CN111363269A - PVC/PVDF/diatomite composite super-hydrophobic material - Google Patents
PVC/PVDF/diatomite composite super-hydrophobic material 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J2327/04—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 chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
Abstract
The invention discloses a PVC/PVDF/diatomite composite super-hydrophobic material, and belongs to the technical field of super-hydrophobic waterproof materials. The super-hydrophobic material mainly comprises the following components: 10-30 parts of PVC, 10-30 parts of PVDF, 30-80 parts of diatomite and 0.1-1 part of coupling agent. The material is prepared by a simple immersion precipitation method, can be prepared into a film or a sheet and is coated on the surface of an object needing super-hydrophobic treatment. The contact angle of the prepared material to water can reach 159 degrees, and the tensile strength reaches 1.2 MPa. The invention has the advantages of low cost and simple process, and the prepared finished material does not contain volatile organic solvent and is green and environment-friendly.
Description
Technical Field
The invention relates to a PVC/PVDF/diatomite composite super-hydrophobic material, belonging to the technical field of super-hydrophobic waterproof materials.
Background
In daily life, some equipment and facilities exposed outdoors for a long time, building outer walls or indoor toilet wall finishing materials and the like have certain requirements on waterproof performance. The existing known waterproof materials are generally realized by isolating water vapor, but after long-term use, the water vapor is adhered to the materials, so that the waterproof performance of the materials is reduced. Some waterproof materials imitating the lotus leaf surface realize the water resistance by utilizing the super-hydrophobic property of the materials, and the super-hydrophobic property achieves the aim of water resistance by avoiding the adhesion of water drops on the materials.
A superhydrophobic material is defined as a material having a contact angle with water of greater than 150 °. Some super-hydrophobic materials used and reported at present usually use polyvinylidene fluoride, polytetrafluoroethylene and other hydrophobic macromolecules as main materials, and the super-hydrophobic performance is realized by constructing a microscopic double coarse structure similar to the lotus leaf surface through a bionic technology. At present, the super-hydrophobic materials on the market are mainly composed of more than 90% of polymers, the super-hydrophobic materials generally have the characteristics of complex preparation process and high cost, and meanwhile, a certain amount of plasticizer and volatile organic matters harmful to human bodies are contained in order to meet certain mechanical strength, so that the wide application of the super-hydrophobic waterproof materials is limited.
Therefore, the environment-friendly super-hydrophobic waterproof material with simpler processing method and lower preparation cost has practical significance for popularization of the super-hydrophobic waterproof material and has wide market prospect.
Disclosure of Invention
In order to solve the problems, the invention provides a PVC/PVDF/diatomite composite super-hydrophobic material, wherein the super-hydrophobic material is obtained by compounding PVC, PVDF and diatomite, the super-hydrophobic performance is ensured by the PVDF under the condition that PVC provides a certain mechanical strength, the raw material of the super-hydrophobic material also comprises a large amount of cheap diatomite, the product cost is greatly reduced, and volatile organic matters harmful to human bodies are not contained.
The invention provides a PVC/PVDF/diatomite composite super-hydrophobic material, which comprises the following components: the composite material comprises, by weight, 10-30 parts of PVC, 10-30 parts of PVDF, 30-80 parts of diatomite and 0.1-1 part of a coupling agent.
In one embodiment of the invention, the composition of the super-hydrophobic material further comprises 1-3 parts of toning dye for preparing super-hydrophobic materials with different colors.
In one embodiment of the present invention, the PVC raw material is a paste resin having a commercially available polymerization degree of 1200 to 1800.
In one embodiment of the present invention, the PVDF raw material is spherical resin particles having a commercially available polymerization degree of 1000 to 2000.
In one embodiment of the present invention, the diatomaceous earth is ground to a diatomaceous earth powder having a particle size of 1 to 50 μm after removing impurities.
In one embodiment of the invention, the coupling agent is an organosiloxane or phthalate ester coupling agent, and the coupling agent is prepared into a mother solution with a mass fraction of 1-10% by using water or ethanol.
The second purpose of the invention is to provide a preparation method of the PVC/PVDF/diatomite composite super-hydrophobic material, wherein the preparation method comprises the following steps: mixing PVC, diatomite, a dissolving solution, a coupling agent and the like, heating and refluxing, standing and defoaming, scraping the mixed solution into a sheet by a scraper, and then immersing and precipitating in a coagulating bath to obtain a substrate; after drying, preparing the PVDF mixed solution by the same process, scraping the obtained substrate into a film and a sheet, and drying and cutting to obtain the final product.
In one embodiment of the present invention, the preparation method of the PVC/PVDF/diatomite composite superhydrophobic material specifically comprises the following steps:
(1) dissolving 10-30 parts by mass of PVC in a dissolving solution, adding 1-10% by mass of a coupling agent mother solution, and refluxing, heating and stirring at 30-100 ℃;
(2) adding 15-40 parts of diatomite into the solution obtained in the step (1), and continuously stirring, heating and stirring to obtain a PVC mixture;
(3) placing the pasty PVC/diatomite mixture obtained in the step (2) into a closed container, and standing and defoaming at 30-70 ℃ for 1-4 hours;
(4) horizontally scraping the film into sheets by using a scraper, wherein the substrate of the scraped film is a glass plane, the distance between the scraper and the substrate is 0.05-2 mm, and standing for 10-600 seconds after scraping;
(5) immersing the glass substrate covered with the PVC/diatomite mixture after standing in the step (4) in a coagulating bath solution, precipitating the covered PVC/diatomite mixture to form a sheet-shaped film, automatically separating the sheet-shaped film from the glass substrate, and drying the sheet-shaped film to obtain a PVC/diatomite composite substrate;
(6) repeating the processes (1) to (3), replacing PVC with PVDF, taking 10-30 parts of PVDF and 15-40 parts of diatomite to prepare a PVDF/diatomite mixed solution, standing at 30-70 ℃ for defoaming for 1-4 hours, scraping a film on the PVC/diatomite composite substrate prepared in the step (5) into a sheet by using a scraper, keeping the distance between the scraper and the substrate at 0.05-2 mm, and standing for 10-600 seconds to fuse the PVDF/diatomite mixed solution on the surface layer and the PVC/diatomite composite substrate on the bottom layer;
(7) and (4) immersing the composite substrate obtained in the step (6) in a coagulating bath solution to enable the PVDF/diatomite mixed solution to be precipitated on the surface of the substrate, and drying after flaking to obtain the soft flaky PVC/PVDF/diatomite composite super-hydrophobic material.
In an embodiment of the present invention, the dissolving solution is one of dimethylformamide, dimethylacetamide, tetrahydrofuran, and cyclohexanone.
In one embodiment of the invention, the amount of the dissolving solution is 5 to 10 times the amount of the PVC or PVDF.
In one embodiment of the invention, the coagulation bath is water, or an aqueous solution containing a small amount of a dissolving solution, the content of the dissolving solution being not more than 30 wt%.
In one embodiment of the invention, the prepared PVC/PVDF/diatomite composite super-hydrophobic material needs to be cut into required sizes.
In one embodiment of the present invention, the mass ratio of PVC and diatomite in the PVC/diatomite mixture in step (3) is: (0.8: 1) to (1: 1).
In one embodiment of the present invention, the mass ratio of PVDF to diatomite in step (6) is: (0.8: 1) to (1: 1).
In one embodiment of the present invention, the mass ratio of PVDF to PVC is: (0.8: 1) to (1: 1).
The third purpose of the invention is to provide the application of the super-hydrophobic material in outdoor equipment and facilities, building outer walls or indoor toilet wall finishing materials.
The invention has the beneficial effects that:
(1) the PVC/PVDF/diatomite composite super-hydrophobic material provided by the invention has mechanical strength provided by a PVC/diatomite composite substrate, and the PVDF is self-assembled by taking diatomite as a framework to form a nano-scale waterproof bionic surface rough structure by using an immersion precipitation method, so that the super-hydrophobic performance of the material is ensured, the cost is greatly saved (the material is formed by more than 50% of cheap diatomite), and volatile organic matters harmful to human bodies are not contained.
(2) The super-hydrophobic material is treated by the coupling agent, so that the material still has good mechanical properties under the condition that more than 70% of diatomite by total mass is added, and the affinity between the diatomite and a polymer can be improved by adding a small amount of the coupling agent in the process of mixing the diatomite.
(3) The super-hydrophobic material prepared by the invention has a porosity of over 60 percent and has air permeability under the condition of ensuring waterproofness.
(4) The invention adopts a simple film scraping forming process, has very low requirement on production equipment and can realize large-scale industrial production.
(5) The super-hydrophobic material obtained by the invention is a sheet or film material light material, the thickness of the super-hydrophobic material is 0.2-2 mm, the porosity is 60-80%, the tensile strength is 1.2Mpa, and the maximum contact angle to water can reach 159 degrees.
Drawings
FIG. 1 is a schematic structural diagram of a superhydrophobic material.
FIG. 2 scanning electron microscope images and contact angle test images of the surface of the superhydrophobic material prepared in example 1.
Fig. 3 a surface scanning electron micrograph and a contact angle test chart of the superhydrophobic material prepared in example 2.
Fig. 4 a scanning electron microscope image and a contact angle test image of the surface of the superhydrophobic material prepared in example 3.
Fig. 5 is an apparent photograph of the superhydrophobic material prepared in comparative example 1.
FIG. 6 is an apparent photograph of the superhydrophobic material prepared in comparative example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described with reference to the following specific embodiments.
Tensile strength test method: according to a tensile strength testing device self-made by national standard JB/T7630.1-2008, a partition plate is cut into dumbbell-shaped strips with the middle width of 1cm and the total length of 5cm, the dumbbell-shaped strips are clamped by clamps, a light plastic container is hung below the clamps, fine sand serving as a weight is slowly added into the plastic container until the partition plate is broken, the fine sand and the weight of a system (comprising the clamps and the plastic container) are weighed, and the tensile strength is calculated according to the following formula.
In the formula, δ: tensile strength (Mp); m: fine sand mass (kg); g: acceleration of gravity; b: fracture cross-sectional length (mm); d: fracture cross-sectional width (mm).
Contact angle test method: a dynamic video contact angle measuring instrument is used, a sitting drop method is adopted, the volume of a liquid drop is 10 mu L, the spreading and wetting absorption process of the liquid drop on the surface of the sheet is tested, and the contact angle of the water drop on the partition plate can be obtained through the contact angle calculation function of software of the instrument.
Example 1
(1) Weighing 25 parts of PVC (polyvinyl chloride) by mass, dissolving the PVC in 150 parts of dimethylformamide, adding 1 part of silane coupling agent KH-550 mother liquor with the mass fraction of 2%, and refluxing, heating and stirring at 80 ℃;
(2) adding 25 parts of diatomite into the solution, and continuously stirring, heating and stirring to obtain a PVC/diatomite mixture;
(3) placing the PVC/diatomite mixture obtained in the step (2) into a closed container, and standing and defoaming for 2 hours at 60 ℃;
(4) horizontally scraping into a sheet by using a scraper, wherein the substrate of the scraped film is a glass plane, the distance between the scraper and the substrate is 1 mm, and standing for 10 seconds;
(5) immersing the substrate covered with the PVC/diatomite mixture after standing in an aqueous solution, and immediately precipitating the mixture to form a flaky PVC/diatomite composite substrate and drying the flaky PVC/diatomite composite substrate;
(6) replacing PVC with PVDF, 25 parts of PVDF and 25 parts of diatomite as shown in the flows of (1) to (3), preparing a PVDF/diatomite mixed solution, standing at 70 ℃ for defoaming for 1 hour, scraping a film on the PVC/diatomite composite substrate prepared in the step (5) into a sheet by using a scraper, keeping the distance between the scraper and the substrate at 1 mm, and standing for 10 seconds;
(7) and (4) immersing and precipitating the PVC/diatomite composite substrate covered with the PVDF/diatomite mixed solution obtained in the step (6) in an aqueous solution, and drying after flaking to obtain the soft flaky PVC/PVDF/diatomite composite super-hydrophobic material.
FIG. 1 is a schematic structural diagram of the prepared superhydrophobic material.
The PVC/PVDF/diatomite composite superhydrophobic material prepared in the embodiment is subjected to a tensile strength test and a contact angle test, and the tensile strength of the superhydrophobic material prepared in the invention is 1.2Mpa, and the thickness of the superhydrophobic material is 1 mm. Fig. 2 is a surface scanning electron microscope image and a contact angle test image of the superhydrophobic material prepared in this example, and as can be seen from fig. 2, the contact angle of the superhydrophobic material reaches 159 °, the surface is formed by irregularly stacking spherical rough PVDF globules with a size of about 2 micrometers (the portion marked by a white circle in the figure), the superhydrophobic material is similar to a lotus leaf surface superhydrophobic microstructure, and bare hydrophilic diatomaceous earth is not seen, which indicates that the diatomaceous earth is well wrapped inside the material to serve as a framework support.
Example 2
(1) Weighing 20 parts of PVC (polyvinyl chloride) by mass, dissolving in 150 parts of dimethylformamide, adding 1 part of KH-550 mother liquor with the mass fraction of 2%, and refluxing, heating and stirring at 80 ℃;
(2) adding 30 parts of diatomite into the solution, and continuously stirring, heating and stirring to obtain a PVC/diatomite mixture;
(3) placing the PVC/diatomite mixture obtained in the step (2) into a closed container, and standing and defoaming for 2 hours at 60 ℃;
(4) horizontally scraping into a sheet by using a scraper, wherein the substrate of the scraped film is a glass plane, the distance between the scraper and a base is 1 mm, and standing for 10 seconds;
(5) immersing the substrate covered with the PVC/diatomite mixture after standing in an aqueous solution, and immediately precipitating the mixture to form a flaky PVC/diatomite composite substrate and drying the flaky PVC/diatomite composite substrate;
(6) replacing PVC with PVDF, 20 parts of PVDF and 30 parts of diatomite as shown in the flows of (1) to (3), preparing a PVDF/diatomite mixed solution, standing at 70 ℃ for defoaming for 1 hour, scraping a membrane on the PVC/diatomite composite substrate prepared in the step (5) by using a scraper to form a sheet, keeping the distance between the scraper and the substrate at 1 mm, and standing for 10 seconds;
(7) and (4) immersing and precipitating the PVC/diatomite composite substrate covered with the PVDF/diatomite mixed solution obtained in the step (6) in an aqueous solution, and drying after flaking to obtain the soft flaky PVC/PVDF/diatomite composite super-hydrophobic material.
The PVC/PVDF/diatomite composite superhydrophobic material prepared by the embodiment is subjected to a tensile strength test and a contact angle test, and the tensile strength of the superhydrophobic material prepared by the method is 0.8MPa, and the thickness of the superhydrophobic material is 2 millimeters. Fig. 3 is a surface scanning electron microscope image and a contact angle test image of the superhydrophobic material prepared in this embodiment, and as can be seen from fig. 3, the contact angle of the superhydrophobic material reaches 151 °, and besides PVDF globules with a size of about 2 μm that can be seen in fig. 2, bare hydrophilic diatomaceous earth (marked by a white circle in the figure) can be seen on the surface, which indicates that the diatomaceous earth is exposed out of the surface of the material due to excessive addition of the diatomaceous earth, and the hydrophobic effect is affected.
Example 3
(1) Weighing 30 parts of PVC (polyvinyl chloride) by mass, dissolving in 150 parts of dimethylformamide, adding 1 part of KH-550 mother liquor with the mass fraction of 2%, and refluxing, heating and stirring at 80 ℃;
(2) adding 20 parts of diatomite into the solution, and continuously stirring, heating and stirring to obtain a PVC/diatomite mixture;
(3) placing the PVC/diatomite mixture obtained in the step (2) into a closed container, and standing and defoaming for 2 hours at 60 ℃;
(4) horizontally scraping into a sheet by using a scraper, wherein the substrate of the scraped film is a glass plane, the distance between the scraper and a base is 1 mm, and standing for 10 seconds;
(5) immersing the substrate covered with the PVC/diatomite mixture after standing in an aqueous solution, and immediately precipitating the mixture to form a flaky PVC/diatomite composite substrate and drying the flaky PVC/diatomite composite substrate;
(6) replacing PVC with PVDF, 30 parts of PVDF and 20 parts of diatomite as shown in the flows of (1) to (3), preparing a PVDF/diatomite mixed solution, standing at 70 ℃ for defoaming for 1 hour, scraping a membrane on the PVC/diatomite composite substrate prepared in the step (5) by using a scraper to form a sheet, keeping the distance between the scraper and the substrate at 1 mm, and standing for 10 seconds;
(7) and (4) immersing and precipitating the PVC/diatomite composite substrate covered with the PVDF/diatomite mixed solution obtained in the step (6) in an aqueous solution, and drying after flaking to obtain the soft flaky PVC/PVDF/diatomite composite super-hydrophobic material.
The PVC/PVDF/diatomite composite superhydrophobic material prepared in the embodiment is subjected to a tensile strength test and a contact angle test, and the tensile strength of the superhydrophobic material prepared in the invention is 1.5Mpa, and the thickness of the superhydrophobic material is 1 mm. Fig. 4 is a surface scanning electron microscope image and a contact angle test image of the superhydrophobic material prepared in this embodiment, and as can be seen from fig. 4, the contact angle of the superhydrophobic material reaches 84 °, the PVDF bead stacking of about 2 micrometers in fig. 2 is not seen on the surface, and the bare hydrophilic diatomaceous earth is not seen on the surface, and the beads formed by the PVDF are greatly fused, which is a result of excessive addition of PVDF and too long standing time, indicating that the bionic microstructure of bead stacking cannot be formed due to excessive addition of PVDF, and the hydrophobic effect is affected.
Comparative example 1 preparation sequence was changed
(1) Weighing 25 parts of PVDF by mass, dissolving in 150 parts of dimethylformamide, adding 1 part of KH-550 mother liquor with the mass fraction of 2%, refluxing at 80 ℃, heating and stirring;
(2) adding 25 parts of diatomite into the solution, and continuously stirring, heating and stirring to obtain a PVDF/diatomite mixture;
(3) placing the PVDF/diatomite mixture obtained in the step (2) in a closed container, standing and defoaming for 2 hours at 60 ℃;
(4) horizontally scraping into a sheet by using a scraper, wherein the substrate of the scraped film is a glass plane, the distance between the scraper and a base is 1 mm, and standing for 10 seconds;
(5) immersing the substrate covered with the PVDF/diatomite mixture after standing in an aqueous solution, and immediately precipitating the mixture to form a flaky PVC/diatomite composite substrate and drying the substrate;
(6) replacing PVDF with PVC, 25 parts of PVC and 25 parts of diatomite as shown in the flows of (1) to (3), preparing a PVC/diatomite mixed solution, standing at 70 ℃ for defoaming for 1 hour, scraping a film on the PVDF/diatomite composite substrate prepared in the step (5) into a sheet by using a scraper, keeping the distance between the scraper and the substrate at 1 mm, and standing for 10 seconds;
(7) and (4) immersing and precipitating the PVDF/kieselguhr composite substrate covered with the PVC/kieselguhr mixed solution obtained in the step (6) in an aqueous solution, and drying after flaking to obtain the soft flaky PVC/PVDF/kieselguhr composite super-hydrophobic material.
This example is comparative example 1, reversing the PVC to PVDF knifing sequence, FIG. 5 is the material obtained, it can be seen that the mechanical properties of the material are very poor, breaking with impact.
Comparative example 2 changing the amount of dimethylformamide
(1) Weighing 25 parts of PVDF by mass, dissolving in 300 parts of dimethylformamide, adding 1 part of KH-550 mother liquor with the mass fraction of 2%, refluxing at 80 ℃, heating and stirring;
(2) adding 25 parts of diatomite into the solution, and continuously stirring, heating and stirring to obtain a PVDF/diatomite mixture;
(3) placing the PVDF/diatomite mixture obtained in the step (2) in a closed container, standing and defoaming for 2 hours at 60 ℃;
(4) horizontally scraping into a sheet by using a scraper, wherein the substrate of the scraped film is a glass plane, the distance between the scraper and a base is 1 mm, and standing for 10 seconds;
(5) immersing the substrate covered with the PVDF/diatomite mixture after standing in an aqueous solution, and immediately precipitating the mixture to form a flaky PVC/diatomite composite substrate and drying the substrate;
(6) replacing PVDF with PVC, 25 parts of PVC and 25 parts of diatomite as shown in the flows of (1) to (3), preparing a PVC/diatomite mixed solution, standing at 70 ℃ for defoaming for 1 hour, scraping a film on the PVDF/diatomite composite substrate prepared in the step (5) into a sheet by using a scraper, keeping the distance between the scraper and the substrate at 1 mm, and standing for 10 seconds;
(7) and (4) immersing and precipitating the PVDF/kieselguhr composite substrate covered with the PVC/kieselguhr mixed solution obtained in the step (6) in an aqueous solution, and drying after flaking to obtain the soft flaky PVC/PVDF/kieselguhr composite super-hydrophobic material.
Fig. 6 shows that the surface flatness of the obtained material is particularly poor, because the excessive solvent dimethyl formamide is used, so that the solution is too thin, excessive shrinkage occurs in the immersion precipitation process, and the surface is wrinkled, which is not beneficial to controlling the size and shape of the product.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A superhydrophobic material, wherein the composition of the superhydrophobic material comprises: the composite material comprises, by weight, 10-30 parts of PVC, 10-30 parts of PVDF, 30-80 parts of diatomite and 0.1-1 part of a coupling agent.
2. The super-hydrophobic material as claimed in claim 1, wherein the diatomite is purified and ground to obtain diatomite powder with a particle size of 1-50 μm.
3. The super-hydrophobic material as claimed in claim 1, wherein the coupling agent is an organosiloxane or phthalate ester coupling agent, and the coupling agent is prepared into a mother solution with a mass fraction of 1-10% by using water or ethanol.
4. The preparation method of the superhydrophobic material of claim 1, characterized in that the preparation method of the superhydrophobic material comprises the following specific steps:
(1) dissolving 10-30 parts by mass of PVC in a dissolving solution, adding 1-10% by mass of a coupling agent mother solution, and refluxing, heating and stirring at 30-100 ℃;
(2) adding 15-40 parts of diatomite into the solution prepared in the step (1), and continuously stirring, heating and stirring to obtain a PVC/diatomite mixture;
(3) placing the pasty PVC/diatomite mixture obtained in the step (2) into a closed container, and standing and defoaming at 30-70 ℃ for 1-4 hours;
(4) horizontally scraping the film into a sheet by using a scraper, wherein the distance between the scraper and the substrate is 0.05-2 mm, and standing for 10-600 seconds after scraping;
(5) immersing the substrate covered with the PVC/diatomite mixture after standing in the step (4) in a coagulating bath solution, precipitating the covered PVC/diatomite mixture to form a sheet-shaped film, automatically separating the sheet-shaped film from the substrate, and drying the sheet-shaped film to obtain a PVC/diatomite composite substrate;
(6) repeating the processes (1) to (3), replacing PVC with PVDF, taking 10-30 parts of PVDF and 15-40 parts of diatomite to prepare a PVDF/diatomite mixed solution, standing at 30-70 ℃ for defoaming for 1-4 hours, scraping a film on the PVC/diatomite composite substrate prepared in the step (5) into a sheet by using a scraper, keeping the distance between the scraper and the substrate at 0.05-2 mm, and standing for 10-600 seconds to fuse the PVDF/diatomite mixed solution on the surface layer and the PVC/diatomite composite substrate on the bottom layer;
(7) and (4) immersing the composite substrate obtained in the step (6) in a coagulating bath solution to enable the PVDF/diatomite mixed solution to be precipitated on the surface of the substrate, and drying after flaking to obtain the soft flaky PVC/PVDF/diatomite composite super-hydrophobic material.
5. The method for preparing the superhydrophobic material of claim 4, wherein the dissolving solution is one of dimethylformamide, dimethylacetamide, tetrahydrofuran and cyclohexanone.
6. The method for preparing the superhydrophobic material of claim 4, wherein the dissolving solution is used in an amount 5-10 times that of the PVC or PVDF.
7. The preparation method of the superhydrophobic material according to claim 4, wherein the mass ratio of the PVC to the diatomite is as follows: (0.8: 1) to (1: 1).
8. The preparation method of the superhydrophobic material according to claim 4, wherein the mass ratio of the PVDF to the diatomite is as follows: (0.8: 1) to (1: 1).
9. The preparation method of the superhydrophobic material according to claim 4, wherein the mass ratio of PVDF to PVC is as follows: (0.8: 1) to (1: 1).
10. Use of the superhydrophobic material of any one of claims 1-3 in outdoor equipment facilities, building exterior walls, or interior toilet wall finishing materials.
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| CN112724929A (en) * | 2021-01-13 | 2021-04-30 | 深圳市顾康力化工有限公司 | Water-in-oil type emulsion adhesive and preparation method thereof |
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| CN103762328A (en) * | 2014-01-24 | 2014-04-30 | 福州大学 | Separator for colloid lead acid storage battery and preparation method thereof |
| CN106823829A (en) * | 2017-02-24 | 2017-06-13 | 天津工业大学 | A kind of preparation method of super-hydrophobicity pvdf membrane |
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| CN112724929A (en) * | 2021-01-13 | 2021-04-30 | 深圳市顾康力化工有限公司 | Water-in-oil type emulsion adhesive and preparation method thereof |
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