CN113860309A - Aerogel foam with silencing function, preparation method thereof and tire - Google Patents

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

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CN113860309A
CN113860309A CN202111267007.6A CN202111267007A CN113860309A CN 113860309 A CN113860309 A CN 113860309A CN 202111267007 A CN202111267007 A CN 202111267007A CN 113860309 A CN113860309 A CN 113860309A
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dispersion liquid
mxene
graphene oxide
aerogel foam
precipitate
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CN113860309B (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 silencing function, a preparation method thereof and a tire. The preparation method comprises the following steps: step S1, mixing MXene dispersion liquid and graphene oxide dispersion liquid to form mixed dispersion liquid; step S2, freeze-drying the mixed dispersion liquid to obtain MXene-doped graphene oxide; step S3, carrying out reduction reaction on the MXene-doped graphene oxide to obtain the aerogel foam with the silencing function. The graphene aerogel foam which is good in flexibility and has a three-dimensional continuous porous network structure and MXene doping can be prepared by the preparation method, the material has a good absorption effect on cavity noise, and when the graphene aerogel foam is applied to a tire, the noise of the tire can be remarkably reduced, the riding comfort of passengers can be improved, and the noise pollution to the environment can be reduced.

Description

Aerogel foam with silencing 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 silencing function, a preparation method of the aerogel foam and a tire.
Background
With the rapid development of the automobile industry in the world, automobiles become important transportation tools indispensable to people in daily life and industrial and agricultural production, the requirements of people on automobiles become higher, the comfort becomes a main concern, and the noise of automobiles is directly related to the riding comfort of passengers.
Automobile noise, i.e. when an automobile runs on a road, a large amount of unpleasant sounds are produced by an internal combustion engine, a horn, tires and the like. In recent years, urban motor vehicles grow rapidly, and the phenomenon of environmental pollution caused by traffic noise is increasingly prominent. Experts consider that the greatest environmental hazard of automobiles is noise pollution. The automotive noise problem includes two aspects: noise inside and outside the car. The former affects passengers inside the vehicle and the latter affects the environment outside the vehicle. The automobile noise is the root cause of urban traffic noise, environmental protection departments in various countries pay great attention to the automobile noise, the allowable standard of the automobile noise is established, 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. The four main sources of car noise are: driveline noise, aerodynamic noise, tire noise, and air conditioning and auto parts noise. Over the past few decades, the automotive industry has concentrated on mechanical and aerodynamic noise, such as power train and automotive streamline windage, and has reduced it to a considerable extent through various noise reduction measures. However, in recent years, it has been found abroad by studying tire/road noise that the tire/road noise is a major source of automobile noise when the vehicle speed exceeds 50-60 km/h. When a vehicle is running on a high speed or high grade road, the main source of running noise is tire/road noise. The faster the vehicle speed and the greater the load, the higher the energy level of the tire noise and the greater the proportion of the tire noise in the vehicle running noise. Therefore, for automobiles, particularly for environmentally-friendly vehicles (non-internal combustion engine-powered vehicles such as electric vehicles) which are vigorously developed in recent years and are not driven by gasoline and diesel engines, reduction of tire noise will be a major problem.
The most important noise influencing the comfort of passengers is the cavity noise of the tires, the cavity noise frequency of all the tires has an obvious single peak or split peak between 200 Hz and 250Hz, and the cavity noise is the noise in the vehicle caused by the cavity resonance caused by the excitation of the road surface and the tires in the running process of the tires and the transmission of a chassis and vehicle body components.
Therefore, how to reduce the noise of the cavity is the 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 an aerogel foam having a muting function, comprising the steps of: step S1, mixing MXene dispersion liquid and graphene oxide dispersion liquid to form mixed dispersion liquid; step S2, freeze-drying the mixed dispersion liquid to obtain MXene-doped graphene oxide; step S3, carrying out reduction reaction on the MXene-doped graphene oxide to obtain the aerogel foam with the silencing function.
Furthermore, the concentration of 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, mixing the MXene dispersion liquid and the graphene oxide dispersion liquid by using an ultrasonic dispersion method to form a mixed dispersion liquid; preferably, the ultrasonic power in the ultrasonic dispersion process is 80-100 Hz, and the ultrasonic time is 15-20 min.
Further, step S1 includes: step S11, adding the powdered MAX into a hydrofluoric acid solution, stirring and mixing, and then performing centrifugal separation to obtain a first precipitate; washing the first precipitate with deionized water, and centrifugally washing to obtain a second precipitate; adding the second precipitate into deionized water, shaking and mixing, performing centrifugal separation, and collecting supernatant to obtain MXene dispersion liquid; step S12, adding the expanded graphite powder into a sulfuric acid solution, and stirring in an ice bath environment to obtain a premixed solution; adding potassium permanganate into the premixed solution under the stirring state to react to form a pre-reaction solution; adding a hydrogen peroxide solution into the pre-reaction solution for reaction, then adding a hydrochloric acid solution, and performing centrifugal separation to obtain a third precipitate; adding the third precipitate into deionized water, performing centrifugal separation, 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 MXene dispersion liquid and graphene oxide dispersion liquid to form mixed dispersion liquid; preferably, the concentration of the hydrofluoric acid solution is 45-49 wt%; preferably, the concentration of the sulfuric acid solution is 95-98 wt%; preferably, the concentration of the hydrogen peroxide solution is 25-30 wt%; preferably, the concentration of the hydrochloric acid solution is 1-1.5 mol/L.
Further, MAX is Ti3AlC2、Ti2AlC、Nb2AlC、V2AlC or Mo2TiAlC2Preferably Ti3AlC2
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 silencing function, which is prepared by the above preparation method.
According to another aspect of the present invention, there is also provided a tire comprising an inner liner, wherein the inner surface of the inner liner is adhered with the aerogel foam having a silencing function.
Further, 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 graphene aerogel foam which is good in flexibility and has a three-dimensional continuous porous network structure and MXene doping can be prepared by the preparation method, the material has a good absorption effect on cavity noise, and when the graphene aerogel foam is applied to a tire, the noise of the tire can be remarkably reduced, the riding comfort of passengers can be improved, and the noise pollution to the environment can be reduced.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 and 2 show SEM plan views at different magnifications of aerogel foam having a silencing function prepared according to example 1 of the present invention; and
fig. 3 shows an SEM cross-sectional view of an aerogel foam having a silencing function prepared according to example 1 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. 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 MXene dispersion liquid and graphene oxide dispersion liquid to form mixed dispersion liquid; step S2, freeze-drying the mixed dispersion liquid to obtain MXene-doped graphene oxide; step S3, carrying out reduction reaction on the MXene-doped graphene oxide to obtain the aerogel foam with the silencing function.
In the preparation method, the mixed dispersion liquid formed by mixing the MXene dispersion liquid and the graphene oxide dispersion liquid is subjected to freeze drying, so that the uniformity of the MXene in the graphene oxide in dispersion and doping can be better maintained. And then reducing to form the MXene-doped graphene aerogel foam with good flexibility and a three-dimensional continuous porous network structure. The material has good absorption effect on cavity noise, can be adhered to the interior of a tire to perform noise reduction treatment on the cavity noise generated during vehicle running during use, and can suppress noise at the source generated by tire noise, so that the effects of absorbing 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 a rich composite type gap structure is formed by the micron-sized macropores and the nanometer-sized mesopores inside, so that the graphene aerogel foam 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, has very low surface density of only 0.16 mg and is less than one fifth of the air density, so that the graphene aerogel serving as the silent foam for the tire does not increase the weight of the tire, and ensures good fuel-saving comfort. The graphene has very high intrinsic thermal conductivity, and due to the property, the thermal conductivity of the graphene is very excellent, so that the safety performance of the tire after excessive friction heating can be ensured. The graphene aerogel foam is an open pore foam for acoustic treatment, can effectively absorb sound, sound energy is transmitted from the surface of the foam to the inside of the foam, the sound energy is lost due to absorption, reflection and vibration, and the energy is dissipated in the form of heat.
However, the airflow resistance of porous materials is mainly determined by the internal structure of the material, including pore size, porosity, and the area fraction of the lattice. Generally, for open or semi-open structures, the smaller the pore size, the smaller the porosity, the larger the lattice area fraction, and the larger the material thickness, the greater the flow resistance of the sample. The open-cell structure and the size of the holes of the pure graphene aerogel foam are large, and in addition, no other barriers are arranged inside the pure graphene aerogel foam, so that the flow resistance and the tortuosity coefficient of the pure graphene aerogel foam are low. In the MXene-doped graphene aerogel foam prepared by the invention, the self-assembled Mxene can randomly and completely or partially cover the holes of the graphene aerogel foam skeleton, so that the transmission of sound waves in the air is hindered to a certain extent, and the porosity of the material is slightly reduced by the addition of the MXene, so that the flow resistance is improved. The added MXene also makes the material less transparent, and the path of sound waves propagating inside is more tortuous, so that the tortuosity coefficient of the material is increased. Therefore, compared with pure graphene aerogel foam, the MXene-doped graphene aerogel foam prepared by the method has higher flow resistance and larger tortuosity coefficient. In addition, for MXene doped graphene aerogel foams, the doped MXene separates the sheets of graphene oxide and also links the graphene backbone, converting the fully open and closed cell structure itself to a semi-open structure. Therefore, the flow resistance and the tortuosity coefficient of the MXene-doped graphene aerogel foam are remarkably improved compared with those of pure graphene aerogel foam.
For graphene and MXene, their specific surface areas are very large. Therefore, the addition of MXene in the graphene aerogel foam matrix can bring greater interface damping to the system. At the same time, carbon materials are good thermal conductors. On the whole, when sound waves enter the material, the whole structure can start to vibrate, and the graphene and MXene have different mechanical properties, so that the graphene and MXene have different vibration modes, and friction and sound energy dissipation are caused. In particular, due to the incorporation of MXene, a plurality of flaky MXene are covered on the surface and edge break of graphene, and when sound waves enter the interior of the material, the flaky MXene structure with extremely large specific surface area can generate a large amount of interaction and friction with air sound waves, so that sound wave energy is converted into heat energy to a large extent.
In summary, the MXene-doped graphene aerogel foam prepared by the present invention has high flow resistance, high tortuosity coefficient and strong interface damping, which are beneficial to the dissipation and absorption of sound by materials, and is very suitable for being applied to tires due to its light weight, good thermal conductivity and good flexibility.
In order to make the doping amount of MXene more appropriate, fully improve the silencing effect of the graphene aerogel foam and simultaneously integrate other performances such as light weight, heat conductivity, flexibility and the like, in a preferred embodiment, the concentration of 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, mixing the MXene dispersion liquid and the graphene oxide dispersion liquid by using an ultrasonic dispersion method to form a mixed dispersion liquid; preferably, the ultrasonic power in the ultrasonic dispersion process is 80-100 Hz, and the ultrasonic time is 15-20 min. The ultrasonic dispersion mode is adopted for mixing, which is beneficial to the dispersion of MXene and graphene oxide, so that MXene is more uniformly doped in the layer structure and the pore structure of graphene oxide.
As mentioned above, MXene is doped mainly to improve the flow resistance, tortuosity and interface damping of graphene aerogel foam, so that a good dispersion doping effect is more beneficial to the improvement of these properties. In a preferred embodiment, step S1 includes:
step S11, adding the powdered MAX into a hydrofluoric acid solution, stirring and mixing, and then performing centrifugal separation to obtain a first precipitate; washing the first precipitate with deionized water, and centrifugally washing to obtain a second precipitate; adding the second precipitate into deionized water, shaking and mixing, performing centrifugal separation, and collecting supernatant to obtain MXene dispersion liquid;
step S12, adding the expanded graphite powder into a sulfuric acid solution, and stirring in an ice bath environment to obtain a premixed solution; adding potassium permanganate into the premixed solution under the stirring state to react to form a pre-reaction solution; adding a hydrogen peroxide solution into the pre-reaction solution for reaction, then adding a hydrochloric acid solution, and performing centrifugal separation to obtain a third precipitate; adding the third precipitate into deionized water, performing centrifugal separation, 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, MXene in the MXene dispersion liquid and 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, the hydrofluoric acid is adopted to remove the metal phase in the powdery MAX phase to form MXene, and after residual acid is further removed by washing, MXene in the supernatant obtained by centrifugal separation is dispersed more stably and has smaller size, so that the subsequent doping of graphene oxide is facilitated. By adopting the process to prepare the graphene oxide, on one hand, stable dispersion liquid can be formed, on the other hand, the graphene oxide has a better pore structure, and after reduction, aerogel foam with a more appropriate pore structure can be formed. More preferably, the concentration of the hydrofluoric acid solution is 45-49 wt%; preferably, the concentration of the sulfuric acid solution is 95-98 wt%; preferably, the concentration of the hydrogen peroxide solution is 25-30 wt%; preferably, the concentration of the hydrochloric acid solution is 1-1.5 mol/L. The solvent of the solution is referred to herein as water.
In the actual preparation process, the MXene dispersion liquid and the graphene oxide dispersion liquid are preferably prepared in the following ways:
MXene dispersion: adding powdery MAX into a hydrofluoric acid solution, wherein each gram of MAX corresponds to 20-30 ml of the hydrofluoric acid solution, then stirring for 12-36 h at the temperature of 25-45 ℃, and performing centrifugal separation to obtain a first precipitate; washing the first precipitate with deionized water, and centrifugally washing until the pH value of the supernatant is 6-7 to obtain a second precipitate; and adding the second precipitate into deionized water, shaking and mixing for 3-10 min, then carrying out centrifugal separation, and collecting supernatant to obtain MXene dispersion liquid.
Graphene oxide dispersion liquid: adding 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 in an ice bath environment to obtain a premixed solution; adding potassium permanganate into the premixed liquid to react under the mechanical stirring state, wherein the weight ratio of potassium permanganate to expanded graphite is 4-10: 1-5, reacting in a water bath environment at the temperature of 30-50 ℃ for 10-60 min, then dropwise adding deionized water into the premixed liquid, and stirring for 12-36 h to form a pre-reaction liquid, wherein the volume ratio of the added deionized water to the sulfuric acid solution is 1-3: 5; dropwise adding a hydrogen peroxide solution into the pre-reaction solution for reaction, wherein the volume ratio of the hydrogen peroxide solution to the sulfuric acid solution is 5-10: 500, then adding a 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, performing centrifugal separation, and washing with deionized water to obtain a fourth precipitate; and dialyzing the fourth precipitate by using a dialysis bag to obtain the 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.
To further improve the overall performance of the MXene doped graphene aerogel foam, in a preferred embodiment MAX is Ti3AlC2、Ti2AlC、Nb2AlC、V2AlC or Mo2TiAlC2Preferably Ti3AlC2. More preferably, the particle size of the powdered MAX is 2 to 6 μm. The above MAX materials are commercially available.
The freeze drying is beneficial to improving the doping dispersion uniformity of MXene and the three-dimensional pore structure of the graphene aerogel foam, so that the material has a better mute function. In the specific operation process, the freeze drying time is preferably 10-30 h.
In order to sufficiently reduce the 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 silencing function, which is prepared by the above preparation method. The graphene aerogel foam which is good in flexibility and has a three-dimensional continuous porous network structure and MXene doping can be prepared by the preparation method, the material has a good absorption effect on cavity noise, and when the graphene aerogel foam is applied to a tire, the noise of the tire can be remarkably reduced, the riding comfort of passengers can be improved, and the noise pollution to the environment can be reduced.
According to another aspect of the present invention, there is also provided a tire comprising an inner liner, wherein the inner surface of the inner liner is adhered with the aerogel foam having a silencing function. The tire generally comprises a tread, a cap ply, a belt, a carcass and an inner liner from the outside to the inside, and the side portions generally have sidewalls, apexes and beads, which are conventional in the art and will not be described herein. The tire disclosed by the invention is characterized in that the aerogel foam is adhered to the inner lining layer, so that the noise of the tire can be obviously reduced, the riding comfort of passengers is improved, and the noise pollution to the environment is reduced. And because the aerogel foam is light in weight and good in thermal conductivity, other performances of the tire cannot be affected after the aerogel foam is applied. Because the deformation of the tire side is larger in the running process of the tire, the aerogel foam is adhered to the inner part of the inner liner, and the deformation is relatively smaller, so that the aerogel foam 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 with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
Preparation of MXene dispersion:
1. 1g MAX powder (Ti)3AlC2Particle size of 2-5 μm) was added to 20ml of 49 wt% HF solution, stirred at 35 ℃ for 24 hours, and centrifuged to obtain a first precipitate.
2. And (3) centrifugally washing the first precipitate in the step 1 by using deionized water until the pH of the supernatant is 6, and collecting a second precipitate.
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 liquid with the concentration of 100 mg/ml;
4. the concentration of MXene dispersion was adjusted to 40mg/ml by adding deionized water.
Preparing a graphene oxide dispersion liquid:
1. 3g of expanded graphite powder is added into 500mL of H with 98 percent of mass fraction2SO4The solution was stirred mechanically in an ice bath environment.
2. Under continuous mechanical stirring, 5g of KMnO4Slowly adding into the mixture obtained in the step 1.
3. And (3) transferring the mixture obtained in the step (2) to a water bath environment at 30 ℃, stirring for 30min, then slowly dropwise adding 200mL of deionized water, and mechanically stirring for 24h at room temperature.
4. 10mL of 30% H2O2The solution was slowly added dropwise to the mixture obtained in step 3, followed by addition of 100mL of 1mol/L HCl solution and centrifugation to obtain a precipitate.
5. And (4) 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 filled in a dialysis bag for dialysis for 15 days to obtain the graphene oxide dispersion liquid with the concentration of 200 mg/ml.
7. The concentration of the graphene oxide dispersion was adjusted to 100mg/ml by adding deionized water.
Preparation of aerogel foam:
1. and adding 100ml of MXene dispersion liquid into 100ml of graphene oxide dispersion liquid, and carrying out ultrasonic treatment at 100Hz for 20min to obtain the MXene-doped graphene oxide dispersion liquid.
2. And (3) freeze-drying the mixed dispersion liquid of 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 MXene-doped graphene aerogel foam with good flexibility.
Fig. 1 is an SEM plan view of the aerogel foam having a silencing function; FIG. 2 is an SEM plan view of the aerogel foam of FIG. 1 at a partial magnification; fig. 3 is an SEM sectional view of aerogel foam having a silencing function obtained by liquid nitrogen brittle fracture.
Example 2
The difference from example 1 is that: the concentration of MXene dispersion was adjusted to 30mg/ml by adding deionized water.
Example 3
The difference from example 1 is that: the concentration of MXene dispersion was adjusted to 50mg/ml by adding deionized water.
Example 4
The difference from example 1 is that: the concentration of the graphene oxide dispersion was adjusted to 80mg/ml by adding deionized water.
Example 5
The difference from example 1 is that: the concentration of the graphene oxide dispersion was adjusted to 120mg/ml by adding deionized water.
Example 6
The difference from example 1 is that: the concentration of MXene dispersion was adjusted to 10mg/ml by adding deionized water.
Example 7
The difference from example 1 is that: MXene dispersion concentration was adjusted to 70mg/ml by adding deionized water.
Example 8
The difference from example 1 is that: the concentration of the graphene oxide dispersion was adjusted to 50mg/ml by adding deionized water.
Example 9
The difference from example 1 is that: the concentration of the graphene oxide dispersion was adjusted to 150mg/ml by adding deionized water.
Example 10
The difference from example 1 is that: MAX is Nb2AlC powder with the particle size of 2-6 μm.
Example 11
The difference from example 1 is that: MAX is Mo2TiAlC2Powder with a particle size of 2-6 μm.
Comparative example 1
The difference from example 1 is that: the pure graphene aerogel foam was obtained without addition of MXene dispersion.
And (3) performance characterization:
the MXene doped graphene aerogel foams or pure graphene aerogel foams prepared in the above examples and comparative examples were subjected to sound absorption performance testing using the national standard test method of GBT 18696.2-2002. The test results are shown in table 1:
TABLE 1
Figure BDA0003327111070000081
Figure BDA0003327111070000091
From the data, the sound absorption coefficient of the MXene doped graphene aerogel foam prepared by the preparation method in the embodiment of the present invention at different frequencies is significantly higher than that of the pure graphene aerogel foam in the comparative example. And the noise reduction capability of the MXene-doped graphene aerogel foam can be further improved by adjusting the concentration of the dispersion liquid within the optimal range. However, when the addition amount of MXene exceeds a certain range, the graphene network structure is blocked, so that the transmission and absorption of noise between aerogel foams are affected, and the sound absorption effect is reduced (as in example 7).
MXene-doped graphene aerogel foam or pure graphene aerogel foam prepared in the above examples and comparative examples were adhered to the inner surface of the tire inner liner with PA glue and EVA glue adhesives, and the thickness was 12 mm. The treated tires were subjected to performance tests (test method adopted GBT18505-2013), and the test results are shown in table 2:
TABLE 2
Figure BDA0003327111070000092
Figure BDA0003327111070000101
The results show that after the MXene-doped graphene aerogel foam is added into the tire, the X-ray, the dynamic balance and the uniformity of the tire all meet the delivery requirements of the tire, namely the MXene-doped graphene aerogel foam is added into the tire, other main performances of the tire are not influenced, and new problems are not brought while noise is reduced.
The noise reduction and silencing performance of the processed tire is tested by adopting a star Ruidan noise tester at the main driving position in the vehicle, wherein the road condition is tested by adopting a highway, the driving speed is 100km/h, and the test result is shown in a table 3:
TABLE 3
Figure BDA0003327111070000102
According to the data, the MXene-doped graphene aerogel foam has obvious tire noise reduction effect after being added into the tire. Especially, the concentration of the dispersion liquid is adjusted in an optimal 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 speaking, if 3dB is increased, the noise level will be increased by 41%, which is 1.4 times of the original level; the noise is increased by 6dB, and the noise is increased by 99% to reach 2 times of the original noise. Compared with the original tire, the tire of the invention has the highest noise reduction of 4.5dB on the expressway with the speed of 100km/h, which shows that the tire has obvious sound absorption performance improvement and the noise reduction of 42%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A preparation method of aerogel foam with a silencing function is characterized by comprising the following steps:
step S1, mixing MXene dispersion liquid and graphene oxide dispersion liquid to form mixed dispersion liquid;
step S2, freeze-drying the mixed dispersion liquid to obtain MXene-doped graphene oxide;
step S3, carrying out reduction reaction on the MXene-doped graphene oxide to obtain the aerogel foam with the silencing function.
2. The preparation method of claim 1, wherein the concentration of 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.
3. The preparation method according to claim 1 or 2, wherein in the step S1, the MXene dispersion liquid and the graphene oxide dispersion liquid are mixed by ultrasonic dispersion to form the mixed dispersion liquid; preferably, the ultrasonic power in the ultrasonic dispersion process is 80-100 Hz, and the ultrasonic time is 15-20 min.
4. The production method according to any one of claims 1 to 3, wherein the step S1 includes:
step S11, adding the powdered MAX into a hydrofluoric acid solution, stirring and mixing, and then performing centrifugal separation to obtain a first precipitate; washing the first precipitate with deionized water, and centrifugally washing to obtain a second precipitate; adding the second precipitate into deionized water, shaking and mixing, performing centrifugal separation, and collecting a supernatant to obtain the MXene dispersion liquid;
step S12, adding the expanded graphite powder into a sulfuric acid solution, and stirring in an ice bath environment to obtain a premixed solution; adding potassium permanganate into the premixed solution under the stirring state to react to form a pre-reaction solution; adding a hydrogen peroxide solution into the pre-reaction solution for reaction, then adding a hydrochloric acid solution, and performing centrifugal separation to obtain a third precipitate; adding the third precipitate into deionized water, performing centrifugal separation, 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;
preferably, the concentration of the hydrofluoric acid solution is 45-49 wt%; preferably, the concentration of the sulfuric acid solution is 95-98 wt%; preferably, the concentration of the hydrogen peroxide solution is 25-30 wt%; preferably, the concentration of the hydrochloric acid solution is 1-1.5 mol/L.
5. The method according to claim 4, wherein MAX is Ti3AlC2、Ti2AlC、Nb2AlC、V2AlC or Mo2TiAlC2Preferably Ti3AlC2
6. The method according to claim 4, wherein the particle size of the powdered MAX is 2-6 μm.
7. The production method according to any one of claims 1 to 6, wherein in the step S3, the temperature of the reduction reaction is 400 to 600 ℃.
8. Aerogel foam having a silencing function, characterized by being prepared by the preparation method of any one of claims 1 to 7.
9. A tire comprising an inner liner, characterized in that the inner surface of the inner liner is adhered with the aerogel foam having a silencing function of claim 8.
10. The tire according to claim 9, wherein the thickness of the aerogel foam having a silencing function is 8 to 15 mm; preferably, the aerogel foam with a silencing function is adhered by a binder selected from one or more of PA glue and EVA glue.
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