder (Ti) 3 AlC 2 Particle size of 2 to 5 μm) was added to 20ml of 49wt% HF solution, stirred at 35 ℃ for 24 hours, and centrifuged to obtain a first precipitate.
2. In the step 1, the first precipitate is centrifugally washed by deionized water, the pH value of the supernatant is 6, and the second precipitate is collected.
3. Adding the second precipitate obtained in the step 2 into 100ml of deionized water, shaking for 5 minutes, centrifuging, and collecting supernatant to obtain MXene dispersion with the concentration of 100 mg/ml;
4. the concentration of the MXene dispersion was adjusted to 40mg/ml by adding deionized water.
Preparation of graphene oxide dispersion:
1. 3g of expanded graphite powder was added to 500mL of 98% by mass H 2 SO 4 The solution was mechanically stirred in an ice bath environment.
2. 5g KMnO was stirred mechanically and continuously 4 Slowly add to the mixture from step 1.
3. And (3) transferring the mixture obtained in the step (2) to a water bath environment at 30 ℃, stirring for 30min, slowly dropwise adding 200mL of deionized water, and mechanically stirring at room temperature for 24h.
4. 10mL of H with a concentration of 30% 2 O 2 Slowly dripping the solution into the mixture obtained in the step 3, adding 100mL of 1mol/L HCl solution, and centrifuging to obtain a precipitate.
5. Dispersing the precipitate obtained in the step 4 in 100mL of deionized water, centrifuging and washing with deionized water to obtain the precipitate.
6. Finally, the precipitate obtained in the step 5 is put in a dialysis bag for dialysis for 15 days, and the graphene oxide dispersion liquid with the concentration of 200mg/ml is obtained.
7. The graphene oxide dispersion concentration was adjusted to 100mg/ml by adding deionized water.
Preparation of aerogel foam:
1. 100ml of the MXene dispersion was added to 100ml of the graphene oxide dispersion, and the mixture was sonicated at 100Hz for 20min to obtain an MXene-doped graphene oxide dispersion.
2. And (3) performing freeze drying on the mixed dispersion liquid of the MXene doped graphene oxide prepared in the step (1) for 24 hours to obtain the MXene doped graphene oxide aerogel.
3. And (3) carrying out high-temperature reduction on the MXene doped graphene oxide aerogel obtained in the step (2) at 500 ℃ to obtain the MXene doped graphene aerogel foam with good flexibility.
Fig. 1 is an SEM plan view of the aerogel foam having a silencing function described above; FIG. 2 is an SEM plan view of the aerogel foam of FIG. 1 with portions enlarged; fig. 3 is an SEM cross-sectional view of aerogel foam with a mute function obtained by liquid nitrogen brittle fracture.
Example 2
The difference from example 1 is that: the concentration of the MXene dispersion was adjusted to 30mg/ml by adding deionized water.
Example 3
The difference from example 1 is that: the concentration of the MXene dispersion was adjusted to 50mg/ml by adding deionized water.
Example 4
The difference from example 1 is that: the graphene oxide dispersion concentration was adjusted to 80mg/ml by adding deionized water.
Example 5
The difference from example 1 is that: the graphene oxide dispersion concentration was adjusted to 120mg/ml by adding deionized water.
Example 6
The difference from example 1 is that: the concentration of the MXene dispersion was adjusted to 10mg/ml by adding deionized water.
Example 7
The difference from example 1 is that: the concentration of the MXene dispersion was adjusted to 70mg/ml by adding deionized water.
Example 8
The difference from example 1 is that: the graphene oxide dispersion concentration was adjusted to 50mg/ml by adding deionized water.
Example 9
The difference from example 1 is that: the graphene oxide dispersion concentration was adjusted to 150mg/ml by adding deionized water.
Example 10
The difference from example 1 is that: MAX is Nb 2 AlC powder with particle size of 2-6 μm.
Example 11
The difference from example 1 is that: MAX is Mo 2 TiAlC 2 The particle size of the powder is 2-6 mu m.
Comparative example 1
The difference from example 1 is that: the pure graphene aerogel foam is prepared without adding MXene dispersion liquid.
Characterization of the properties:
the MXene doped graphene aerogel foam or the pure graphene aerogel foam prepared in the examples and the comparative examples are subjected to sound absorption performance test, and GBT18696.2-2002 national standard test method is adopted. The test results are shown in Table 1:
TABLE 1
Figure BDA0003327111070000081
Figure BDA0003327111070000091
From the above data, the MXene doped graphene aerogel foam prepared by the preparation method in the embodiment of the present invention has significantly higher sound absorption coefficient at different frequencies than the pure graphene aerogel foam in the comparative example. And the silencing capability of the MXene doped graphene aerogel foam can be further improved by adjusting the concentration of the dispersion liquid within a preferable range. However, when the amount of MXene added exceeds a certain range, the network structure of graphene is blocked, thereby affecting the transmission and absorption of noise between aerogel foams, so that the sound absorption effect is reduced (e.g., embodiment 7).
The MXene-doped graphene aerogel foam or the pure graphene aerogel foam prepared in the above examples and comparative examples was adhered to the inner surface of the tire inner liner with PA gel and EVA gel adhesive, both having a thickness of 12mm. The treated tires were subjected to performance testing (test method using GBT 18505-2013) with the test results shown in table 2:
TABLE 2
Figure BDA0003327111070000092
Figure BDA0003327111070000101
The above results show that after the MXene doped graphene aerogel foam is added into the tire, the X-ray, dynamic balance and uniformity of the tire meet the factory requirements of the tire, namely, the addition of the MXene doped graphene aerogel foam into the tire does not influence other main performances of the tire, and the new problem is not caused while the noise is reduced.
The noise reduction and silence performance of the processed tire is tested by adopting a Star Ruida noise tester at the main driving position in the automobile, wherein the test road condition is expressway, the running speed is 100km/h, and the test result is shown in Table 3:
TABLE 3 Table 3
Figure BDA0003327111070000102
From the above data, the tire has obvious tire noise reduction effect after the MXene doped graphene aerogel foam is added into the tire. Especially, the concentration of the dispersion liquid is adjusted within a preferable range, so that the noise reduction capability of the MXene doped graphene aerogel foam can be further improved, and the noise reduction effect of the tire can be further enhanced. Generally, when the noise level is increased by 3dB, the noise level is increased by 41% to 1.4 times of the original noise level; the noise level is increased by 99% by 6dB, and the original noise level is 2 times. On the expressway with the speed of 100km/h, the noise of the tire is reduced by 4.5dB at most compared with that of the original tire, which shows that the tire has obvious sound absorption performance improvement and the noise size is reduced by 42 percent.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (13)

1. The tire comprises an inner liner, and is characterized in that aerogel foam with a silencing function is adhered to the inner surface of the inner liner, and the preparation method of the aerogel foam with the silencing function comprises the following steps of:
step S1, mixing an MXene dispersion liquid and a graphene oxide dispersion liquid to form a mixed dispersion liquid;
s2, freeze-drying the mixed dispersion liquid to obtain MXene doped graphene oxide;
and S3, carrying out a reduction reaction on the MXene doped graphene oxide to obtain the aerogel foam with the mute function.
2. Tyre according to claim 1, characterized in that the concentration of MXene in said MXene dispersion is between 30 and 50mg/ml; the concentration of graphene oxide in the graphene oxide dispersion liquid is 80-120 mg/ml.
3. Tyre according to claim 2, characterized in that the volume ratio of said MXene dispersion and said graphene oxide dispersion is comprised between 1:1 and 3.
4. A tyre according to any one of claims 1 to 3, wherein in step S1, the MXene dispersion and the graphene oxide dispersion are mixed by means of ultrasonic dispersion to form the mixed dispersion.
5. Tyre according to claim 4, characterized in that the ultrasonic power of the ultrasonic dispersion process is 80-100 Hz and the ultrasonic duration is 15-20 min.
6. A tyre according to any one of claims 1 to 3, wherein said step S1 comprises:
step S11, adding powdery MAX into hydrofluoric acid solution, stirring and mixing, and centrifugally separating to obtain a first precipitate; centrifugal washing is carried out on the first precipitate by adopting deionized water washing, so as to obtain a second precipitate; adding the second precipitate into deionized water, shaking, mixing, centrifugally separating, and collecting supernatant to obtain the MXene dispersion;
step S12, adding the expanded graphite powder into sulfuric acid solution, and stirring in an ice bath environment to obtain a premix; adding potassium permanganate into the pre-mixed solution under the stirring state for reaction to form a pre-reaction solution; adding hydrogen peroxide solution into the pre-reaction solution for reaction, then adding hydrochloric acid solution, and centrifugally separating to obtain a third precipitate; adding the third precipitate into deionized water, centrifugally separating, and washing with deionized water to obtain a fourth precipitate; dialyzing the fourth precipitate by using a dialysis bag to obtain the graphene oxide dispersion liquid;
step S13, mixing the MXene dispersion liquid and the graphene oxide dispersion liquid to form the mixed dispersion liquid.
7. The tire of claim 6, wherein the hydrofluoric acid solution has a concentration of 45 to 49wt%; the concentration of the sulfuric acid solution is 95-98 wt%; the concentration of the hydrogen peroxide solution is 25-30wt%; the concentration of the hydrochloric acid solution is 1-1.5 mol/L.
8. Tyre according to claim 6, characterized in that said MAX is Ti 3 AlC 2 、Ti 2 AlC、Nb 2 AlC、V 2 AlC or Mo 2 TiAlC 2 One or more of the following.
9. Tyre according to claim 8, characterized in that said MAX is Ti 3 AlC 2
10. Tyre according to claim 6, characterized in that the particle size of said MAX in powder form is between 2 and 6 μm.
11. A tyre according to any one of claims 1 to 3, wherein in step S3 the temperature of the reduction reaction is between 400 and 600 ℃.
12. Tyre according to claim 1, characterized in that said aerogel foam with a silencing function has a thickness of 8-15 mm.
13. The tire of claim 12, wherein the aerogel foam having a mute function is adhered by a binder selected from one or more of PA gum and EVA gum.
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