CN110144135A - A kind of super-amphiphobic coating material and preparation method thereof and super-amphiphobic coating - Google Patents
A kind of super-amphiphobic coating material and preparation method thereof and super-amphiphobic coating Download PDFInfo
- Publication number
- CN110144135A CN110144135A CN201910429147.5A CN201910429147A CN110144135A CN 110144135 A CN110144135 A CN 110144135A CN 201910429147 A CN201910429147 A CN 201910429147A CN 110144135 A CN110144135 A CN 110144135A
- Authority
- CN
- China
- Prior art keywords
- powder
- super
- amphiphobic coating
- nano
- micro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
-
- 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
- C08K2201/011—Nanostructured additives
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention provides a kind of super-amphiphobic coating material and preparation method thereof and super-amphiphobic coating, the preparation method includes: preparation inorganic oxide powder, the inorganic oxide powder includes micro-powder and nano-powder, and the mass percent that the micro-powder accounts for total weight is 15%-50%；Step 2, it carries out hydrophobic processing respectively to the micro-powder and nano-powder and hates oil processing；Step 3, by after the hydrophobic handles and hates oil processing the micro-powder and nano-powder be dispersed in Organic Alcohol, obtain the super-amphiphobic coating material.Preparation method according to an embodiment of the present invention carries out grain composition by using nano-powder and micro-powder, can be effectively formed micro-nano structure when preparing super-amphiphobic coating；By carrying out hydrophobic processing to inorganic oxide powder and hating oil processing surface modification twice, very outstanding super-hydrophobic superoleophobic effect is obtained, super-amphiphobic coating material performance prepared by this process program is stablized, and the service life is long.
Description
Technical field
The invention belongs to material science and Surface Science field, have not only water repellent (hydrophobic) in particular to one kind but also refuse
Oily (oleophobic), i.e. super-amphiphobic coating material and preparation method thereof and super-amphiphobic coating.
Background technique
Conventional material can be divided into polar material, non-polar material according to its surface characteristic, not consider the microcosmic table of material
Under the premise of the pattern of face, usual polar material surface is easy hydrophilic, and non-polar material surface is easy oleophylic.
How to make material surface neither hydrophilic, also not oleophylic, not only made material super-hydrophobic but also superoleophobic material it is super double
Coating material is dredged, is difficult point in the industry, this is necessary not only for consideration material surface polar character itself, it is also necessary to consider that material is micro-
See structure.
In addition, the usual interface of super-hydrophobic this kind material is all a kind of micro-nano labyrinth of organic film, due to complexity
Microstructure to cause it to prepare difficulty big, in addition in durability, all showed in terms of ageing resistance poor.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of simple easily system, raw materials to be easy to get, is suitble to large-scale industry raw
The preparation method of the super-amphiphobic coating material of production.
Another object of the present invention is to a kind of super-amphiphobic coating materials that above-mentioned preparation method is prepared, and are used to prepare
Super-amphiphobic coating.
Yet another object of the invention is that providing a kind of water angle of wetting and oily angle of wetting is up to 150 ° or more super double
Open coat.
In order to solve the above technical problems, the invention adopts the following technical scheme:
The preparation method of the super-amphiphobic coating material of embodiment according to a first aspect of the present invention, includes the following steps:
Step 1, prepare inorganic oxide powder, the inorganic oxide powder includes micro-powder and nano-powder, institute
State micro-powder be micron aluminum oxide, micron silica, or mixtures thereof, the nano-powder be nanometer three oxidation two
Aluminium, nano silica, or mixtures thereof, the micro-powder account for total weight mass percent be 15%-50%；
Step 2, it carries out hydrophobic processing respectively to the micro-powder and nano-powder and hates oil processing；
Step 3, by after the hydrophobic handles and hates oil processing the micro-powder and nano-powder be dispersed in
In machine alcohol, the super-amphiphobic coating material is obtained.
According to some embodiments of the present invention, the partial size of the micro-powder is 100-200 μm, the grain of the nano-powder
Diameter is 20~50nm.
From control cost standpoint, it is preferable that the micro-powder is micron aluminum oxide, and the nano-powder is
Nano silica.
According to some embodiments of the present invention, the micro-powder and nano-powder are hated through Hydrophobing agent respectively
Water process and oil-treatment agent is hated to carry out hating oil processing.Herein, it is to be understood that carried out after both can first carrying out hydrophobic processing
Hydrophobic processing may be reversed progress hydrophobic processing after first carrying out hating oil processing；In addition, can be by micro-powder and nanometer
Powder respectively carries out hydrophobic processing respectively and/or hates oil processing, can also hate simultaneously to micro-powder and nano-powder
Water process and/or oil processing is hated (that is, using micro-powder and nano-powder as mixed powder, to be completed at the same time two kinds
Oil processing is hated in the hydrophobic processing of powder).Preferably, it carries out hating oil processing after first carrying out hydrophobic processing, it is highly preferred that right simultaneously
Micro-powder and nano-powder first carry out hydrophobic processing, then carry out hating oil processing.
Wherein, the Hydrophobing agent includes at least one of polysiloxanes, silicon fluoride, described to hate oil-treatment agent including complete
More than one of fluorine octanoic acid and its derivative.
Further, the polysiloxanes include polymethyl hydrogen siloxane, dimethyl silicone polymer more than one；It is described
Silicon fluoride is ten difluoro heptyl oxypropyl trimethyl oxysilane, tridecafluoro-n-octyltriethoxysilane, 17 fluorine decyl, three ethoxy
One or more of base silane, 3- (seven fluorine isopropoxies) propyl-triethoxysilicane.
Further, the hydrophobic processing specifically includes: dissolving in dehydrated alcohol acetone in the ratio of 5:95, mixes
Afterwards, the Hydrophobing agent is added, the Hydrophobing agent is 3~8wt% relative to the inorganic oxide powder content, then
PH=5 is adjusted with glacial acetic acid, the inorganic oxide powder is added, is stirred 8-15 hours, is hereafter heated to reflux and is separated,
It is finally dried, obtains the inorganic oxide powder handled through hydrophobic.
Further, described that oil processing is hated to specifically include: it is 0.5-1g/L that concentration, which is added, in the inorganic oxide powder
Amine Solutions in, stir evenly, the 0.5-1mol/L that then addition accounts for total volume 15%~20% hates the oil-treatment agent molten
Liquid, and it is described hate oil-treatment agent solution relative to the inorganic oxide powder content be 15-30wt%, ultrasonic disperse 0.5-
1.5 hours, hereafter continues stirring 2 hours, be then heated to reflux and separated, is finally dried, obtained through hating oil
The inorganic oxide powder of processing.
According to some embodiments of the present invention, in the step 1, the nano-powder is nano silica powder,
Preparation process is as follows:
Prepare ethanol water；
Catalyst is added in the ethanol water, the catalyst is ammonium hydroxide, obtains pre-mixing liquor；
It is warming up to 20-70 DEG C while stirring the pre-mixing liquor, ethyl orthosilicate is added wherein；
It keeps the temperature and continues stirring 3-6 hours, silica colloidal；
The silica colloidal is separated by solid-liquid separation, and 2-8 hours dry in 120~150 DEG C of baking ovens, obtains institute
State nano silica powder.
Further, the concentration of the relatively described pre-mixing liquor of the ethyl orthosilicate is 0.1~0.4mol/L, and the ammonium hydroxide exists
Concentration in the pre-mixing liquor is 0.2~1.2mol/L.
The super-amphiphobic coating material of embodiment according to a second aspect of the present invention, according to system described in any of the above-described embodiment
Preparation Method is prepared.
The super-amphiphobic material of embodiment according to a third aspect of the present invention, the super-amphiphobic material include: material body and
The super-amphiphobic coating on the material body surface layer is set, and the super-amphiphobic coating is coated by super-amphiphobic described in any of the above embodiments
Material is formed, and the water angle of wetting of the super-amphiphobic material and oily angle of wetting are respectively 150 ° or more.
Preferably, adhesive layer is also formed between the material body and the super-amphiphobic coating.
Above-mentioned technical proposal of the invention one of at least has the advantages that:
The preparation method of super-amphiphobic coating material according to an embodiment of the present invention, by using nano-powder and micro-powder
Grain composition is carried out, micro-nano structure can be effectively formed when preparing super-amphiphobic coating；
By carrying out hydrophobic processing to inorganic oxide powder and hating oil processing surface modification twice, obtain very outstanding
Super-hydrophobic superoleophobic effect, super-amphiphobic coating material performance prepared by this process program are stablized, and the service life is long；
Super-amphiphobic coating material according to an embodiment of the present invention, selectivity are even dripped using spraying, spraying, coating, spin coating
It applies or techniques, simple process, the equipment costs such as brushing is low；
In addition, in order to improve the durability of super-amphiphobic coating and ageing resistance, before spraying or coating, first in material sheet
Binder is precoated on body, then rapid spraying super-amphiphobic dispersing liquid, after baking-curing, it is preferably double thin can to obtain durability
Material, and this method is simple and reliable, and has good adaptability.
Detailed description of the invention
Fig. 1 is the flow chart of the super-amphiphobic coating material preparation method of the embodiment of the present invention.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill
Personnel's every other embodiment obtained, shall fall within the protection scope of the present invention.
The preparation method of super-amphiphobic coating material according to an embodiment of the present invention is specifically described in conjunction with attached drawing first below
Flow chart.
As shown in Figure 1, the preparation method of super-amphiphobic coating material according to an embodiment of the present invention includes the following steps:
Step 1, prepare inorganic oxide powder, the inorganic oxide powder includes micro-powder and nano-powder, institute
State micro-powder be micron aluminum oxide, micron silica, or mixtures thereof, the nano-powder be nanometer three oxidation two
Aluminium, nano silica, or mixtures thereof, the micro-powder account for total weight mass percent be 15%-50%.
Wherein, consider that it is preferable to use commercially available micro- for micro-powder from cost, easness of starting with, chemical stability etc.
Rice aluminum oxide powder, it is further preferred that the nano-powder is preferably nano silica.
As nano silica, it both can be commercially available product, can also voluntarily prepare by the following method:
Prepare ethanol water；Catalyst is added in the ethanol water, the catalyst is ammonium hydroxide, is obtained prewired
Liquid；It is warming up to 20-70 DEG C while stirring the pre-mixing liquor, ethyl orthosilicate is added wherein；Keep the temperature and continue stir 3-6 it is small
When, silica colloidal；The silica colloidal is separated by solid-liquid separation, and dry 2-8 is small in 120~150 DEG C of baking ovens
When, obtain the nano silica powder.The nano silica prepared by this method, size tunable, and particle diameter distribution
Narrow range, at low cost, simple process.
Preferably, the concentration of the relatively described pre-mixing liquor of the ethyl orthosilicate is 0.1~0.4mol/L, and the ammonium hydroxide is in institute
Stating the concentration in pre-mixing liquor is 0.2~1.2mol/L.
It is further preferred that the particle size range of micro-powder is 100-200 μm, the particle size range of the nano-powder is
20~50nm.By the way that micro-powder and nano-powder are carried out gradation, can be effectively formed when preparing super-amphiphobic coating micro-
Micro-nano structure, to contribute to form stable super-amphiphobic structure.
Step 2, it carries out hydrophobic processing respectively to the micro-powder and nano-powder and hates oil processing.
For example, the micro-powder and nano-powder can be carried out hydrophobic processing through Hydrophobing agent respectively and hated
Oil-treatment agent carries out hating oil processing.
Herein, it is to be understood that carry out hating oil processing after both can first carrying out hydrophobic processing, may be reversed and first carry out
Hydrophobic processing is carried out after hating oil processing；In addition, hydrophobic processing respectively can be carried out respectively for micro-powder and nano-powder
And/or hates oil processing, hydrophobic processing can also be carried out to micro-powder and nano-powder simultaneously and/or hate oil processing (also
It is to say, using micro-powder and nano-powder as mixed powder, is completed at the same time the hydrophobic processing of two kinds of powders, hates oil processing).
Preferably, it carries out hating oil processing after first carrying out hydrophobic processing, it is highly preferred that simultaneously first carrying out micro-powder and nano-powder
Hydrophobic processing then carries out hating oil processing.
Wherein, the Hydrophobing agent includes at least one of polysiloxanes, silicon fluoride.
Further, the polysiloxanes include polymethyl hydrogen siloxane, dimethyl silicone polymer more than one.It is described
Silicon fluoride is ten difluoro heptyl oxypropyl trimethyl oxysilane, tridecafluoro-n-octyltriethoxysilane, 17 fluorine decyl, three ethoxy
One or more of base silane, 3- (seven fluorine isopropoxies) propyl-triethoxysilicane.
The hydrophobic processing can specifically include: dissolving in dehydrated alcohol acetone in the ratio of 5:95, after mixing, be added
The Hydrophobing agent, the Hydrophobing agent are 3~8wt% relative to the inorganic oxide powder content, then with ice vinegar
The inorganic oxide powder is added in acid for adjusting pH=5, stirs 8-15 hours, is hereafter heated to reflux and is separated, most laggard
Row drying obtains the inorganic oxide powder handled through hydrophobic.Hydrophobic is handled under mildly acidic conditions, on the one hand, is conducive to make
The abundant spread apart of Hydrophobing agent is obtained, forms growth chain, on the other hand, the Hydrophobing agent for being conducive to the long chain is attached to
Micro-powder and nano powder surface, to be conducive to improve durability while improving super-hydrophobicity.
In addition, described, to hate oil-treatment agent include more than one of perfluoro caprylic acid and its derivative.It can specifically include perfluor
Octanoic acid, Sodium perfluorooctanoate, Perfluorooctanoic acid potassium salt and its mixture etc..
Further, described that oil processing is hated to specifically include: it is 0.5-1g/L that concentration, which is added, in the inorganic oxide powder
Amine Solutions in, stir evenly, the 0.5-1mol/L that then addition accounts for total volume 15%~20% hates the oil-treatment agent molten
Liquid, and it is described hate oil-treatment agent solution relative to the inorganic oxide powder content be 15-30wt%, ultrasonic disperse 0.5-
1.5 hours, hereafter continues stirring 2 hours, be then heated to reflux and separated, is finally dried, obtained through hating oil
The inorganic oxide powder of processing.
More specifically, it is equipped with organic amine aqueous solution and hates oil-treatment agent solution.(preferably by inorganic oxide powder first
For the inorganic oxide powder by hydrophobic processing) it is dispersed in Amine Solutions, then wherein oil-treatment agent solution is hated in addition,
Further progress is dispersed, is heated to reflux, is dried, and obtains through hating the inorganic oxide powder of oil processing.When carrying out hating oil processing,
By being dispersed in powder in advance in weakly alkaline Amine Solutions, the dispersibility of powder is helped to improve, while can
So that can preferably be combined between powder surface and oleophobic agent.
It as Amine Solutions, such as can be the aqueous solution of polydimethyldiallyl ammonium chloride, specifically, can incite somebody to action
Polydimethyldiallyl ammonium chloride is substantially dissolved in deionized water, the poly dimethyl two that preparation concentration is 0.6~1.2g/L
Acrylic ammonium chloride solution seals spare.
As oil-treatment agent solution is hated, specifically, such as Sodium perfluorooctanoate is substantially dissolved in deionized water prepare it is dense
Degree is the perfluoro caprylic acid sodium solution of 0.06~0.12mol/L, is sealed spare.
Wherein it is preferred to which described hate oil-treatment agent solution to account for the 15%~20% of total volume number.
By carrying out hydrophobic processing to inorganic oxide powder and hating oil processing surface modification twice, can obtain very excellent
Elegant super-hydrophobic superoleophobic effect, super-amphiphobic coating material performance prepared by this process program are stablized, and the service life is long.
Step 3, by after the hydrophobic handles and hates oil processing the micro-powder and nano-powder be dispersed in
In machine alcohol, the super-amphiphobic coating material is obtained.
Finally, will be handled by hydrophobic and the inorganic oxide powder of oil processing is hated to be dispersed in Organic Alcohol, such as methanol,
In ethyl alcohol, super-amphiphobic coating material can be obtained.
The super double coating materials being prepared can be applied, dipping, spin coating by spraying, and the various methods such as spraying are in glass
The surfaces such as glass, metal prepare super-amphiphobic coating.The water droplet contact angle of obtained super-amphiphobic coating is greater than 165 °, oil droplet angle of wetting
Greater than 155 °, 150 ° are all larger than, i.e., not only there is super-hydrophobic effect, but also there is superoleophobic effect, before there is very extensive application
Scape.
In addition, in order to improve the durability of super-amphiphobic coating and ageing resistance, before spraying or coating, first in material sheet
Binder is precoated on body, then rapid spraying super-amphiphobic dispersing liquid, after baking-curing, it is preferably double thin can to obtain durability
Material, and this method is simple and reliable, and has good adaptability.
In the following, the present invention is described in further detail by specific embodiment.
Embodiment 1
Firstly, preparing nano silica powder: in beaker, adding dehydrated alcohol by the concentration of 600mL/L, press
15mol/L adds deionized water, then adds ammonium hydroxide by the concentration of 0.8mol/L, stirs evenly and is warming up to 40 DEG C, presses
0.25mol/L concentration is slowly added to ethyl orthosilicate, finally uses deionized water constant volume.Hereafter, it keeps the temperature and to continue stirring 5 small
When, obtain milky silica colloidal.Then by being centrifugated (centrifuge speed 10000rpm).Then, it will separate
Obtained solid sediment is added dehydrated alcohol and is cleaned by ultrasonic, is centrifugated, operates repeatedly three times, finally dry at 125 DEG C
Dry 4 hours, obtain nanometer grade silica.It is measured by laser particle analyzer, confirms that its partial size is 20~30nm.
Secondly, weighing the nanometer grade silica of 0.5g and the micron order aluminum oxide (aluminum oxide of 0.5g respectively
Using commercially available product, partial size 200nm).
Then, hydrophobic processing is carried out to silicon-dioxide powdery and aluminum oxide powder respectively: in the ratio of 5:95 by third
Ketone dissolves in dehydrated alcohol, and after mixing, ten difluoro heptyl oxypropyl trimethyl oxysilane are added, and (mass number is silicon-dioxide powdery
With the 5.5% of aluminum oxide powder total mass number), then pH=5 is adjusted with glacial acetic acid, it is separately added into above two powder, is stirred
It mixes 10 hours, is heated to reflux separation, be spare after lower drying 120.
Then, it carries out hating oil processing: the poly dimethyl for being 0.8g/L by hydrophobic treated above-mentioned powder is added to concentration
It in dipropenyl ammonium chloride solution, stirs evenly, then adds the perfluoro caprylic acid sodium solution of the 0.8mol/L of 20% volume fraction,
The perfluoro caprylic acid sodium solution is 20wt% relative to the content of above-mentioned powder.It ultrasonic disperse 60 minutes, is stirred for 2 hours.Reaction
After, it is heated to reflux, separates, is dried in vacuo, it is spare.
Finally, the powder for being hated oil processing after drying is distributed in dehydrated alcohol, super-amphiphobic coating material is acquired.
By obtained super-amphiphobic coating material by the method for spraying, sprays to and be clean glass baseplate surface, it is dry
Afterwards, super-amphiphobic coating is formed in glass baseplate surface.
Detection angle of wetting is gone with water and peanut oil respectively, it is 165 ° that discovery water droplet wetting, which is named, and oil droplet angle of wetting is 155 °.Really
Obtained material interface is recognized with good super-amphiphobic characteristic.
Embodiment 2
Firstly, preparing nano silica powder: in beaker, adding dehydrated alcohol by the concentration of 500mL/L, press
20mol/L adds deionized water, then adds ammonium hydroxide by the concentration of 1mol/L, stirs evenly and be warming up to 50 DEG C, by 0.3mol/
L concentration is slowly added to ethyl orthosilicate, finally uses deionized water constant volume.Hereafter, stirring 4 hours are kept the temperature and continued, cream is obtained
White silica colloidal.Then by being centrifugated (centrifuge speed 8000rpm).Then, by isolated solid
Sediment is added dehydrated alcohol and is cleaned by ultrasonic, is centrifugated, operates repeatedly three times, finally 6 hours dry at 110 DEG C, obtains
To nanometer grade silica.It is measured by laser particle analyzer, confirms that its partial size is 30~50nm.
Secondly, weighing the nanometer grade silica of 1.5g and the micron order aluminum oxide (aluminum oxide of 0.5g respectively
Using commercially available product, partial size 200nm).
Then, hydrophobic processing is carried out to silicon-dioxide powdery and aluminum oxide powder respectively: in the ratio of 5:95 by third
Ketone dissolves in dehydrated alcohol, and after mixing, dimethyl silicone polymer is added, and (mass number is inorganic oxide powder mass number
4.5%), (mass number is silicon-dioxide powdery and the total matter of aluminum oxide powder to ten difluoro heptyl oxypropyl trimethyl oxysilane
Measure the 5.0% of number), then pH=5 is adjusted with glacial acetic acid, be separately added into above two powder, stir 12 hours, is heated to reflux point
From spare after dry at 100 DEG C.
Then, it carries out hating oil processing: the poly dimethyl for being 0.8g/L by hydrophobic treated above-mentioned powder is added to concentration
It in dipropenyl ammonium chloride solution, stirs evenly, then adds the perfluoro caprylic acid solution of the 0.8mol/L of 15% volume fraction, it should
Perfluoro caprylic acid sodium solution is 25wt% relative to the content of above-mentioned powder.It ultrasonic disperse 1.5 hours, is stirred for 2 hours.Reaction knot
Shu Hou is heated to reflux, separates, is dried in vacuo, spare.
Finally, the powder for being hated oil processing after drying is distributed in dehydrated alcohol, super-amphiphobic coating material is acquired.
By obtained super-amphiphobic coating material by the method for spraying, sprays to and be clean metallic substrate surfaces, it is dry
Afterwards, super-amphiphobic coating is formed in metallic substrate surfaces.Wherein, before spraying the super-amphiphobic coating material, in the metal substrate
Surface sprays one layer of organic siliconresin as binder, sprays super-amphiphobic coating material immediately after.
Detection angle of wetting is gone with water and peanut oil respectively, it is 158 ° that discovery water droplet wetting, which is named, and oil droplet angle of wetting is 162 °.Really
Obtained material interface is recognized with good super-amphiphobic characteristic.
In addition, obtained super-amphiphobic coating shells non-glass with hand, intensity is significantly increased.
Preparing sample using above-mentioned process program is only sample, can be amplified according to a certain percentage, as extensive
Industrial production uses, it can be widely applied to the field of various self-cleaning glass applications.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of super-amphiphobic coating material, which comprises the steps of:
Step 1, prepare inorganic oxide powder, the inorganic oxide powder includes micro-powder and nano-powder, described micro-
The mass percent that rice flour body accounts for total weight is 15%-50%；
Step 2, it carries out hydrophobic processing respectively to the micro-powder and nano-powder and hates oil processing；
Step 3, by after the hydrophobic handles and hates oil processing the micro-powder and nano-powder be dispersed in Organic Alcohol
In, obtain the super-amphiphobic coating material.
2. the preparation method of super-amphiphobic coating material according to claim 1, which is characterized in that the grain of the micro-powder
Diameter is 100-200 μm, and the partial size of the nano-powder is 20~50nm.
3. super-amphiphobic coating material preparation method according to claim 1, in the step 2, the micro-powder and
Nano-powder carries out hydrophobic processing through Hydrophobing agent respectively and oil-treatment agent is hated to carry out hating oil processing, the Hydrophobing agent
At least one including polysiloxanes, silicon fluoride, described to hate oil-treatment agent include more than one of perfluoro caprylic acid and its derivative.
4. super-amphiphobic coating material preparation method according to claim 3, which is characterized in that the polysiloxanes includes poly-
Methyl hydrogen siloxane, dimethyl silicone polymer more than one；The silicon fluoride is ten difluoro heptyl oxypropyl trimethyl oxygroup silicon
Alkane, tridecafluoro-n-octyltriethoxysilane, heptadecafluorodecyl triethoxysilane, 3- (seven fluorine isopropoxies) propyl triethoxy
One or more of silane.
5. the preparation method of super-amphiphobic coating material according to claim 3, which is characterized in that the hydrophobic processing is specific
Include: to dissolve in acetone in dehydrated alcohol in the ratio of 5:95, after mixing, the Hydrophobing agent, the hydrophobic processing is added
Agent is 3~8wt% relative to the inorganic oxide powder content, then adjusts pH=5 with glacial acetic acid, and the inorganic oxide is added
Powder stirs 8-15 hours, is hereafter heated to reflux and is separated, is finally dried, and obtains handling through hydrophobic inorganic
Oxide powder.
6. the preparation method of super-amphiphobic coating material according to claim 3, which is characterized in that described to hate oil processing specific
Include:
The inorganic oxide powder is added in the Amine Solutions that concentration is 0.5-1g/L, is stirred evenly, then addition accounts for
The 0.5-1mol/L's of total volume 15%~20% hates oil-treatment agent solution, wherein described to hate oil-treatment agent solution relative to institute
State inorganic oxide powder content be 15-30wt%, ultrasonic disperse 0.5-1.5 hour, hereafter continue stir 2 hours, then into
Row is heated to reflux and is separated, and is finally dried, obtains through hating the inorganic oxide powder of oil processing.
7. the preparation method of super-amphiphobic coating material according to claim 1, which is characterized in that described in the step 1
Nano-powder is nano silica powder, and preparation process is as follows:
Prepare ethanol water；
Catalyst is added in the ethanol water, the catalyst is ammonium hydroxide, obtains pre-mixing liquor；
It is warming up to 20-70 DEG C while stirring the pre-mixing liquor, ethyl orthosilicate is added wherein；
It keeps the temperature and continues stirring 3-6 hours, silica colloidal；
The silica colloidal is separated by solid-liquid separation, and 2-8 hours dry in 120~150 DEG C of baking ovens, obtains described receive
Rice silicon-dioxide powdery.
8. the preparation method of super-amphiphobic coating material according to claim 7, which is characterized in that the ethyl orthosilicate phase
Concentration to the pre-mixing liquor is 0.1~0.4mol/L, and concentration of the ammonium hydroxide in the pre-mixing liquor is 0.2~1.2mol/
L。
9. a kind of super-amphiphobic coating material, which is characterized in that be prepared by the described in any item preparation methods of claim 1 to 8
It arrives.
10. a kind of super-amphiphobic material, which is characterized in that the super-amphiphobic material includes: material body and is arranged in the material
Expect that the super-amphiphobic coating of this surface layer, the super-amphiphobic coating are coated by super-amphiphobic according to any one of claims 1 to 9
Material is formed, and the water angle of wetting of the super-amphiphobic material and oily angle of wetting are respectively 150 ° or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910429147.5A CN110144135A (en) | 2019-05-22 | 2019-05-22 | A kind of super-amphiphobic coating material and preparation method thereof and super-amphiphobic coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910429147.5A CN110144135A (en) | 2019-05-22 | 2019-05-22 | A kind of super-amphiphobic coating material and preparation method thereof and super-amphiphobic coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110144135A true CN110144135A (en) | 2019-08-20 |
Family
ID=67592645
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910429147.5A Pending CN110144135A (en) | 2019-05-22 | 2019-05-22 | A kind of super-amphiphobic coating material and preparation method thereof and super-amphiphobic coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110144135A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2723518C2 (en) * | 2018-08-27 | 2020-06-11 | Федеральное государственное бюджетное учреждение науки Пермского федерального исследовательского центра Уральского отделения Российской академии наук (ПФИЦ УрО РАН) | Rheological additive for fire-extinguishing powder formulations |
| CN111908480A (en) * | 2020-02-25 | 2020-11-10 | 成都普界科技有限公司 | Super-amphiphobic material, preparation method thereof and preparation method of super-amphiphobic surface coating |
| CN116117943A (en) * | 2023-01-16 | 2023-05-16 | 点金新型材料研究院(厦门)有限公司 | Anti-fingerprint skin-feel matte melamine veneer and manufacturing method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315871A (en) * | 2015-11-25 | 2016-02-10 | 华南理工大学 | Device and method for producing super-amphiphobic paint with modification of modified particles |
| CN106893454A (en) * | 2017-04-21 | 2017-06-27 | 黑龙江凯恩琪新材料科技有限公司 | A kind of preparation method of sprayable and durable super-amphiphobic coating |
| CN107022291A (en) * | 2017-04-21 | 2017-08-08 | 黑龙江凯恩琪新材料科技有限公司 | A kind of preparation method of the super-amphiphobic coating of sprayable and lasting freezing |
-
2019
- 2019-05-22 CN CN201910429147.5A patent/CN110144135A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315871A (en) * | 2015-11-25 | 2016-02-10 | 华南理工大学 | Device and method for producing super-amphiphobic paint with modification of modified particles |
| CN106893454A (en) * | 2017-04-21 | 2017-06-27 | 黑龙江凯恩琪新材料科技有限公司 | A kind of preparation method of sprayable and durable super-amphiphobic coating |
| CN107022291A (en) * | 2017-04-21 | 2017-08-08 | 黑龙江凯恩琪新材料科技有限公司 | A kind of preparation method of the super-amphiphobic coating of sprayable and lasting freezing |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2723518C2 (en) * | 2018-08-27 | 2020-06-11 | Федеральное государственное бюджетное учреждение науки Пермского федерального исследовательского центра Уральского отделения Российской академии наук (ПФИЦ УрО РАН) | Rheological additive for fire-extinguishing powder formulations |
| CN111908480A (en) * | 2020-02-25 | 2020-11-10 | 成都普界科技有限公司 | Super-amphiphobic material, preparation method thereof and preparation method of super-amphiphobic surface coating |
| CN116117943A (en) * | 2023-01-16 | 2023-05-16 | 点金新型材料研究院(厦门)有限公司 | Anti-fingerprint skin-feel matte melamine veneer and manufacturing method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104987520B (en) | A kind of super-hydrophobic nano clear coat and preparation method thereof | |
| CN110144135A (en) | A kind of super-amphiphobic coating material and preparation method thereof and super-amphiphobic coating | |
| JP4335446B2 (en) | Titanium oxide sol, thin film and method for producing them | |
| CN104910656B (en) | A kind of method that super-hydrophobic silica powder and super-hydrophobic coat are prepared with compound silicon source | |
| CN101955697A (en) | Ceramic non-stick coating with bacteriostasis action and coating method thereof | |
| CN111068997B (en) | Preparation method of coating for realizing super-hydrophobic property of condensing heat exchange tube and condensing heat exchange tube | |
| CN111534162B (en) | Montmorillonite-based photocatalytic super-hydrophobic coating and preparation method thereof | |
| CN101549959B (en) | A method of nano self-cleaning glass production in the float glass production line | |
| CN101982560B (en) | Low-cost superhydrophobic surface treatment method of aluminum alloy | |
| CN1701105A (en) | Photocatalyst coating liquid, photocatalyst film and photocatalyst member | |
| CN111908480A (en) | Super-amphiphobic material, preparation method thereof and preparation method of super-amphiphobic surface coating | |
| CN102849962A (en) | Preparation method of SiO2 super-hydrophobic film and super-hydrophobic material | |
| CN101914314A (en) | Heat-insulating powder for coating and preparation method thereof | |
| CN109487245A (en) | A kind of preparation method of super-hydrophobic aqua oxidation aluminium film | |
| CN108774447A (en) | A kind of carbon-silver microballoon/epoxy resin super-hydrophobic coat preparation method | |
| CN107983327A (en) | A kind of method for improving ZnO nano-rod array photocatalysis performance | |
| CN106319601A (en) | Preparing method for super-hydrophobic type porous metal coating | |
| CN106629793B (en) | A kind of hollow rodlike MgF2The preparation method of particle and its application in automatically cleaning antireflective film | |
| CN103508681B (en) | Preparation method of super-hydrophilic anti-reflection coating and super-hydrophilic anti-reflection coating | |
| CN104497647A (en) | Preparation method of self-cleaning anticorrosion sol for metal substrate | |
| CN102732071A (en) | Preparation method for self-cleaning nanometer composite sol for metal aluminum plate corrosion resistance | |
| CN115011195A (en) | Water-based heat-insulation reflective composite coating with low heat conductivity coefficient and preparation process thereof | |
| CN106830076B (en) | A kind of preparation method of glass nanometer heat reflection composite functional material | |
| CN111020591B (en) | Preparation method of aluminum alloy with polished hydrophobic surface | |
| CN113004728A (en) | Coating with hydrophilic self-cleaning capability and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190820 |
|
| WD01 | Invention patent application deemed withdrawn after publication |