CN110170252A - A kind of method that sprayed deposit prepares super-hydrophobic film - Google Patents
A kind of method that sprayed deposit prepares super-hydrophobic film Download PDFInfo
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- CN110170252A CN110170252A CN201910444586.3A CN201910444586A CN110170252A CN 110170252 A CN110170252 A CN 110170252A CN 201910444586 A CN201910444586 A CN 201910444586A CN 110170252 A CN110170252 A CN 110170252A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/04—Hydrophobization
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/38—Hydrophobic membranes
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Abstract
The present invention is a kind of method that sprayed deposit prepares super-hydrophobic film, its main feature is that, comprising the following three steps: fluorinated modified nano silica preparation, the preparation of fluorinated modified nano silica mixed solution and super-hydrophobic film preparation, by mass parts, 28 parts of cyclohexane solvent, 1 part of silicon fluoride low-surface-energy reagent, 0.5-2.5 parts of nano silica proportions, obtain fluorinated modified nano silica；Fluorinated modified nano silica is melted into anhydrous ethanol solvent, at room temperature, stirs to get uniform fluorinated modified nano silica mixed solution；Using spray deposition, uniform mixed solution is made and is deposited on PVDF basement membrane, skin drying after the completion of deposition forms super-hydrophobic layer in PVDF membrane surface；The nano coating of spraying, almost without damage, makes film keep hydrophobicity, maintains stable effluent quality and permeation flux, the nano coating anti-fouling performance of spraying is excellent, long service life to basement membrane.
Description
Technical field
The present invention relates to super-hydrophobic film method field is prepared, the side of super-hydrophobic film is prepared more particularly to a kind of sprayed deposit
Method.
Background technique
Lotus leaf surface has the function of super-hydrophobic automatic cleaning, and the microstructure and low surface free energy of super hydrophobic surface are super thin
Two key factors of water surface simulate the microcosmic or nano-scale structures of super-hydrophobic biological surface, by film when preparing membrane distillation
Material surface is processed into super-hydrophobicity, then can reduce fouling membrane caused by feed liquid solute, during long-play, makes film
Hydrophobicity is kept, stable effluent quality and permeation flux are maintained.
Currently, the method for building super hydrophobic surface has very much, such as sol-gel method, template, plasma treatment, receive
Rice corpuscles deposition, using silicon fluoride coating and multicomponent mixture, mutually separation prepares super hydrophobic surface, these routes can pass through
The surface free energy or surfacing roughening of rough surface are reduced, it can also the two combination generation super hydrophobic surface.
Material surface tension is determined by the chemical component on surface, and the geometry on surface determines how these power act on
In liquid, therefore, surface wettability can be adjusted by changing one of the two parameters.By low-surface-energy material, especially
It is the functionalization of silicon fluoride to reduce surface free energy, is to generate the most common method of super hydrophobic surface, in addition, also attempting to generate
Nanostructured surface pattern with multistage surface roughness, it is some nano combined to adjust surface wettability to extreme value
Material can be used to rough surface, such as nano-titanium dioxide, nano silica etc..Currently, due to Nano particles of silicon dioxide
Good performance and compatibility are shown in the preparation of nano composite membrane, it is super thin to combine preparation to silica and silicon fluoride
There are many research of water surface, but it is more complicated to face preparation process, higher cost, it is difficult to the problem of being mass produced.
Summary of the invention
In view of the problems of the existing technology, creativeness proposes the method that sprayed deposit prepares super-hydrophobic film to the present invention,
One layer of nanoscale super hydrophobic surface is formed on Kynoar (PVDF) basement membrane, and super-hydrophobic nano composite membrane is prepared,
For the nano coating of spraying to basement membrane almost without damage, anti-fouling performance is good.
The technical solution adopted by the present invention is that: a kind of method that sprayed deposit prepares super-hydrophobic film, characterized in that it includes
Following steps:
(1) fluorinated modified nano silica preparation:
By mass parts, 28 parts of cyclohexane solvent, 1 part of silicon fluoride low-surface-energy reagent, 0.5-2.5 parts of nano silica match
Than, 0.5-2.5 parts of nano silicas and 28 parts of hexamethylenes are placed in container, container is placed in supersonic cleaning machine, ultrasound
After shaking 20min, uniform nano silicon dioxide dispersion is formed, the container equipped with nano silicon dioxide dispersion is set in magnetic
It is stirred on power blender, then is added dropwise to 1 part of silicon fluoride low-surface-energy reagent equipped with nano silicon dioxide dispersion
Container in, stir 4-8h, temperature control at 50 DEG C, obtain fluorinated modified nanosilica solution, be centrifuged through 2500r/min
Machine after being centrifuged 10min, removes supernatant liquor, obtains fluorinated modified nanometer titanium dioxide Silica hydrogel, at 80-120 DEG C, dries 3-
After 5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica mixed solution preparation:
By mass parts ratio, 1 part of fluorinated modified nano silica in step (1) is melted into 79 parts of anhydrous ethanol solvents
In, at room temperature, 2-4h is stirred, obtains uniform fluorinated modified nano silica mixed solution；
(3) prepared by super-hydrophobic film:
Uniform fluorinated modified nano silica mixed solution will be obtained in step (2), using spray deposition, spraying
Pressure is controlled in 0.2-0.6Mpa, spray distance 10-15cm, is deposited on Kynoar (PVDF) basement membrane, quiet after spraying
20-40min is set, at 60-100 DEG C, forced air drying 3-5h obtains super-hydrophobic film.
In step (1), by mass parts ratio, 1 part of silicon fluoride low-surface-energy reagent, 1 part of nano silica.
In step (1), the partial size of nano silica is 25-35nm.
The low surface energy fluorine silane reagent is 1H, 1H, 2H, and 2H-perfluoro capryl trichlorosilane (PFTS) group becomes
C8H4Cl3F13Si, density are 1.65g/ml or 1H, 1H, 2H, and 2H- perfluoro decyl trichlorosilane group becomes C10H4Cl3F17Si, density
For 1.71g/ml.
In step (1), the cyclohexane solvent density is 0.77g/ml.
In step (2), the anhydrous ethanol solvent density is 0.79g/ml.
A kind of sprayed deposit of the present invention prepares having the beneficial effect that for the method for super-hydrophobic film
1, it is super-hydrophobic to form one layer of nanoscale on PVDF basement membrane for a kind of method that sprayed deposit prepares super-hydrophobic film
Surface, coating surface static contact angle can be greater than 150 °, and surface roughness is larger while having good thermal stability, by 70
Ultrasonic cleaner is ultrasonically treated 180min at DEG C, and water contact still keeps 140 ° or so, and the nano coating of spraying is several to basement membrane
It does not damage, so that film is kept hydrophobicity, maintain stable effluent quality and permeation flux；
2, a kind of method that sprayed deposit prepares super-hydrophobic film, Processes and apparatus is simple, raw material is easy to get, is at low cost, is making
In standby coating procedure, it is only necessary to configure spray solution and be sprayed, not need to carry out the processing such as the modification in later period, be better than other
Processing mode, be suitble to large area spraying, the nano coating anti-fouling performance of spraying is excellent, long service life.
Detailed description of the invention
Fig. 1 is in a kind of method that sprayed deposit prepares super-hydrophobic film, under nano silica different quality portion rate
Static Contact Angle Measurements figure；
Fig. 2 is that a kind of sprayed deposit is prepared in the method for super-hydrophobic film, is that 1:1 chooses nano fluorine-silicon alkane by mass parts ratio
Fluorinated modified nano silica is made in low-surface-energy reagent and silica, and uniform mixed solution is made in stirring, in difference
Super-hydrophobic layer static contact angle result figure under spray pressure；
Fig. 3 is that a kind of sprayed deposit is prepared in the method for super-hydrophobic film, and it is low to be that 1:1 chooses nano fluorine-silicon alkane by mass parts ratio
Fluorinated modified nano silica is made by different mixings time in surface energy reagent and silica, and stirring is made uniformly
Mixed solution, the super-hydrophobic layer static contact angle result figure under 0.5Mpa spray pressure.
Specific embodiment
The present invention is described in further detail below in conjunction with the drawings and specific embodiments, specific implementation described herein
Example is not intended to limit the present invention only to explain the present invention.
In embodiment:
28 parts=60ml of cyclohexane solvent；1 part=1ml of silicon fluoride low-surface-energy reagent；0.5 part of nano silica=
0.825g；1 part=1.65g of nano silica；1.5 parts=2.475g of nano silica；2 parts of nano silica=
3.3g；2.5 parts=4.125g of nano silica；Fluorinated modified 1 part=0.3g of nano silica；79 parts of anhydrous ethanol solvent
=30ml.
In 1-embodiment of embodiment 5, received in a kind of method that sprayed deposit prepares super-hydrophobic film referring to attached drawing 1
Static Contact Angle Measurements under rice silica different quality portion rate.
A kind of embodiment 1: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 0.825g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in ultrasonic cleaning
In machine, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the appearance of nano silicon dioxide dispersion will be housed
Device is set to be stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to equipped with nano silica point
In the container of dispersion liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nano-silica
SiClx solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 2: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It places and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nanometer titanium dioxide
Silicon solution removes supernatant after being centrifuged 10min, obtains fluorinated modified nanometer titanium dioxide Silica hydrogel through 2500r/min centrifuge,
At 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 3: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 2.475g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in ultrasonic cleaning
In machine, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the appearance of nano silicon dioxide dispersion will be housed
Device is set to be stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to equipped with nano silica point
In the container of dispersion liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nano-silica
SiClx solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 4: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 3.3g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nanometer titanium dioxide
Silicon solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 5: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 4.125g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in ultrasonic cleaning
In machine, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the appearance of nano silicon dioxide dispersion will be housed
Device is set to be stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to equipped with nano silica point
In the container of dispersion liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nano-silica
SiClx solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
In 6-embodiment of embodiment 10, referring to attached drawing 3, a kind of sprayed deposit is prepared in the method for super-hydrophobic film, by matter
Amount part, which is compared, chooses nano fluorine-silicon alkane low-surface-energy reagent and silica for 1:1, and fluorination is made by different mixings time and changes
Property nano silica, stirring uniform mixed solution is made, the super-hydrophobic layer static contact angle under 0.5Mpa spray pressure
As a result.
A kind of embodiment 6: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 4h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nano silica
Solution removes supernatant after being centrifuged 10min, obtains fluorinated modified nanometer titanium dioxide Silica hydrogel through 2500r/min centrifuge,
At 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, dry super-hydrophobic film is obtained.
A kind of embodiment 7: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 5h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nano silica
Solution removes supernatant liquor after being centrifuged 10min, obtains fluorinated modified nanometer titanium dioxide Silica hydrogel through 2500r/min centrifuge,
At 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 8: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 6h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nano silica
Solution removes supernatant liquor after being centrifuged 10min, obtains fluorinated modified nanometer titanium dioxide Silica hydrogel through 2500r/min centrifuge,
At 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, dry super-hydrophobic film is obtained.
A kind of embodiment 9: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 7h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nano silica
Solution removes supernatant liquor after being centrifuged 10min, obtains fluorinated modified nanometer titanium dioxide Silica hydrogel through 2500r/min centrifuge,
At 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 10: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container equipped with nano silicon dioxide dispersion is set
It is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to equipped with nano silicon dioxide dispersion
Container in, stir 8h, at 50 DEG C, revolution is controlled in 300r/min for temperature control, and it is molten to obtain fluorinated modified nano silica
Liquid removes supernatant liquor after being centrifuged 10min, obtains fluorinated modified nanometer titanium dioxide Silica hydrogel through 2500r/min centrifuge,
At 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
In 11-embodiment of embodiment 15, referring to attached drawing 2, a kind of sprayed deposit is prepared in the method for super-hydrophobic film, is pressed
Mass parts ratio is that 1:1 chooses nano fluorine-silicon alkane low-surface-energy reagent and nano silica, and fluorinated modified nano-silica is made
Uniform mixed solution is made in SiClx, stirring, the super-hydrophobic layer static contact angle result under different spray pressures.
A kind of embodiment 11: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nanometer titanium dioxide
Silicon solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.2Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 12: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nanometer titanium dioxide
Silicon solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.3Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 13: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nanometer titanium dioxide
Silicon solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.4Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 14: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nanometer titanium dioxide
Silicon solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.5Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
A kind of embodiment 15: method that sprayed deposit prepares super-hydrophobic film, comprising the following steps:
(1) 1.65g nano silica and 60ml cyclohexane solvent are placed in container, container is placed in supersonic cleaning machine
In, ultrasonic vibration 20min forms uniform nano silicon dioxide dispersion, and the container of nano silicon dioxide dispersion will be housed
It sets and is stirred on magnetic stirring apparatus, then 1ml silicon fluoride low-surface-energy reagent is added to and is dispersed equipped with nano silica
In the container of liquid, 4-8h is stirred, at 50 DEG C, revolution is controlled in 300r/min for temperature control, obtains fluorinated modified nanometer titanium dioxide
Silicon solution removes supernatant liquor after being centrifuged 10min through 2500r/min centrifuge, and it is solidifying to obtain fluorinated modified nano silica
Glue, at 80-120 DEG C, after drying 3-5h, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica 0.3g is dissolved in 30ml anhydrous ethanol solvent, at room temperature, stirring
2-4h obtains uniform fluorinated modified nano silica mixed solution；
(3) uniform fluorinated modified nano silica mixed solution will be obtained, using spray deposition, spray pressure control
System is deposited on Kynoar (PVDF) basement membrane in 0.6Mpa, spray distance 10-15cm, 20-40min is stood after spraying,
In 60-100 DEG C of forced air drying 3-5h, super-hydrophobic film is obtained.
The above is only preferred embodiment of the invention, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the present invention, several improvements and modifications can also be made, these improvements and modifications should also regard
For protection scope of the present invention.
Claims (6)
1. a kind of method that sprayed deposit prepares super-hydrophobic film, characterized in that it the following steps are included:
(1) fluorinated modified nano silica preparation:
By mass parts, 28 parts of hexamethylene, 1 part of silicon fluoride low-surface-energy reagent, 0.5-2.5 parts of nano silica proportions will
0.5-2.5 parts of nano silicas and 28 parts of cyclohexane solvents are placed in container, and container is placed in supersonic cleaning machine, ultrasound shake
Dynamic 20min, forms uniform nano silicon dioxide dispersion, and the container equipped with nano silicon dioxide dispersion is set and is stirred in magnetic force
It mixes and is stirred on device, then by 1 part of silicon fluoride low-surface-energy reagent, be added dropwise to the appearance equipped with nano silicon dioxide dispersion
In device, 4-8h is stirred, temperature is controlled at 50 DEG C, fluorinated modified nanosilica solution is obtained, through 2500r/min centrifuge,
After being centrifuged 10min, supernatant liquor is removed, fluorinated modified nanometer titanium dioxide Silica hydrogel is obtained, at 80-120 DEG C, dries 3-5h
Afterwards, grinding obtains fluorinated modified nano silica；
(2) fluorinated modified nano silica mixed solution preparation:
By mass parts ratio, 1 part of fluorinated modified nano silica in step (1) is melted into 79 parts of anhydrous ethanol solvents,
Under room temperature, 2-4h is stirred, uniform fluorinated modified nano silica mixed solution is obtained；
(3) prepared by super-hydrophobic film:
Uniform fluorinated modified nano silica mixed solution will be obtained in step (2), using spray deposition, spray pressure
Control is deposited on Kynoar (PVDF) basement membrane in 0.2-0.6Mpa, spray distance 10-15cm, 20- is stood after spraying
40min, at 60-100 DEG C, forced air drying 3-5h obtains super-hydrophobic film.
2. the method that a kind of sprayed deposit according to claim 1 prepares super-hydrophobic film, characterized in that in step (1),
By mass parts ratio, 1 part of silicon fluoride low-surface-energy reagent, 1 part of nano silica.
3. the method that a kind of sprayed deposit according to claim 1 prepares super-hydrophobic film, characterized in that in step (1),
The partial size of nano silica is 25-35nm.
4. the method that a kind of sprayed deposit according to claim 1 prepares super-hydrophobic film, characterized in that the low surface
Energy silicon fluoride reagent is 1H, 1H, 2H, and 2H-perfluoro capryl trichlorosilane (PFTS) group becomes C8H4Cl3F13Si, density 1.65g/
Ml or 1H, 1H, 2H, 2H- perfluoro decyl trichlorosilane group become C10H4Cl3F17Si, density 1.71g/ml.
5. the method that a kind of sprayed deposit according to claim 1 prepares super-hydrophobic film, characterized in that the hexamethylene is molten
Agent density is 0.77g/ml.
6. the method that a kind of sprayed deposit according to claim 1 prepares super-hydrophobic film, characterized in that in step (2),
The anhydrous ethanol solvent density is 0.79g/ml.
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