CN105080357B - A kind of method that water dispersible particle prepares super-hydrophobic composite film - Google Patents
A kind of method that water dispersible particle prepares super-hydrophobic composite film Download PDFInfo
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Abstract
A kind of method that water dispersible particle prepares super-hydrophobic composite film, the present invention relates to a kind of method that water dispersible particle prepares super-hydrophobic composite film.It is organic phase the invention aims to solve dispersed phase used in existing super-hydrophobic film, causes the waste of organic solvent and the problem of to environmental disruption, method：First, octadecylamine is dissolved in toluene solution, in the alkaline aqueous solution being then added to, stirring obtains mixed solution A；2nd, Dopamine hydrochloride is dissolved in mixed solution A, stirs, obtain mixed solution B；3rd, mixed solution B is centrifuged, takes solid formation to be washed with deionized, then ultrasonic disperse, then filtered through the filtration apparatus equipped with polymeric membrane, obtain composite membrane, be placed in air drying, that is, complete.The present invention realize it is hydrophilic arrive super-hydrophobic conversion, both efficiently avoid the waste of organic solvent, while also give composite membrane with self-healing properties.The present invention is used for inorganic and high-molecular organic material field.
Description
Technical field
The present invention relates to a kind of method that water dispersible particle prepares super-hydrophobic composite film.
Background technology
In recent years, super-hydrophobic film automatically cleaning, miniflow system, drag reduction, the energy recover, it is antifouling and it is special separation etc.
Potential application, it has been recognized that tremendous influence of the hydrophobic film to practical application.Therefore superhydrophobic films are prepared as grinding
The person's of studying carefully focus of attention.In general, the contact angle of film surface water is more than 120 ° to be super-hydrophobic, and most of researchs in recent years
It is super-hydrophobic that person thinks that contact angle is just called more than 150 °.Dispersed phase used in existing super-hydrophobic film is organic phase, this is resulted in
The waste of organic solvent and to environmental disruption.
The content of the invention
It is organic phase the invention aims to solve dispersed phase used in existing super-hydrophobic film, causes the wave of organic solvent
Take and the problem of to environmental disruption, there is provided a kind of method that water dispersible particle prepares super-hydrophobic composite film.
A kind of method that water dispersible particle prepares super-hydrophobic composite film, specifically prepares according to following steps：
First, octadecylamine is dissolved in toluene solution, obtains the toluene solution containing octadecylamine, be then added to while stirring
PH is in 8.0~9.5 alkaline aqueous solution, continues 10~30min of stirring, obtains mixed solution A；The wherein first containing octadecylamine
The volume ratio of benzole soln and the pH alkaline aqueous solutions for being 8.0~9.5 is 1:(9~12)；
2nd, Dopamine hydrochloride is dissolved in mixed solution A, stirs 12~36h, obtain mixed solution B；
3rd, mixed solution B is centrifuged, takes solid formation to be washed with deionized, then ultrasonic disperse obtains water in water phase
Phase dispersant liquid；
4th, the aqueous dispersion liquid for obtaining step 3 passes through the filtration apparatus equipped with polymeric membrane and filters, and obtains composite membrane, will
Composite membrane is placed in air drying, obtains super-hydrophobic composite film.
The present invention prepares composite membrane using water dispersible particle through suction filtration, is realized by standing hydrophilic to super-hydrophobic turn
Change, both efficiently avoid the waste of organic solvent, while also give composite membrane with self-healing properties.Skill according to the invention
Super-hydrophobic composite film prepared by art can be widely applied to hydrophobically modified and water-oil separating field.
Brief description of the drawings
Fig. 1 is the picture that aqueous dispersion liquid stands after a week in embodiment one；
Fig. 2 is the digital photograph of super-hydrophobic composite film prepared by embodiment one；
Fig. 3 is one Zhong Shui of embodiment, water phase dyestuff, the digital photograph of milk, coffee droplet on super-hydrophobic composite film；
Fig. 4 is the contact angle picture of poly- cellulose acetate film and water in embodiment one；
Fig. 5 is the contact angle picture of super-hydrophobic composite film prepared by embodiment one and water；
Fig. 6 is the selfreparing test result figure of super-hydrophobic composite film prepared by embodiment one.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, further include each embodiment it
Between any combination.
Embodiment one：The method that a kind of water dispersible particle of present embodiment prepares super-hydrophobic composite film, specifically
It is to be prepared according to following steps：
First, octadecylamine is dissolved in toluene solution, obtains the toluene solution containing octadecylamine, be then added to while stirring
PH is in 8.0~9.5 alkaline aqueous solution, continues 10~30min of stirring, obtains mixed solution A；The wherein first containing octadecylamine
The volume ratio of benzole soln and the pH alkaline aqueous solutions for being 8.0~9.5 is 1:(9~12)；
2nd, Dopamine hydrochloride is dissolved in mixed solution A, stirs 12~36h, obtain mixed solution B；
3rd, mixed solution B is centrifuged, takes solid formation to be washed with deionized, then ultrasonic disperse obtains water in water phase
Phase dispersant liquid；
4th, the aqueous dispersion liquid for obtaining step 3 passes through the filtration apparatus equipped with polymeric membrane and filters, and obtains composite membrane, will
Composite membrane is placed in air drying, obtains super-hydrophobic composite film.
Present embodiment prepares composite membrane using water dispersible particle through suction filtration, is realized by standing hydrophilic to super-hydrophobic
Conversion, both efficiently avoid the waste of organic solvent, while also give composite membrane with self-healing properties.According to this implementation
Super-hydrophobic composite film prepared by the technology of mode can be widely applied to hydrophobically modified and water-oil separating field.
Embodiment two：The present embodiment is different from the first embodiment in that：Contain ten described in step 1
Final concentration of 5~20mg/mL of octadecylamine in the toluene solution of eight amine.It is other identical with embodiment one.
Embodiment three：The present embodiment is different from the first and the second embodiment in that：Containing described in step 1
There is the final concentration of 10mg/mL of octadecylamine in the toluene solution of octadecylamine.It is other the same as one or two specific embodiments.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Described in step 1
Alkaline aqueous solution pH value be 8.5.It is other identical with one of embodiment one to three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Described in step 1
Alkaline aqueous solution be by the trishydroxymethylaminomethane of concentration 0.1mol/L, the hydrochloric acid of concentration 0.1mol/L and water by volume
1:(0.27~0.31):The buffer solution that the ratio of (0.68~0.71) is formulated.Other and embodiment one to four
One of it is identical.
Embodiment six：Unlike one of present embodiment and embodiment one to five：Described in step 2
Mixed solution B in Dopamine hydrochloride final concentration of 0.5~5mg/mL.Other phases one of with embodiment one to five
Together.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：Described in step 2
Mixed solution B in Dopamine hydrochloride final concentration of 2mg/mL.It is other identical with one of embodiment one to six.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：Described in step 2
Mixing time be 24h.It is other identical with one of embodiment one to seven.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：Described in step 3
The power of ultrasonic disperse be 450W, frequency 20KHZ.It is other identical with one of embodiment one to eight.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：Described in step 4
Polymeric membrane be poly- cellulose acetate film or polyvinylidene fluoride film.It is other identical with one of embodiment one to nine.
Beneficial effects of the present invention are verified using following embodiments：
Embodiment 1：The method that the present embodiment water dispersible particle prepares super-hydrophobic composite film, specifically according to following steps
Prepare：
First, octadecylamine is dissolved in toluene solution, obtains the toluene solution containing octadecylamine, be then added to while stirring
PH is in 8.5 alkaline aqueous solution, continues to stir 20min, obtains mixed solution A；Wherein in the toluene solution containing octadecylamine
The final concentration of 10mg/mL of octadecylamine；Alkaline aqueous solution is trishydroxymethylaminomethane, the concentration 1mol/L by concentration 1mol/L
Hydrochloric acid and water by volume 1：0.3：The buffer solution that 0.7 ratio is formulated；Toluene solution and pH containing octadecylamine
Volume ratio for 8.5 alkaline aqueous solution is 1:10；
2nd, Dopamine hydrochloride is dissolved in mixed solution A, stirs 24h, obtain mixed solution B；Wherein mixed solution B
The final concentration of 2mg/mL of middle Dopamine hydrochloride；
3rd, mixed solution B is centrifuged, takes solid formation to be washed with deionized, then ultrasonic disperse obtains water in water phase
Phase dispersant liquid；The power of ultrasonic disperse is 450W, frequency 20KHZ；
4th, the aqueous dispersion liquid for obtaining step 3 passes through the filtration apparatus equipped with poly- cellulose acetate film and filters, and is answered
Film is closed, composite membrane is placed in air drying, obtains super-hydrophobic composite film.
The aqueous dispersion liquid of the present embodiment step 3 stands picture after a week as shown in Figure 1, as shown in Figure 1, step 3
Aqueous dispersion liquid still can disperse by the standing of one week.
The digital photograph of super-hydrophobic composite film manufactured in the present embodiment is as shown in Fig. 2, as shown in Figure 2, water dispersible particle
The super-hydrophobic composite film of preparation can be bent than more uniform.
Jiang Shui, water phase dyestuff, milk, coffee droplet are tested on super-hydrophobic composite film, and the results are shown in Figure 3, by Fig. 3
Understand, water, dyestuff, milk, coffee drop on the super-hydrophobic composite film of water dispersible particle preparation respectively, and contact angle is larger, liquid
Body does not soak composite membrane.
The contact angle picture of commercially available poly- cellulose acetate film and water is as shown in figure 4, manufactured in the present embodiment super-hydrophobic multiple
The contact angle picture of film and water is closed as shown in figure 5, as shown in Figure 4, the contact angle of macromolecule basement membrane and water is almost 0 °, by Fig. 5
Understand, super-hydrophobic composite film and the contact angle of water prepared by water dispersible particle is more than 150 °.
Irradiate 30 seconds through oxygen gas plasma and circulated in 80 DEG C of baking oven heating 30min for one, test the present embodiment
The self-healing properties of the super-hydrophobic composite film of preparation, as a result it will be appreciated from fig. 6 that illustrating the test of obtained hydrophobic composite membrane in figure
Data, show that obtained composite membrane has self-healing properties.
Embodiment 2：The method that the present embodiment water dispersible particle prepares super-hydrophobic composite film, specifically according to following steps
Prepare：
First, octadecylamine is dissolved in toluene solution, obtains the toluene solution containing octadecylamine, be then added to while stirring
PH is in 8.5 alkaline aqueous solution, continues to stir 15min, obtains mixed solution A；Wherein in the toluene solution containing octadecylamine
The final concentration of 15mg/mL of octadecylamine；Alkaline aqueous solution is trishydroxymethylaminomethane by concentration 0.1mol/L, concentration
The hydrochloric acid and water of 0.1mol/L by volume 1：0.3：The buffer solution that 0.7 ratio is formulated；Toluene containing octadecylamine
The volume ratio of solution and the pH alkaline aqueous solutions for being 8.5 is 1:10；
2nd, Dopamine hydrochloride is dissolved in mixed solution A, stirs 24h, obtain mixed solution B；Wherein mixed solution B
The final concentration of 2.5mg/mL of middle Dopamine hydrochloride；
3rd, mixed solution B is centrifuged, takes solid formation to be washed with deionized, then ultrasonic disperse obtains water in water phase
Phase dispersant liquid；The power of ultrasonic disperse is 450W, frequency 20KHZ；
4th, the aqueous dispersion liquid for obtaining step 3 passes through the filtration apparatus equipped with polyvinylidene fluoride film and filters, and obtains compound
Film, is placed in air drying by composite membrane, obtains super-hydrophobic composite film.
The contact angle of super-hydrophobic composite film and water manufactured in the present embodiment is more than 150 °, to manufactured in the present embodiment super-hydrophobic
Composite membrane carries out self-healing properties test, the results showed that super-hydrophobic composite film manufactured in the present embodiment has self-healing properties.
Embodiment 3：The method that the present embodiment water dispersible particle prepares super-hydrophobic composite film, specifically according to following steps
Prepare：
First, octadecylamine is dissolved in toluene solution, obtains the toluene solution containing octadecylamine, be then added to while stirring
PH is in 8.5 alkaline aqueous solution, continues to stir 30min, obtains mixed solution A；Wherein in the toluene solution containing octadecylamine
The final concentration of 20mg/mL of octadecylamine；Alkaline aqueous solution is trishydroxymethylaminomethane by concentration 0.1mol/L, concentration
The hydrochloric acid and water of 0.1mol/L by volume 1：0.3：The buffer solution that 0.7 ratio is formulated；Toluene containing octadecylamine
The volume ratio of solution and the pH alkaline aqueous solutions for being 8.5 is 1:10；
2nd, Dopamine hydrochloride is dissolved in mixed solution A, stirs 24h, obtain mixed solution B；Wherein mixed solution B
The final concentration of 5mg/mL of middle Dopamine hydrochloride；
3rd, mixed solution B is centrifuged, takes solid formation to be washed with deionized, then ultrasonic disperse obtains water in water phase
Phase dispersant liquid；The power of ultrasonic disperse is 450W, frequency 20KHZ；
4th, the aqueous dispersion liquid for obtaining step 3 passes through the filtration apparatus equipped with poly- cellulose acetate film and filters, and is answered
Film is closed, composite membrane is placed in air drying, obtains super-hydrophobic composite film.
The contact angle of super-hydrophobic composite film and water manufactured in the present embodiment is more than 150 °, to manufactured in the present embodiment super-hydrophobic
Composite membrane carries out self-healing properties test, the results showed that super-hydrophobic composite film manufactured in the present embodiment has self-healing properties.
Embodiment 4：The method that the present embodiment water dispersible particle prepares super-hydrophobic composite film, specifically according to following steps
Prepare：
First, octadecylamine is dissolved in toluene solution, obtains the toluene solution containing octadecylamine, be then added to while stirring
PH is in 8.5 alkaline aqueous solution, continues to stir 20min, obtains mixed solution A；Wherein in the toluene solution containing octadecylamine
The final concentration of 5mg/mL of octadecylamine；Alkaline aqueous solution is trishydroxymethylaminomethane, the concentration 1mol/L by concentration 1mol/L
Hydrochloric acid and water by volume 1：0.3：The buffer solution that 0.7 ratio is formulated；Toluene solution and pH containing octadecylamine
Volume ratio for 8.5 alkaline aqueous solution is 1:10；
2nd, Dopamine hydrochloride is dissolved in mixed solution A, stirs 24h, obtain mixed solution B；Wherein mixed solution B
The final concentration of 0.5mg/mL of middle Dopamine hydrochloride；
3rd, mixed solution B is centrifuged, takes solid formation to be washed with deionized, then ultrasonic disperse obtains water in water phase
Phase dispersant liquid；The power of ultrasonic disperse is 450W, frequency 20KHZ；
4th, the aqueous dispersion liquid for obtaining step 3 passes through the filtration apparatus equipped with polyvinylidene fluoride film and filters, and obtains compound
Film, is placed in air drying by composite membrane, obtains super-hydrophobic composite film.
The contact angle of super-hydrophobic composite film and water manufactured in the present embodiment is more than 150 °, to manufactured in the present embodiment super-hydrophobic
Composite membrane carries out self-healing properties test, the results showed that super-hydrophobic composite film manufactured in the present embodiment has self-healing properties.
In conclusion the present invention prepares composite membrane using water dispersible particle through suction filtration, hydrophilic arrive is realized by standing
Super-hydrophobic conversion, both efficiently avoid the waste of organic solvent, while also give composite membrane with self-healing properties.According to
Super-hydrophobic composite film prepared by the technology of the present invention can be widely applied to hydrophobically modified and water-oil separating field.
Claims (10)
1. a kind of method that water dispersible particle prepares super-hydrophobic composite film, it is characterised in that this method is to follow these steps reality
It is existing：
Octadecylamine, be dissolved in toluene solution by step (1), obtains the toluene solution containing octadecylamine, then adds while stirring
In the alkaline aqueous solution for being 8.0~9.5 to pH, continue 10~30min of stirring, obtain mixed solution A；Wherein containing octadecylamine
The volume ratio of toluene solution and the pH alkaline aqueous solutions for being 8.0~9.5 is 1:(9~12)；
Dopamine hydrochloride, be dissolved in mixed solution A by step (2), stirs 12~36h, obtains mixed solution B；
Step (3), centrifuge mixed solution B, takes solid formation to be washed with deionized, then ultrasonic disperse obtains in water phase
Aqueous dispersion liquid；
Step (4), the aqueous dispersion liquid for obtaining step (3) pass through the filtration apparatus equipped with polymeric membrane and filter, and obtain composite membrane,
Composite membrane is placed in air drying, obtains super-hydrophobic composite film.
2. the method that a kind of water dispersible particle according to claim 1 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly in the toluene solution containing octadecylamine described in (1) octadecylamine final concentration of 5~20mg/mL.
3. the method that a kind of water dispersible particle according to claim 2 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly in the toluene solution containing octadecylamine described in (1) octadecylamine final concentration of 10mg/mL.
4. the method that a kind of water dispersible particle according to claim 1 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly the pH value of the alkaline aqueous solution described in (1) is 8.5.
5. the method that a kind of water dispersible particle according to claim 1 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly the alkaline aqueous solution described in (1) be by the trishydroxymethylaminomethane of concentration 0.1mol/L, the hydrochloric acid of concentration 0.1mol/L and
Water by volume 1:(0.27~0.31):The buffer solution that the ratio of (0.68~0.71) is formulated.
6. the method that a kind of water dispersible particle according to claim 1 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly in the mixed solution B described in (2) Dopamine hydrochloride final concentration of 0.5~5mg/mL.
7. the method that a kind of water dispersible particle according to claim 6 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly in the mixed solution B described in (2) Dopamine hydrochloride final concentration of 2mg/mL.
8. the method that a kind of water dispersible particle according to claim 1 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly the mixing time described in (2) is 24h.
9. the method that a kind of water dispersible particle according to claim 1 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly the power of the ultrasonic disperse described in (3) is 450W, frequency 20KHz.
10. the method that a kind of water dispersible particle according to claim 1 prepares super-hydrophobic composite film, it is characterised in that step
Suddenly the polymeric membrane described in (4) is poly- cellulose acetate film or polyvinylidene fluoride film.
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| CN109487561A (en) * | 2017-09-10 | 2019-03-19 | 北京林业大学 | A kind of hydrophobic bamboo fibre and preparation method thereof based on mussel protein biomimetic modification |
| CN109173740A (en) * | 2018-10-26 | 2019-01-11 | 哈尔滨工业大学宜兴环保研究院 | A kind of preparation method of water single channel film |
| CN109576997B (en) * | 2018-11-16 | 2020-03-06 | 江南大学 | Preparation method of self-repairing super-hydrophobic fabric |
| CN113341011B (en) * | 2021-06-01 | 2022-11-29 | 中国药科大学 | Solid phase extraction material for extracting and enriching PAHs and application thereof in polycyclic aromatic hydrocarbon compound detection |
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| CN102961893B (en) * | 2012-11-07 | 2014-11-26 | 清华大学 | Super-hydrophobic and super-oleophylic oil-water separating mesh membrane and preparation method thereof |
| CN104275099B (en) * | 2014-10-30 | 2016-08-24 | 哈尔滨工业大学 | A kind of preparation method of the most superoleophobic modified polyvinilidene fluoride film |
| CN104831534B (en) * | 2015-03-06 | 2016-08-31 | 哈尔滨工业大学宜兴环保研究院 | A kind of super-hydrophobic super-oleophylic cloth preparation method for material |
| CN104826363A (en) * | 2015-04-30 | 2015-08-12 | 清华大学 | Super-hydrophobic super-lipophilic emulsion separating mesh membrane, and production method and application thereof |
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