CN109235037A - A kind of preparation method of nano-starch super-hydrophobic coat - Google Patents
A kind of preparation method of nano-starch super-hydrophobic coat Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
The invention discloses a kind of preparation methods of super-hydrophobic coat containing nano-starch, specifically includes the following steps: first using ultrasonication starch, prepare nano-starch dispersion liquid；Secondly, nano-starch dispersion liquid is surface-treated with double bond containing silane coupling agent；Again, surface treated nano-starch is polymerize with vinyl acetate emulsion, synthesizes hydrophobic lotions；Finally, on the substrate surface by lotion dip-coating, drying is obtained with ultra-hydrophobicity coating.The nano material that method of the invention uses is starch, low-surface energy substance is polyvinyl acetate, and material therefor is low in cost to be easy to get, and has good environmental-protecting performance, and there is good ultra-hydrophobicity using the coating of this method preparation, to the contact angle of water more than 151.6 °.
Description
Technical field
The invention belongs to super hydrophobic material preparation technical fields, are related to a kind of preparation side of nano-starch super-hydrophobic coat
Method.
Background technique
Super hydrophobic material is a kind of new material, because contact angle of its surface to water is greater than 150 °, so super hydrophobic surface
The performances such as waterproof, antifouling, automatically cleaning, freezing are relatively good, therefore super hydrophobic material has in industrial or agricultural field and daily life
There is good application prospect.The basic skills for preparing super hydrophobic surface is that nano material and low-surface energy substance act synergistically,
At present frequently with nano material such as titanium oxide, zinc oxide, silica etc., it is not only with high costs, and dirt can be caused to environment
Dye.In addition, the low-surface energy substance used now is mainly fluorine-containing or siliceous chemicals, price is higher, will also result in environment
Pollution.Therefore, these above-mentioned defects all limit the development and application of super hydrophobic surface.
Summary of the invention
The object of the present invention is to provide a kind of nano-starch super-hydrophobic coats, solve existing in the prior art super-hydrophobic
Coating production higher cost easily causes the problem of pollution.
The technical scheme adopted by the invention is that a kind of preparation method of super-hydrophobic coat containing nano-starch, specifically according to
Following steps are implemented:
Step 1, using ultrasonication starch, prepare nano-starch dispersion liquid；
Step 2 is surface-treated nano-starch dispersion liquid, prepares surface treated nano-starch；
Surface treated nano-starch polymerize, hydrophobic synthetic lotion by step 3 with vinyl acetate emulsion；
Step 4, by hydrophobic lotions dip-coating on the substrate surface, preparation have ultra-hydrophobicity coating.
The detailed process of step 1 are as follows: starch, which is added to the water stirring, keeps starch dispersion uniform, then carries out at 2-10 DEG C
Ultrasonication obtains nano-starch dispersion liquid.
The process that nano-starch dispersion liquid is surface-treated in step 2 are as follows: sequentially added into nano-starch dispersion liquid anhydrous
Ethyl alcohol and silane coupling agent containing double bond are centrifuged, wash, obtain surface treated after stirring 1-8h at 40-80 DEG C
Nano-starch.
The detailed process of hydrophobic synthetic lotion in step 3 are as follows: emulsifier and initiator are added to the water and stirred evenly, is connect
Sequentially add surface treated nano-starch and vinylacetate, after mixing in 40-60 DEG C of emulsion polymerisation 4-8h,
Obtain hydrophobic lotions.
The process of hydrophobic lotions dip-coating is carried out in step 4 to stromal surface are as follows: first by matrix distilled water ultrasonic cleaning
Drying after 1-4 times, the matrix after taking drying, immerses in hydrophobic lotions, after stirring 5-30min at room temperature, is put into baking oven in 20-80
DEG C drying, repeat immerse, drying 1-3 times after, obtain super-hydrophobic coat.
Ultrasonic treatment time is 4-8h in step 1, and the mass ratio of starch and water is 5-10:100.
The volume ratio of nano-starch dispersion liquid and dehydrated alcohol is 1:1, the additive amount of the silane coupling agent containing double bond in step 2
It is the 2% of nano-starch dispersion liquid quality.
The mass ratio of emulsifier and water is 2-6:100 in step 3, and the mass ratio of initiator and water is 0.1-0.3:100, is received
The mass ratio of rice starch and water is 1-5:100, and the mass ratio of vinylacetate and water is 5-15:100.
Starch is cornstarch, potato starch, starch from sweet potato, tapioca, wheaten starch, any in green starch
Kind；Silane coupling agent containing double bond is gamma-methyl allyl acyloxypropyl trimethoxysilane, vinyltriethoxysilane, ethylene
Any one of base trimethoxy silane；Emulsifier is neopelex, lauryl sodium sulfate, potassium oleate, tristearin
Any one of sour sodium；Initiator is any one of potassium peroxydisulfate, sodium peroxydisulfate, hydrogen peroxide, isopropyl benzene hydroperoxide.
Matrix is any one of cotton fabric, nylon fabric, dacron, acrylic fabric, polypropylene fabric.
The invention has the advantages that a kind of preparation method of super-hydrophobic coat containing nano-starch, including nano-starch point
The preparation of dispersion liquid, the surface treatment of nano-starch dispersion liquid, nano-starch polymerize with vinyl acetate emulsion, hydrophobic lotions are to base
The dip-coating of matter obtains super-hydrophobic coat containing nano-starch.The present invention uses starch as nano material, not only cheap, and
And there is excellent environmental-protecting performance；Use polyvinyl acetate as low-surface energy substance, price is than fluorine-containing or siliceous chemistry
Product are cheap, and are significantly reduced to the harm of environment.The method for preparing super-hydrophobic coat is dip coating, with self-assembly method, wet
Chemical method, sol-gel method are compared with chemical vapour deposition technique, and technical process is simple, without expensive equipment, and use the party
The coating of method preparation has good ultra-hydrophobicity, to the contact angle of water more than 151.6 °.
Specific embodiment
The present invention is described in detail With reference to embodiment.
A kind of preparation method of the super-hydrophobic coat containing nano-starch, is specifically implemented according to the following steps:
Step 1, using ultrasonication starch, prepare nano-starch dispersion liquid；
Detailed process are as follows: weigh starch and water in mass ratio for 5-10:100, starch, which is added to the water stirring, makes starch point
Dissipate uniformly, then at 2-10 DEG C carry out ultrasonication 4-8h, obtain nano-starch dispersion liquid, wherein starch be cornstarch,
Any one of potato starch, starch from sweet potato, tapioca, wheaten starch, green starch；.
Step 2 is surface-treated nano-starch dispersion liquid, prepares surface treated nano-starch；
Detailed process are as follows: dehydrated alcohol and silane coupling agent containing double bond are sequentially added into nano-starch dispersion liquid, in 40-
After stirring 1-8h at 80 DEG C, it is centrifuged, washs, obtain surface treated nano-starch, wherein nano-starch dispersion liquid
Volume ratio with dehydrated alcohol is 1:1, and the additive amount of the silane coupling agent containing double bond is the 2% of nano-starch dispersion liquid quality, is contained
Double bond silane coupling agent is γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, vinyl three
Any one of methoxy silane.
Surface treated nano-starch polymerize, hydrophobic synthetic lotion by step 3 with vinyl acetate emulsion；
Detailed process are as follows: emulsifier and initiator are added to the water and stirred evenly, surface treated is then sequentially added
Nano-starch and vinylacetate obtain hydrophobic lotions after mixing in 40-60 DEG C of emulsion polymerisation 4-8h, wherein emulsification
The mass ratio of agent and water is 2-6:100, and the mass ratio of initiator and water is 0.1-0.3:100, the mass ratio of nano-starch and water
For 1-5:100, the mass ratio of vinylacetate and water is 5-15:100, and emulsifier is neopelex, dodecyl
Any one of sodium sulphate, potassium oleate, odium stearate；Initiator is potassium peroxydisulfate, sodium peroxydisulfate, hydrogen peroxide, isopropylbenzene mistake
Any one of hydrogen oxide.
Step 4, by hydrophobic lotions dip-coating on the substrate surface, preparation have ultra-hydrophobicity coating；
Detailed process are as follows: first by distilled water ultrasonic cleaning 1-4 times rear drying of matrix, take the matrix after drying, immerse
It in hydrophobic lotions, after stirring 5-30min at room temperature, is put into baking oven and is dried in 20-80 DEG C, repeat to immerse, after drying 1-3 times, obtain
Super-hydrophobic coat, wherein matrix is any one of cotton fabric, nylon fabric, dacron, acrylic fabric, polypropylene fabric.
Embodiment 1
5g cornstarch is added in 100g water step 1, after mixing evenly in 2 DEG C of progress ultrasonication 8h, obtains nanometer
Starch dispersion liquid；
80g dehydrated alcohol is added into nano-starch dispersion liquid for step 2, adds 2g γ-methacryloxypropyl
Trimethoxy silane is stirred to react 8h at 40 DEG C, after being centrifuged, washing, obtains surface treated nano-starch.
2g neopelex and 0.1g potassium peroxydisulfate are added in 100g water and stir evenly by step 3, then plus
Enter the nano-starch and 5g vinylacetate being surface-treated through 1g, after mixing in 40 DEG C of progress emulsion polymerizations, reacts 8h, obtain
Hydrophobic lotions；
Step 4, by cotton fabric with drying after distilled water ultrasonic cleaning 1 time, the fabric after taking drying is immersed in step 3
In the hydrophobic lotions of preparation, stir 5min at room temperature, be put into baking oven dried in 20 DEG C lotion dip-coating fabric, repeat immerse,
After drying 1 time, the cotton fabric of super-hydrophobic coat containing nano-starch is obtained.
Embodiment 2
A kind of preparation method of the super-hydrophobic coat containing nano-starch, is specifically implemented according to the following steps:
10g potato starch is added in 100g water after mixing evenly in 10 DEG C of progress ultrasonications, processing step 1
Time is 4h, obtains nano-starch dispersion liquid；
80g dehydrated alcohol is added into nano-starch dispersion liquid for step 2, adds 2g vinyltriethoxysilane,
80 DEG C are stirred to react 1h, and surface treated nano-starch is obtained after being centrifuged, washing.
Step 3 will stir evenly in 6g lauryl sodium sulfate and 0.3g ammonium persulfate addition 100g water, be subsequently added into
The nano-starch and 15g vinylacetate being surface-treated through 5g react 4h, obtain after mixing in 60 DEG C of progress emulsion polymerizations
Hydrophobic lotions；
Step 4, by nylon fabric with drying after distilled water ultrasonic cleaning 4 times, the fabric after taking drying is immersed in step
In the hydrophobic lotions of 3 preparations, 30min is stirred at room temperature, is put into baking oven in the fabric of 80 DEG C of lotion dip-coatings obtained by drying, is repeated to soak
After entering, drying 3 times, the nylon fabric of super-hydrophobic coat containing nano-starch is obtained.
Embodiment 3
A kind of preparation method of the super-hydrophobic coat containing nano-starch, is specifically implemented according to the following steps:
5g starch from sweet potato is added in 100g water after mixing evenly in 8 DEG C of progress ultrasonications step 1, handles the time
For 6h, nano-starch dispersion liquid is obtained；
80g dehydrated alcohol is added into nano-starch dispersion liquid for step 2, adds 2g vinyltrimethoxysilane,
60 DEG C are stirred to react 4h, up to surface treated nano-starch after being centrifuged, washing.
Step 3 will stir evenly in 2g potassium oleate and 0.1g hydrogen peroxide addition 100g water, be subsequently added into through the surface 1g
The nano-starch and 5g vinylacetate of processing react 8h, obtain hydrophobic lotions after mixing in 40 DEG C of progress emulsion polymerizations；
Step 4, by dacron with drying after distilled water ultrasonic cleaning 1 time, the fabric after taking drying is immersed in step
In the hydrophobic lotions of 3 preparations, 5min is stirred at room temperature, is put into baking oven in the fabric of 30 DEG C of lotion dip-coatings obtained by drying, is repeated to soak
After entering, drying 2 times, the dacron of super-hydrophobic coat containing nano-starch is obtained.
Embodiment 4
A kind of preparation method of the super-hydrophobic coat containing nano-starch, specifically according to the following steps
10g tapioca is added in 100g water after mixing evenly in 2 DEG C of progress ultrasonications step 1, handles the time
For 7h, nano-starch dispersion liquid is obtained；
80g dehydrated alcohol is added into nano-starch dispersion liquid for step 2, adds 2g γ-methacryloxypropyl
Trimethoxy silane is stirred to react 7h at 40 DEG C, is centrifuged, washs, obtains surface treated nano-starch.
Step 3 will stir evenly in 6g odium stearate and 0.3g isopropyl benzene hydroperoxide addition 100g water, be subsequently added into
The nano-starch and 15g vinylacetate being surface-treated through 1g react 6h, i.e., after mixing in 50 DEG C of progress emulsion polymerizations
Obtain hydrophobic lotions；
Step 4, by acrylic fabric with drying after distilled water ultrasonic cleaning 2 times, the fabric after taking drying is immersed in step
In the hydrophobic lotions of 3 preparations, 10min is stirred at room temperature, baking oven is put into and dries in 40 DEG C, obtain the fabric of lotion dip-coating, repeats to soak
After entering, drying 3 times, the acrylic fabric of super-hydrophobic coat containing nano-starch is obtained.
Embodiment 5
A kind of preparation method of the super-hydrophobic coat containing nano-starch, specifically according to the following steps
5g wheaten starch is added in 100g water after mixing evenly in 10 DEG C of progress ultrasonications step 1, handles the time
It is 3h to get nano-starch dispersion liquid；
80g dehydrated alcohol is added into nano-starch dispersion liquid for step 2, adds 2g vinyltriethoxysilane,
40 DEG C are stirred to react 8h, after being centrifuged, washing, obtain surface treated nano-starch.
Step 3 will stir evenly in 4g neopelex and 0.2g isopropyl benzene hydroperoxide addition 100g water,
It is subsequently added into the nano-starch and 8g vinylacetate being surface-treated through 3g, after mixing in 60 DEG C of progress emulsion polymerizations, instead
4h is answered, hydrophobic lotions are obtained；
Step 4, by polypropylene fabric with drying after distilled water ultrasonic cleaning 3 times, the fabric after taking drying is immersed in step
In the hydrophobic lotions of 3 preparations, 20min is stirred at room temperature, baking oven is put into and dries in 60 DEG C, obtain the fabric of lotion dip-coating, repeats to soak
After entering, drying 2 times, the polypropylene fabric of super-hydrophobic coat containing nano-starch is obtained.
Embodiment 6
A kind of preparation method of the super-hydrophobic coat containing nano-starch, is specifically implemented according to the following steps:
10g green starch is added in 100g water after mixing evenly in 2 DEG C of progress ultrasonications step 1, handles the time
It is 8h to get nano-starch dispersion liquid；
80g dehydrated alcohol is added into nano-starch dispersion liquid for step 2, adds 2g silane coupling agent vinyl front three
Oxysilane is stirred to react 1h at 80 DEG C, after being centrifuged, washing, obtains surface treated nano-starch.
Step 3 will stir evenly in 6g lauryl sodium sulfate and 0.1g ammonium persulfate addition 100g water, be subsequently added into
The nano-starch and 15g vinylacetate being surface-treated through 1g react 4h, obtain after mixing in 60 DEG C of progress emulsion polymerizations
Hydrophobic lotions；
Step 4, by cotton fabric with drying after distilled water ultrasonic cleaning 4 times, the fabric after taking drying is immersed in step 3
In the hydrophobic lotions of preparation, 30min is stirred at room temperature, is put into baking oven in the fabric of 80 DEG C of lotion dip-coatings obtained by drying, is repeated to soak
After entering, drying 3 times, the cotton fabric of super-hydrophobic coat containing nano-starch is obtained.
The calculating process of dehydrated alcohol quality in 1-6 of the embodiment of the present invention are as follows:
Starch, which is added to the water stirring, keeps starch dispersion uniform, obtains nano-starch dispersion liquid, wherein the matter of starch and water
Amount takes the water of 100mL, the starch of 5g-10g is added, then nano-starch dispersion liquid is similar to 100mL, nanometer than being 5-10:100
The volume ratio of starch dispersion liquid and dehydrated alcohol is 1:1, then ethyl alcohol volume is 100mL, and the density of ethyl alcohol is 0.789g/cm3,
Then the quality of ethyl alcohol is 78.9g, about 80g.
Super-hydrophobic coat performance prepared in the above embodiments is tested below by two kinds of test modes:
Test one: the hydrophobicity of super-hydrophobic coat is tested
It is knitted using video optics contact angle measurement (JW-360A type, China) measurement distilled water in the cotton that embodiment 1 obtains
Contact angle on object.On cotton fabric prepared by the test result display present invention, water contact angle is 155.9 °, and is continued
30min is without significant change, it is shown that the ultra-hydrophobicity of the fabric.Simultaneously inventor to the embodiment of the present invention 2, embodiment 3,
Embodiment 4, embodiment 5, the 5 kinds of fabrics prepared in embodiment 6 have done same test, and test result is shown in Table 1, shows the present invention
Super-hydrophobic coat fabric be provided with ultra-hydrophobicity.
The hydrophobic performance tables of data of 1 super-hydrophobic coat fabric of table
| Fabric | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Contact angle | 155.9° | 153.2° | 154.3° | 151.6° | 152.7° | 161.5.5° |
Test two: the washability of super-hydrophobic coat is tested
Embodiment 1 is obtained cotton fabric to be dipped in the aqueous solution that mass concentration is 1% liquid detergent, the revolving speed of 200 turns/min
Lower stirring 30min, then dries at room temperature, so repeats 30 times, measures cotton fabric to the contact angle of water, test result shows
Cotton fabric is still both greater than 150 ° to the contact angle of water.Inventor is to the embodiment of the present invention 2, embodiment 3, embodiment 4, reality simultaneously
Apply example 5,5 kinds of fabrics preparing in embodiment 6 have done same test, test result is shown in Table 2, and test result shows of the invention
Super-hydrophobic coat fabric is all larger than 150 ° to the contact angle of water, these results explanation, super-hydrophobic coat fabric of the invention has
Good washability.
The washability tables of data of the test super-hydrophobic coat fabric of table 2
| Fabric | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Contact angle | 152.3° | 150.7° | 152.1° | 150.4° | 150.7° | 150.5° |
Claims (10)
1. a kind of preparation method of super-hydrophobic coat containing nano-starch, which is characterized in that be specifically implemented according to the following steps:
Step 1, using ultrasonication starch, prepare nano-starch dispersion liquid；
Step 2 is surface-treated nano-starch dispersion liquid, prepares surface treated nano-starch；
Surface treated nano-starch polymerize, hydrophobic synthetic lotion by step 3 with vinyl acetate emulsion；
Step 4, by hydrophobic lotions dip-coating on the substrate surface, preparation have ultra-hydrophobicity coating.
2. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 1, which is characterized in that the step
Rapid 1 detailed process are as follows: starch, which is added to the water stirring, keeps starch dispersion uniform, then carries out at ultrasonic wave at 2-10 DEG C
Reason, obtains nano-starch dispersion liquid.
3. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 1, which is characterized in that the step
The process that nano-starch dispersion liquid is surface-treated in rapid 2 are as follows: dehydrated alcohol is sequentially added into nano-starch dispersion liquid and containing double
Key silane coupling agent is centrifuged, washs, obtain surface treated nano-starch after stirring 1-8h at 40-80 DEG C.
4. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 1, which is characterized in that the step
The detailed process of hydrophobic synthetic lotion in rapid 3 are as follows: emulsifier and initiator are added to the water and stirred evenly, is then sequentially added
Surface treated nano-starch and vinylacetate obtain hydrophobic cream after mixing in 40-60 DEG C of emulsion polymerisation 4-8h
Liquid.
5. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 1, which is characterized in that the step
The process of hydrophobic lotions dip-coating is carried out in rapid 4 to stromal surface are as follows: first by distilled water ultrasonic cleaning 1-4 times rear baking of matrix
Dry, after taking drying matrix immerses in hydrophobic lotions, after stirring 5-30min at room temperature, is put into baking oven and dries in 20-80 DEG C, weight
It is multiple to immerse, after drying 1-3 times, obtain super-hydrophobic coat.
6. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 2, which is characterized in that the step
Ultrasonic treatment time is 4-8h in rapid 1, and the mass ratio of starch and water is 5-10:100.
7. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 3, which is characterized in that the step
The volume ratio of nano-starch dispersion liquid and dehydrated alcohol is 1:1 in rapid 2, and the additive amount of the silane coupling agent containing double bond is nano-starch
The 2% of dispersion liquid quality.
8. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 4, which is characterized in that the step
The mass ratio of emulsifier and water is 2-6:100 in rapid 3, and the mass ratio of initiator and water is 0.1-0.3:100, nano-starch and water
Mass ratio be 1-5:100, the mass ratio of vinylacetate and water is 5-15:100.
9. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 1-8, feature exist
In, the starch be cornstarch, potato starch, starch from sweet potato, tapioca, wheaten starch, any in green starch
Kind；The silane coupling agent containing double bond be gamma-methyl allyl acyloxypropyl trimethoxysilane, vinyltriethoxysilane,
Any one of vinyltrimethoxysilane；The emulsifier is neopelex, lauryl sodium sulfate, oleic acid
Any one of potassium, odium stearate；The initiator is potassium peroxydisulfate, in sodium peroxydisulfate, hydrogen peroxide, isopropyl benzene hydroperoxide
It is any.
10. a kind of preparation method of super-hydrophobic coat containing nano-starch according to claim 9, which is characterized in that described
Matrix is any one of cotton fabric, nylon fabric, dacron, acrylic fabric, polypropylene fabric.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810982787.4A CN109235037B (en) | 2018-08-27 | 2018-08-27 | Preparation method of nano-starch super-hydrophobic coating |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5618621A (en) * | 1979-07-26 | 1981-02-21 | Asahi Fiber Glass Co Ltd | Production of glass fiber-reinforced thermoplastic resin molding material |
| CN85108817A (en) * | 1984-12-07 | 1986-05-10 | 第一工业制药株式会社 | Permeable tarpaulin paint for fabric |
| JPH04147843A (en) * | 1990-10-11 | 1992-05-21 | Toray Ind Inc | Coated article |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5618621A (en) * | 1979-07-26 | 1981-02-21 | Asahi Fiber Glass Co Ltd | Production of glass fiber-reinforced thermoplastic resin molding material |
| CN85108817A (en) * | 1984-12-07 | 1986-05-10 | 第一工业制药株式会社 | Permeable tarpaulin paint for fabric |
| JPH04147843A (en) * | 1990-10-11 | 1992-05-21 | Toray Ind Inc | Coated article |
Non-Patent Citations (2)
| Title |
|---|
| YANHUA ZHANG，ET AL.: "Preparation and properties of a starch-based wood adhesive with highbonding strength and water resistance", 《CARBOHYDRATE POLYMERS》 * |
| 商品学教材编写组: "《商品学》", 28 February 1981 * |
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