CN111777794B - Hard wear-resistant super-hydrophobic material and preparation method thereof - Google Patents
Hard wear-resistant super-hydrophobic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hard wear-resistant super-hydrophobic material and a preparation method thereof, wherein the super-hydrophobic material is a porous hard block structure, polyurethane foam is used as a template, polytetrafluoroethylene nano-particles are used as a matrix phase, carbon nano-tubes are used as a reinforcing phase, and the mass ratio of the polytetrafluoroethylene nano-particles to the carbon nano-tubes is (3-24): 1; the preparation method comprises the steps of firstly preparing a dispersion liquid containing polytetrafluoroethylene nano-particles and carbon nano-tubes, then taking polyurethane foam as a template, facilitating the dispersion liquid to completely soak the template until the mass of the template is not increased any more, finally curing the soaked template, completely decomposing the polyurethane foam template through high-temperature curing, and finally preparing the superhydrophobic material with a porous hard block structure. The super-hydrophobic material provided by the invention has excellent super-hydrophobic performance, high temperature resistance and other performances, the preparation method provided by the invention is simple in process, and suitable for large-scale production, and the prepared product has excellent performance.
Description
Technical Field
The invention relates to the technical field of preparation of multifunctional super-hydrophobic materials, in particular to a hard wear-resistant super-hydrophobic material and a preparation method thereof.
Background
Since the scientific scientists Barthlott, neinhuis and the like in Germany explain the physical and chemical basis of the super-hydrophobic phenomenon, different types of super-hydrophobic materials are prepared by constructing the surfaces with low surface energy and micro-nano structures, and the number of coatings is large. Due to the fragile rough structure of the coating and the inevitable interface combination with the matrix, the coating is easy to lose the super-hydrophobic property when being subjected to the actions of friction, corrosion and high temperature of the external environment. This largely prevents large-scale application of superhydrophobic materials. Compared with the prior art, the super-hydrophobic bulk material can well overcome the defect of unsatisfactory wear resistance of the coating, and is expected to solve the problem of durability. However, the super-hydrophobic block prepared at present is mostly a flexible foam and is mainly used for oil-water separation, and although a larger block can be prepared, the applicability is limited due to the larger deformability. In addition, although the hard super-hydrophobic block is prepared in the prior art, the performances, particularly the temperature resistance and the wear resistance, need to be improved.
Disclosure of Invention
The invention provides a hard wear-resistant super-hydrophobic material and a preparation method thereof, which are used for overcoming the defects of insufficient temperature resistance and wear resistance and the like of a hard super-hydrophobic block in the prior art.
In order to achieve the purpose, the invention provides a hard wear-resistant super-hydrophobic material, which is a porous hard block structure, takes polyurethane foam as a template, takes Polytetrafluoroethylene (PTFE) nanoparticles as a matrix phase and takes Carbon Nanotubes (CNTs) as a reinforcing phase;
the mass ratio of the polytetrafluoroethylene nano particles to the carbon nano tubes is (3-24) to 1.
In order to achieve the above object, the present invention further provides a preparation method of a hard wear-resistant superhydrophobic material, the preparation method comprising:
s1: mixing polytetrafluoroethylene nano particles and carbon nano tubes according to the mass ratio of (3-24) to 1, placing the mixture in an organic solvent, performing ultrasonic treatment, and stirring to obtain a dispersion liquid;
s2: circularly soaking polyurethane foam in the dispersion liquid, drying and weighing the polyurethane foam after each soaking, and stopping the circular soaking when the mass of the polyurethane foam is not increased any more to obtain filled foam;
s3: and curing the filling foam in an inert atmosphere to obtain the hard wear-resistant super-hydrophobic material.
Compared with the prior art, the invention has the beneficial effects that:
1. the hard wear-resistant super-hydrophobic material provided by the invention is of a porous hard block structure, takes polyurethane foam as a template, takes polytetrafluoroethylene nanoparticles as a matrix phase and takes carbon nanotubes as a reinforcing phase; the mass ratio of the polytetrafluoroethylene nano particles to the carbon nano tubes is (3-24) to 1. The polyurethane foam is easy to decompose through pyrolysis, the block can have a porous structure after decomposition, the porous structure can provide a micro-nano secondary structure for the inside of the super-hydrophobic material, and when the surface of the super-hydrophobic material is abraded, the micro-nano secondary structure inside the super-hydrophobic material can still keep super-hydrophobicity. The polytetrafluoroethylene nano-particles have good hydrophobic property, chemical corrosion resistance, high temperature resistance and extremely low friction coefficient. The carbon nano tube can greatly improve the mechanical property of the porous hard block structure, so that the porous hard block structure can keep the structural stability in a general stress environment. Therefore, the super-hydrophobic material provided by the invention has excellent super-hydrophobic performance, good linear friction resistance, particle impact resistance, corrosion resistance, high temperature resistance and other performances.
2. The hard wear-resistant super-hydrophobic material provided by the invention has good friction resistance. The surface of the super-hydrophobic material can still keep good super-hydrophobicity by linear friction of 48m on 80-mesh sand paper under the pressure of 5 KPa. The porous structure of the super-hydrophobic material can continuously provide a micro-nano secondary structure, and super-hydrophobicity can be ensured in the whole friction process, so that the super-hydrophobic material provided by the invention is far beyond the wear resistance of common super-hydrophobic coatings and blocks.
3. The hard wear-resistant super-hydrophobic material provided by the invention has good gravel impact resistance. It still has good superhydrophobic performance after being impacted by 4kg gravel at a height of 30 cm.
4. Hair brushThe hard wear-resistant super-hydrophobic material has good corrosion resistance. The super-hydrophobic material can still maintain the super-hydrophobic performance after being soaked in 5mol/L NaOH solution for 48h or soaked in aqua regia for 48 h. The super-hydrophobic hard blocks reported in the prior literature are mostly SiO 2 The substrate (Journal of Materials Chemistry A6 (2018) 357-362, journal of Materials Chemistry 22 (2012)) can only endure corrosion of about 1h under strong acid (PH = 1) and strong alkali (PH = 14).
5. The hard wear-resistant super-hydrophobic material provided by the invention has good high-temperature resistance. The super-hydrophobic material provided by the invention is heated for 300min in a high-temperature environment of 400 ℃, and the coarse structure and good super-hydrophobicity can be still maintained; the existing hard block super-hydrophobic material can only bear the high temperature of 250 ℃; compared with the prior art, the super-hydrophobic material provided by the invention has more excellent high-temperature resistance.
6. The hard wear-resistant super-hydrophobic material provided by the invention has good mechanical properties. Although the super-hydrophobic material presents a porous structure, due to the reinforcing effect of CNTs on PTFE, the porous hard block structure provided by the invention has excellent compressive strength and compressive modulus, has the compressive strength of 2.9MPa and the compressive modulus of 8.4GPa, and can meet the general stress environment of the material. The tensile modulus of the existing superhydrophobic blocks is only 0.55MPa.
7. The preparation method of the hard wear-resistant super-hydrophobic material provided by the invention adopts a template method to prepare, firstly, a dispersion liquid containing polytetrafluoroethylene nano-particles and carbon nano-tubes is prepared, then polyurethane foam is used as a template, the template is favorably and completely soaked by the dispersion liquid until the mass of the template is not increased any more, finally, the soaked template is cured, the polyurethane foam template is completely decomposed by high-temperature curing, and finally, the super-hydrophobic material with a porous hard block structure is prepared. The preparation method provided by the invention is simple in process and suitable for large-scale production, and the prepared super-hydrophobic material has excellent super-hydrophobic property, good linear friction resistance, particle impact resistance, corrosion resistance, high temperature resistance and other properties.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is an SEM image at 50 μm of the superhydrophobic material prepared in example 1;
FIG. 2 is an SEM image at 5 μm of the superhydrophobic material prepared in example 1;
FIG. 3 is a graph illustrating the wear resistance test of the superhydrophobic material prepared in example 1;
FIG. 4 is a sand impact test result of the superhydrophobic material prepared in example 1;
FIG. 5 is a graph showing the results of a corrosion resistance test on the superhydrophobic material prepared in example 1;
FIG. 6 is a graph showing the result of a high temperature resistance test of the superhydrophobic material prepared in example 1;
FIG. 7 is an SEM photograph at 1 μm of the material prepared in comparative example 2;
FIG. 8 is an SEM image at 50 μm of the material prepared in comparative example 2.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The drugs/reagents used are all commercially available without specific indication.
The invention provides a hard wear-resistant super-hydrophobic material, which is of a porous hard block structure, takes polyurethane foam as a template, takes polytetrafluoroethylene nanoparticles as a matrix phase and takes carbon nanotubes as a reinforcing phase;
the mass ratio of the polytetrafluoroethylene nano particles to the carbon nano tubes is (3-24) to 1.
The hard wear-resistant super-hydrophobic material provided by the invention is of a porous hard block structure, takes polyurethane foam as a template, takes polytetrafluoroethylene nanoparticles as a matrix phase and takes carbon nanotubes as a reinforcing phase; the mass ratio of the polytetrafluoroethylene nano particles to the carbon nano tubes is (3-24) to 1. The polyurethane foam is easy to decompose through pyrolysis, the block can have a porous structure after decomposition, the porous structure can provide a micro-nano secondary structure for the inside of the super-hydrophobic material, and when the surface of the super-hydrophobic material is abraded, the micro-nano secondary structure in the super-hydrophobic material can still keep super-hydrophobicity. The polytetrafluoroethylene nano-particles have good hydrophobic property, chemical corrosion resistance, high temperature resistance and extremely low friction coefficient. The carbon nano tube can greatly improve the mechanical property of the porous hard block structure, so that the porous hard block structure can keep the structural stability in a general stress environment. Therefore, the super-hydrophobic material provided by the invention has excellent super-hydrophobic performance, good linear friction resistance, particle impact resistance, corrosion resistance, high temperature resistance and other performances.
Preferably, the carbon nanotube is a modified carbon nanotube, and the modifying step of the modified carbon nanotube is as follows: mixing carbon nanotubes, 1H, 2H-perfluorodecyltrimethoxysilane, ethanol and water according to the mass ratio of 1: 0.5.
After the carbon nano tube is modified by the fluorosilane, the corresponding fluorosilane long chain is modified on the surface defects and ports of the carbon nano tube, so that the dispersity and the surface performance of the carbon nano tube are improved.
Preferably, the particle size of the polytetrafluoroethylene nanoparticles is 0.1-10 μm, and an ideal dispersion is difficult to obtain if the particle size is too large or too small, which is not favorable for penetrating the foam template.
The carbon nano tube has the diameter of 4-6 nm, the length of 2-500 mu m, the diameter is too short to play a role in enhancing, and the diameter is too long, so that the uniformity of the dispersion liquid is poor due to the winding of the carbon nano tube, and the carbon nano tube is difficult to permeate the foam template.
The invention also provides a preparation method of the hard wear-resistant super-hydrophobic material, which comprises the following steps:
s1: mixing polytetrafluoroethylene nano particles and carbon nano tubes according to the mass ratio of (3-24) to 1, placing the mixture in an organic solvent, performing ultrasonic treatment, and stirring to obtain a dispersion liquid (for use in situ);
the ultrasonic time is preferably 10-30 min, and the stirring time is preferably 10-20 min, so that the polytetrafluoroethylene nanoparticles and the carbon nanotubes are fully and uniformly mixed and uniformly dispersed in the organic solvent.
Preferably, the mass ratio of the organic solvent to the carbon nanotubes is 50. The mass ratio is controlled to control the concentration of the polytetrafluoroethylene nanoparticles and the carbon nanotubes in the dispersion, the dispersion is difficult to soak the foam when the concentration is too high, and the efficiency is low when the concentration is too low.
Preferably, the organic solvent is one of ethanol, acetone and ethyl acetate, and has good dispersibility on the nanoparticles.
Preferably, the particle size of the polytetrafluoroethylene nanoparticles is 0.1-10 μm, and an ideal dispersion is difficult to obtain if the particle size is too large or too small, which is not favorable for penetrating the foam template.
The carbon nano tube has the diameter of 4-6 nm, the length of 2-500 mu m, too short diameter and no reinforcing effect, and too long diameter, the dispersion liquid has poor uniformity due to the winding of the carbon nano tube, and the foam template is difficult to permeate.
S2: circularly soaking polyurethane foam in the dispersion liquid, drying and weighing the polyurethane foam after each soaking, and stopping the circular soaking when the mass of the polyurethane foam is not increased any more to obtain filled foam;
preferably, the cyclic soaking is performed at normal temperature, and the complete penetration of the polyurethane foam by the dispersion liquid can be realized at normal temperature.
Preferably, the number of cycles of the cyclic soaking is 9 to 12 to ensure that the polyurethane foam is completely impregnated with the dispersion.
S3: and curing the filling foam in an inert atmosphere to obtain the hard wear-resistant super-hydrophobic material.
Preferably, the curing is to heat the filled foam from room temperature to 365-400 ℃ and keep the temperature at 365-400 ℃ for 1-3 h.
Curing to completely decompose the polyurethane foam template to form the superhydrophobic material of the porous hard block structure.
Preferably, the inert atmosphere is argon or nitrogen to prevent oxidation of the carbon nanotubes.
The preparation method of the hard wear-resistant super-hydrophobic material provided by the invention adopts a template method to prepare, firstly, a dispersion liquid containing polytetrafluoroethylene nano-particles and carbon nano-tubes is prepared, then polyurethane foam is used as a template, the template is favorably and completely soaked by the dispersion liquid until the mass of the template is not increased any more, finally, the soaked template is cured, the polyurethane foam template is completely decomposed by high-temperature curing, and finally, the super-hydrophobic material with a porous hard block structure is prepared. The preparation method provided by the invention is simple in process and suitable for large-scale production, and the prepared super-hydrophobic material has excellent super-hydrophobic performance, good linear friction resistance, particle impact resistance, corrosion resistance, high temperature resistance and other performances.
Example 1
The embodiment provides a hard wear-resistant super-hydrophobic material, which is a porous hard block structure, takes polyurethane foam as a template, takes Polytetrafluoroethylene (PTFE) nanoparticles as a matrix phase, and takes Carbon Nanotubes (CNTs) as a reinforcing phase;
the mass ratio of the polytetrafluoroethylene nanoparticles to the carbon nanotubes is 7.33:1.
the embodiment also provides a preparation method of the hard wear-resistant super-hydrophobic material, which comprises the following steps:
s1: mixing 8.8g of polytetrafluoroethylene nanoparticles and 1.2g of carbon nanotubes, placing the mixture in 60g of ethanol solution, then carrying out ultrasonic dispersion in an ultrasonic dispersion instrument for 20min, and then carrying out high-speed shearing and stirring for 10min to obtain a dispersion liquid;
s2: circularly soaking a rectangular polyurethane foam in the dispersion liquid obtained in the step S1 for 10 times, drying and weighing the polyurethane foam after each soaking, and obtaining filling foam when the mass of the polyurethane foam is not increased any more when the rectangular polyurethane foam is circularly soaked to the 10 th time;
s3: and in a nitrogen atmosphere, heating the filled foam in a tube furnace to 375 ℃, preserving the heat at 375 ℃ for 2h, and cooling to room temperature to obtain the hard wear-resistant super-hydrophobic material.
The super-hydrophobic material prepared by the embodiment has excellent mechanical properties, the compression strength is 2.9MPa, and the modulus is 8.4GPa.
Fig. 1 and 2 are SEM images of the superhydrophobic material in this example. From the figure, the micro-nano secondary structure of the surface of the super-hydrophobic material prepared by the embodiment can be obviously observed, and the micro-nano secondary structure is important for the super-hydrophobic performance.
Fig. 3 is a wear resistance test chart of the superhydrophobic material prepared in this example. After 1200 times of cyclic friction (distance is 48 m) under the condition of using 800-mesh sand paper and 5kPa pressure, the contact angle of the surface of the super-hydrophobic material can still be kept above 150 degrees, and the rolling angle is kept below 10 degrees.
Fig. 4 is a sand impact test result of the superhydrophobic material prepared in this example. As can be seen from the graph, the surface of the super-hydrophobic material prepared by the embodiment has excellent gravel impact resistance, and after 20 times of impact (the weight of the gravel is 4000 g), the contact angle of the surface can still be kept above 150 degrees, and the rolling angle is kept below 10 degrees.
Fig. 5 is a graph of a result of a corrosion resistance test of the superhydrophobic material prepared in this example, and it can be seen from the graph that after soaking in aqua regia (left side of fig. 5) and 5mol/L NaOH solution (right side of fig. 5) for 48 hours, a contact angle of a block surface can be still maintained above 150 °, and a rolling angle is maintained below 10 °.
FIG. 6 is a graph showing the test results of the superhydrophobic material prepared in this example, wherein after the pattern is heated at 400 ℃ for 300min, the surface contact angle is still maintained above 150 degrees, and the rolling angle is maintained below 10 degrees.
Comparative example 1
The comparative example provides a method for preparing a superhydrophobic material, and compared with example 1, the dispersion of the comparative example only contains Polytetrafluoroethylene (PTFE) nanoparticles, and the other steps are the same as example 1.
The material prepared by the preparation method provided by the comparative example cannot be molded, i.e., cannot form a porous hard block structure.
Comparative example 2
Compared with the example 1, the mass ratio of the PTFE nano particles to the CNTs in the comparative example is 3.
Although the material prepared by the comparative example can be molded, the mechanical property is poor, and as can be seen from fig. 7 and 8, the CNTs prepared by the comparative example have an agglomeration phenomenon, so that the reinforcing effect of the CNTs cannot be exerted.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. A preparation method of a hard wear-resistant super-hydrophobic material is characterized by comprising the following steps:
s1: mixing polytetrafluoroethylene nanoparticles and carbon nanotubes according to a mass ratio of (3 to 24) to 1, placing the mixture in an organic solvent, carrying out ultrasonic dispersion, and then carrying out high-speed shearing stirring to obtain a dispersion liquid;
s2: circularly soaking polyurethane foam in the dispersion liquid, drying and weighing the polyurethane foam after each soaking, and stopping the circular soaking when the mass of the polyurethane foam is not increased any more to obtain filled foam;
s3: curing the filling foam in an inert atmosphere to obtain a hard wear-resistant super-hydrophobic material;
the super-hydrophobic material is in a porous hard block structure, takes polyurethane foam as a template, takes polytetrafluoroethylene nano-particles as a matrix phase and takes carbon nano-tubes as a reinforcing phase.
2. The method of claim 1, wherein the carbon nanotubes are modified carbon nanotubes, and the step of modifying the modified carbon nanotubes comprises: mixing carbon nanotubes, 1H, 2H-perfluorodecyltrimethoxysilane, ethanol and water according to the mass ratio of 1: 0.5.
3. The production method according to claim 1, wherein in step S1, the mass ratio of the organic solvent to the carbon nanotubes is 50.
4. The method according to claim 1 or 3, wherein the organic solvent is one of ethanol, acetone and ethyl acetate.
5. The production method according to claim 1 or 3, wherein the particle size of the polytetrafluoroethylene nanoparticle is 0.1 to 10 μm; the diameter of the carbon nano tube is 4 to 6nm, and the length of the carbon nano tube is 2 to 500 mu m.
6. The method according to claim 1, wherein the number of cycles of the cyclic soaking in step S2 is 9 to 12.
7. The preparation method according to claim 1, wherein in the step S3, the curing is carried out by heating the filled foam from room temperature to 365 to 400 ℃ and keeping the temperature at 365 to 400 ℃ for 1 to 3 hours.
8. The method of claim 1 or 7, wherein the inert atmosphere is argon or nitrogen.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20180086838A (en) * | 2017-01-24 | 2018-08-01 | 주식회사 엘지화학 | Superhydrophobic film and manufacturing method thereof |
| CN109777012A (en) * | 2019-01-30 | 2019-05-21 | 中国人民解放军国防科技大学 | Epoxy-based super-hydrophobic fiber reinforced composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180086838A (en) * | 2017-01-24 | 2018-08-01 | 주식회사 엘지화학 | Superhydrophobic film and manufacturing method thereof |
| CN109777012A (en) * | 2019-01-30 | 2019-05-21 | 中国人民解放军国防科技大学 | Epoxy-based super-hydrophobic fiber reinforced composite material and preparation method thereof |
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| Title |
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| Superhydrophobic 3D Porous PTFE/TiO2 Hybrid Structures;Oral Cenk Aktas et al;《Advanced Material Interfaces》;20190130(第6期);第1-5页 * |
| 油水分离用超浸润表面制备及其性能研究;陈发泽;《中国博士学位论文全文数据库》;20190615(第06期);第1.4、4.1节 * |
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