CN112011083A - Preparation of multifunctional wax-impregnated porous PVDF film with convertible temperature response surface and corrosion resistance - Google Patents
Preparation of multifunctional wax-impregnated porous PVDF film with convertible temperature response surface and corrosion resistance Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/42—Impregnation with macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/044—Elimination of an inorganic solid phase
- C08J2201/0442—Elimination of an inorganic solid phase the inorganic phase being a metal, its oxide or hydroxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
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Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides a preparation method of a multifunctional wax-impregnated porous PVDF film with a convertible temperature response surface and corrosion resistance, belonging to the technical field of material preparation and comprising the following steps: before the PVDF film is formed, zinc oxide nano-particles are doped into a PVDF polymer as a pore-foaming agent; then, simple acid washing is carried out to remove zinc oxide, so as to generate a porous film; finally, the porous film is lubricated by wax, and the characteristic enhances the wettability of the surface of the PVDF film, thereby showing a surface with thermal response, anticorrosion protection and firm structure.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to preparation of a multifunctional wax-impregnated porous PVDF film with a convertible temperature response surface and corrosion resistance.
Background
The progress of science and technology provides wide development space for the development of interface materials. Moisture resistant substrates have received great attention over the past decade due to their wide application in microfluidic self-cleaning coatings, corrosion protection, anti-icing, anti-fogging, and reduction of viscous drag.
The superhydrophobicity of the surface of the superhydrophobic material is due to air entrapped in the surface nanostructures when it is in contact with water droplets. This air trapping phenomenon leads to inconsistent three-phase (solid/air/water) contact on the surface, resulting in low adhesion. While the surface of the material can provide high water resistance, the surface cavities make it vulnerable to harsh operating conditions. These problems are solved by the introduction of a new functional material, called a liquid injection surface. Tests were conducted using this concept to retain a thin layer of lubricating structure in the porous network, forming a smooth, consistent and chemically uniform coating, resistant to various liquids, low adhesion and resistance to wetting, providing stability at extreme temperatures and pressures. In making a robust multifunctional film smooth surface, selecting an appropriate porous scaffold surface has a beneficial contribution to lubricant absorption stability in the core of processing and structural design.
PVDF was chosen as the porous scaffold surface in this subject. PVDF is a vinylidene fluoride homopolymer or a copolymer of vinylidene fluoride with other minor amounts of a fluorine-containing vinyl monomer. It is chemically stable and resistant to degradation when exposed to corrosive solvents including acids. PVDF has four semi-crystalline phases (α, β, g and d), although the nonpolar α phase is the most common phase in commercial production, but can induce phases accordingly depending on the application requirements, resulting in different properties.
Disclosure of Invention
The technical task of the invention is to provide the preparation of a multifunctional wax-impregnated porous PVDF film with a switchable temperature response surface and corrosion resistance aiming at the defects of the prior art.
The innovation points of the invention are mainly as follows:
1. PVDF was chosen as the porous scaffold surface because of its chemical stability and its ability to resist environmental corrosion when exposed to corrosive media.
2. The crystallinity or molecular orientation of the polymer can influence the interfacial property, and the crystallinity of the material is improved through the addition of a seed crystal or a pore-forming agent, so that the wettability is adjusted.
3. Zinc oxide particles are introduced into a PVDF solution as a porogen, creating interconnected pores in the film and inducing partial charges in the PVDF interface, which can induce beta phase nucleation or surface exposure of C-F polar bonds.
4. Wax is injected as a lubricant to introduce a temperature response effect to the material.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the preparation of multifunctional wax-impregnated porous PVDF film with switchable temperature response surface and corrosion resistance comprises the following steps:
before the PVDF film is formed, zinc oxide nano-particles are doped into a PVDF polymer as a pore-foaming agent;
then, simple acid washing is carried out to remove zinc oxide, so as to generate a porous film;
finally, the porous film is lubricated by wax, and the characteristic enhances the wettability of the surface of the PVDF film, thereby showing a surface with thermal response, anticorrosion protection and firm structure.
Optionally, the specific steps are as follows:
step S1, mixing PVDF powder with DMF, heating at 65 ℃ to prepare PVDF coating solution;
step S2, then, adding zinc oxide particles of different amounts to the PVDF solution to manufacture different porous films, sonicating the mixture for 30 minutes to uniformly mix the PVDF-zinc oxide mixture, and then casting the mixture on a petri dish to form a casting film;
step S3, subjecting the casting film to acid etching in which zinc oxide is to be dissolved by the acid to produce a porous film;
step S4, a quantity of wax lubricant is heated at 80 ℃ above its melting point, and the porous PVDF membrane is then dipped into the liquefied wax for 4 hours to ensure complete penetration.
Optionally, the zinc oxide particles are added in an amount of 0-30% by mass of the PVDF.
Optionally, PVDF and DMF are mixed in a mass ratio of m (PVDF) to m (DMF) of 1: 0.8-1.2.
Optionally, the resulting porous PVDF and wax are mixed in a mass ratio m (wax): m (porous PVDF): 1: 0.9-1.3.
Compared with the prior art, the preparation of the multifunctional wax-impregnated porous PVDF film with the convertible temperature response surface and the corrosion resistance has the following beneficial effects:
1. zinc oxide nanoparticles were incorporated into PVDF polymer as a porogen prior to casting, and then subjected to simple acid washing to remove the zinc oxide, thereby producing a porous membrane. The result is the creation of interconnected pores in the film and the induction of partial charges at the PVDF interface, initiating beta phase nucleation or surface exposure of C-F polar bonds.
2. Porous PVDF was impregnated with wax to construct a new film with thermal response and corrosion resistance. Provides a new idea for the construction of novel corrosion-resistant materials and super-hydrophobic materials.
Drawings
To more clearly illustrate the operation of the present invention in the preparation of a multifunctional wax-impregnated porous PVDF film having a switchable temperature responsive surface and corrosion resistance, a schematic diagram is shown below for further illustration.
FIG. 1 is an infrared spectrum of a multifunctional wax-impregnated porous PVDF film of the invention with switchable temperature response surface and corrosion resistance properties, with different zinc oxide contents;
FIG. 2 is a thickness test chart of PVDF films with different zinc oxide contents of the multifunctional wax-impregnated porous PVDF film with convertible temperature response surface and corrosion resistance;
FIG. 3 is an intra-film pore size test of a multifunctional wax-impregnated porous PVDF film with switchable temperature response surface and corrosion resistance, with different zinc oxide contents;
FIG. 4 is a test chart of wax loading of a multifunctional wax-impregnated porous PVDF film with switchable temperature response surface and corrosion resistance for PVDF films with different zinc oxide contents;
FIG. 5 is a water contact angle test chart of different temperatures of PVDF films with different zinc oxide contents of the multifunctional wax-impregnated porous PVDF film with convertible temperature response surface and anti-corrosion performance;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 5 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 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.
Example one
As shown in fig. 1 to 5, the preparation of a multifunctional wax-impregnated porous PVDF film with a switchable temperature response surface and corrosion resistance according to the present invention comprises the following steps:
before the PVDF film is formed, zinc oxide nano-particles are used as a pore-foaming agent to be doped into the PVDF polymer;
then, simple acid washing is carried out to remove zinc oxide, so as to generate a porous film;
finally, the porous film is lubricated by wax, and the characteristic enhances the wettability of the surface of the PVDF film, thereby showing a surface with thermal response, anticorrosion protection and firm structure.
The reagents adopted by the invention are as follows:
polyvinylidene fluoride (PVDF), N, N-dimethylformamide (DMF, 99%) and zinc oxide: (
Mesh powder) was purchased from Alfa Aesar. Hydrochloric acid (HCl, 37%) was purchased from Acros Organics. Paraffin wax was obtained from Aldrich Chemistry. Tetrabutylammonium acetate was purchased from Tokyo chemical industries, Inc. Ammonia was purchased from Duksan Pure Chemical Co., LTD. Sulfuric acid was purchased from Matsuneon Chemicals Ltd.
The method comprises the following specific steps:
step S1, mixing PVDF powder and DMF according to the mass ratio of 1:1, heating at 65 ℃ to prepare PVDF coating solution;
step S2, then, different amounts of zinc oxide particles were added to the PVDF solution, the amounts being 10%, 20%, 30% of the mass of the PVDF film, respectively, to manufacture different porous films. The mixture was sonicated for 30 minutes to uniformly mix the PVDF-zinc oxide mixture, and then the mixture was cast on a petri dish to form a casting film;
step S3, subjecting the casting film to acid etching in which zinc oxide is to be dissolved by the acid to produce a porous film;
step S4, weighing a certain amount of wax at a mass ratio of m (wax): m (porous PVDF): 1, heating the wax lubricant at 80 ℃ above its melting point, and then immersing the porous PVDF membrane in the liquefied wax for 4h to ensure complete penetration.
As shown in FIG. 1, the presence of the bicrystal phase of PVDF was confirmed by Fourier transform infrared spectroscopy, and the characteristic peaks of the alpha phase were at 762 and 1072cm, respectively-1It was observed. These peaks suddenly decrease or disappear as the zinc oxide content increases. At 773, 840, 975, 1276 and 1431cm-1The corresponding beta phase peak can be clearly distinguished, on the other hand, after zinc oxide is added into the PVDF film, the thickness is 441 cm, 481 cm and 501cm-1The peak observed therein demonstrates the formation of the beta phase.
As shown in fig. 2, which is a film thickness versus zinc oxide content increase, the film thickness increases with increasing zinc oxide content, which decreases the film density and provides more lubricant loading space for the film.
As shown in fig. 3, the diameter of the aperture was tested. It can be observed that the pore size gradually increases with increasing zinc oxide content. The resulting film has a structure that supports stable bonding of the lubricant. The zinc oxide content is too low to form a sufficient interconnected matrix of pores to facilitate loading of the wax lubricant.
As shown in fig. 4, PVDF porous substrates of varying zinc oxide content were tested for wax absorption. As the zinc oxide content increases, the coating thickness and pore size increase and the loading of the wax lubricant increases.
As shown in fig. 5, PVDF porous substrates of varying zinc oxide content were tested for lubrication stability. The difference in contact angle between PVDF films with different zinc oxide contents at 25 c is small due to the uneven distribution of wax on the surface of the porous PVDF film. In contrast, the phase change of the wax from solid to liquid is initiated by exposing the WIS film at Tm. At lower zinc oxide levels, the contact angle is lower due to lower amounts of wax lubrication. For lower zinc oxide concentrations, the films produced tend to be less porous and do not accommodate enough wax for slip, and the injected wax does not achieve a uniform wax interface.
Example two
The second embodiment is the same as the first embodiment except that:
in step S1, PVDF and DMF are mixed at a mass ratio of m (PVDF) to m (DMF) of 1: 0.8.
In step S4, the obtained porous PVDF and the wax are mixed in a mass ratio of m (wax) to m (porous PVDF) of 1: 1.3.
EXAMPLE III
The third embodiment is the same as the first embodiment except that:
in step S1, PVDF and DMF are mixed at a mass ratio of m (PVDF) to m (DMF) of 1: 1.2.
In step S4, the obtained porous PVDF and the wax are mixed in a mass ratio of m (wax) to m (porous PVDF) of 1: 0.9.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The preparation method of the multifunctional wax-impregnated porous PVDF film with a switchable temperature response surface and corrosion resistance is characterized by comprising the following steps:
before the PVDF film is formed, zinc oxide nano-particles are used as a pore-foaming agent to be doped into the PVDF polymer;
then, simple acid washing is carried out to remove zinc oxide, so as to generate a porous film;
finally, the porous film is lubricated by wax, and the characteristic enhances the wettability of the surface of the PVDF film, thereby showing a surface with thermal response, anticorrosion protection and firm structure.
2. The preparation method of the multifunctional wax-impregnated porous PVDF film with the convertible temperature response surface and the corrosion resistance performance according to claim 1 is characterized by comprising the following specific steps:
step S1, mixing PVDF powder with DMF, heating at 65 ℃ to prepare PVDF coating solution;
step S2, then, adding zinc oxide particles of different amounts to the PVDF solution to manufacture different porous films, sonicating the mixture for 30 minutes to uniformly mix the PVDF-zinc oxide mixture, and then casting the mixture on a petri dish to form a casting film;
step S3, subjecting the casting film to acid etching in which zinc oxide is to be dissolved by the acid to produce a porous film;
step S4, a quantity of wax lubricant is heated at 80 ℃ above its melting point, and the porous PVDF membrane is then dipped into the liquefied wax for 4 hours to ensure complete penetration.
3. The preparation method of the multifunctional wax-impregnated porous PVDF film with the switchable temperature response surface and the corrosion resistance performance as claimed in claim 2, wherein the addition amount of the zinc oxide particles is 0-30% of the mass of the PVDF.
4. The preparation of a multifunctional wax-impregnated porous PVDF film with switchable temperature response surface and anti-corrosion property as claimed in claim 2, wherein PVDF and DMF are mixed according to mass ratio m (PVDF) m (DMF) 1: 0.8-1.2.
5. The preparation method of the multifunctional wax-impregnated porous PVDF film with switchable temperature response surface and anti-corrosion property according to claim 2, wherein the obtained porous PVDF and wax are mixed according to the mass ratio m (wax) to m (porous PVDF) of 1: 0.9-1.3.
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