CN105860120A - Super-hydrophobic polypropylene film and preparation method thereof - Google Patents
Super-hydrophobic polypropylene film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to super-hydrophobic film materials and provides a super-hydrophobic polypropylene film and a preparation method thereof. The super-hydrophobic polypropylene film is characterized in that an isotactic polypropylene-b-polyethylene glycol diblock copolymer serves as a surface modifier to construct a micronano composite structure on the surface of the polypropylene film. The preparation method includes steps: dissolving the isotactic polypropylene-b-polyethylene glycol diblock copolymer in an alkane solvent to obtain a polymer solution, coating to the surface of the polypropylene film by spin coating, putting the polypropylene film subjected to surface modification into a vacuum drying oven, and performing vacuum drying to obtain the super-hydrophobic polypropylene film. The super-hydrophobic polypropylene film and the preparation method thereof have advantages that simplicity in operation is achieved, complex chemical treatment is avoided, and expensive equipment is not needed; the preparation method is high in efficiency, feasible, environment friendly, low in cost and easy for industrialization; the prepared super-hydrophobic polypropylene film has excellent surface structural stability.
Description
Technical field
The present invention is about superhydrophobic thin film material technical field, particularly to a kind of super-hydrophobic polypropylene film and preparation method thereof.
Background technology
Nature exists multiple biology there is superhydrophobic property, the hydrophobic phenomenon of such as lotus leaf surface is that the globule on its surface is also taken away the pollutant of lotus leaf surface while rolling, thus playing self-cleaning effect, this effect is the waxy substance by lotus leaf surface and micro nano structure causes.Research about super hydrophobic material at present is concentrated mainly on polymeric material and metal material.Polypropylene (PP) is cheap, environmental friendliness, be widely used, and has excellent mechanical property, heat resistance, electrical property, chemical stability and weatherability.Super hydrophobic material with polypropylene as matrix has been widely used at self-cleaning material, drag-reducing coating, anticorrosion, the aspect such as waterproof, antifog, anti-pollution.
The preparation method of super-hydrophobic polypropylene film mainly has two technology paths: one is the rough surface structure in polypropylene surface structure micron-nanometer level；Two is to be chemically modified rough surface structure by low-surface energy substance.Mainly include template, phase separation method, plasma etching method, chemical vapour deposition technique etc..
Template is the more commonly used method, if Lin Xunliang etc. is with anodised aluminium as template, uses hot pressing lift-off technology to be prepared for super-hydrophobic PP film, and contact angle has reached 150 ° (Chemical Industry in Guangzhous, 2013,41 (12): 112).Polypropylene solution, with sulphurated siliastic as template, is cast in sulphurated siliastic soft template by Wu Junliang etc., and tears after drying in atmosphere at room temperature environment and be super-hydrophobic polypropylene film (Chinese invention patent, application number: 201210260474.0).Template technique is simple, but service life is the longest.
Erbil etc. use phase separation method, dissolve isotactic polypropylene particle with dimethylbenzene for solvent, and add butanone and be adjusted being prepared for super-hydrophobic polypropylene film to the structure of PP as non-solvent, and contact angle reaches 160 ° (Science, 2003,299:1377).Lucky petrels etc. dissolve isotactic polypropylene particle with dimethylbenzene for solvent, and add acetone and as non-solvent, the structure of PP is adjusted, being prepared for super-hydrophobic polypropylene film by the tape casting, contact angle reaches 152～174 ° (Chinese invention patent, application numbers: 200910024925.9).Phase separation method equipment is simple, low cost, but has certain toxicity about solvent in the report of phase separation method and non-solvent at present more, is unfavorable for the application of method.
Huo Zhengyuan etc. use plasma etching method that PP surface is performed etching process, make material surface produce loose structure, and top layer exists certain roughness.Subsequently by dodecafluoroheptyl methacrylate glycerol polymerization to the PP substrate surface processed, contact angle is more than 150 ° (science and technology circulars, 2009,25:711).Plasma etching technology is to prepare rough surface directly effective method, but the mechanical strength of rough surface is relatively low, makes super-hydrophobic poor stability, and along with the increase of standing time, its effect gradually weakens.
Jiang etc. use chemical vapour deposition technique, with porous polypropylene fibre for matrix deposition n-octyl trichlorosilane.The contact angle super hydrophobic material (The Journal of The Textile Institute, 2013,104:790) more than 156 ° is prepared by this kind of method.The preparation cost of chemical vapour deposition technique is high, is unfavorable for large-scale production.Fluorine has the lowest surface energy, and fluoropolymer can be used for super hydrophobic material, it is common that use fluorochemical monomer polymerization or the method being directly fluorinated material.Purerskiy etc. are prepared for perfluorooctylethyl group iodine and the silicone-modified silicon dioxide granule mixed liquor of 3-aminopropyl-triethoxy, afterwards by thin film dipped for PP in mixed liquor, obtain the PP material (Langmuir, 2012,28:3679) possessing superhydrophobic property.But, fluorochemical is expensive, limits the popularization and application of the method to a certain extent.
Summary of the invention
Present invention is primarily targeted at and overcome deficiency of the prior art, it is provided that a kind of super-hydrophobic polypropylene film and efficient, easy, environmental protection thereof and lower-cost preparation method.For solving above-mentioned technical problem, the solution of the present invention is:
Thering is provided a kind of super-hydrophobic polypropylene film, main body is polypropylene film, and with isotactic polypropylene-b-polyethylene glycol two block thing, i.e. iPP-b-PEG is surface modifier, and the surface construction at polypropylene film has (stable) micron and nanometer composite structure；
Described micron and nanometer composite structure, i.e. utilizes iPP segment and PEG chain segment in iPP-b-PEG to be easy crystalline segment, when separating out in the solution, and respective distinct crystalline and the micron and nanometer composite structure that formed.
In the present invention, described super-hydrophobic polypropylene film surface is 141～157 ° with the contact angle of water, and the water droplet roll angle on super-hydrophobic polypropylene film surface is less than 10 °.
The method of super-hydrophobic polypropylene film described in preparation is provided, specifically includes following step:
Isotactic polypropylene-b-polyethylene glycol two block thing (iPP-b-PEG) is dissolved in alkane solvent, obtains polymer solution；Then polymer solution is spin-coated on polypropylene film surface, polypropylene film is carried out surface modification；Again the polypropylene film through surface modification is placed in vacuum drying oven, vacuumizes and be dried and reclaim the solvent evaporated, i.e. obtain super-hydrophobic polypropylene film.
In the present invention, described when preparing polymer solution, use and weigh iPP-b-PEG when joining in alkane solvent, temperature is risen to 100 DEG C～120 DEG C, under magnetic stirring, forms the polymer solution that concentration is 1～50mg/mL.
In the present invention, described alkane solvent uses normal octane or normal heptane.
In the present invention, in described iPP-b-PEG, the number-average molecular weight of iPP segment is 1000～15000g/mol, and the number-average molecular weight of PEG chain segment is 300～5300g/mol.
The principle of the present invention: provide a kind of isotactic polypropylene-b-polyethylene glycol two block thing (iPP-b-PEG) and preparation method thereof in Chinese invention patent ZL 2,013 1 0419485.3, this preparation method step is simple, efficient, easily realizes；The raw material used is the common raw material of industry, cheap, it is easy to industrialized production；Can be by regulating the length of two kinds of segments, the performance of regulation and control block thing；In two block things of preparation, isotactic polypropylene segment maintains the highest isotacticity.In iPP-b-PEG, iPP segment and PEG chain segment are easy crystalline segment, when they separate out in the solution, respective distinct crystalline are formed micron and nanometer composite structure.Additionally, iPP-b-PEG has between iPP segment and polypropylene film good compatibility, if being coated in polypropylene film surface with iPP-b-PEG for surface modifier, iPP-b-PEG will " grappling " on polypropylene film surface, form constitutionally stable micron and nanometer composite structure at film surface, thus give polypropylene film ultra-hydrophobicity.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention is simple to operate, it is not necessary to complicated chemical treatment, it is not required that expensive equipment, preparation method is efficient, easy, environmental protection and cost relatively low, it is easy to industrialization.The super-hydrophobic polypropylene film obtained has good surface texture stability.
Accompanying drawing explanation
Fig. 1 is the super-hydrophobic polypropylene film photo with water contact angle of embodiment 1 preparation.
Fig. 2 is the stereoscan photograph on the super-hydrophobic polypropylene film surface of embodiment 1 preparation.
Fig. 3 is the magnified sweep electromicroscopic photograph of black box in Fig. 2.
Fig. 4 is the stereoscan photograph on the super-hydrophobic polypropylene film surface of embodiment 1 preparation.
Detailed description of the invention
With detailed description of the invention, the present invention is described in further detail below in conjunction with the accompanying drawings:
The following examples can make the professional and technical personnel of this specialty that the present invention is more fully understood, but limits the present invention never in any form.
Embodiment 1
Weigh 17.6mg iPP-b-PEG (wherein the number-average molecular weight of iPP segment is 7800g/mol), the number-average molecular weight of PEG chain segment is 2300g/mol, it is placed in 5mL volumetric flask, add normal octane to scale, being heated to 110 DEG C makes polymer be completely dissolved, and then uses spin coating instrument that polymer solution is spin-coated on clean polypropylene film surface (water contact angle of polypropylene film itself is 100 °).Finally it is placed on the polypropylene film through surface modification in vacuum drying oven to vacuumize and is dried and reclaims the solvent evaporated, obtain super-hydrophobic polypropylene film.Using OCAH200 contact angle tester to test the wetability of this film surface, result shows that this surface is 153 ° with the contact angle of water, and roll angle is less than 10 °, such as Fig. 1.Use Sirion-100 type field emission scanning electron microscope that film surface appearance is observed, find that this film surface exists micron and nanometer composite structure, such as Fig. 2.Film tipping upside down on 45° angle the beaker mouth filling 95 DEG C of hot water, carries out stifling 96 hours with the steam of heat, the most so-called hot mist is tested.Test result indicate that, the super-hydrophobic polypropylene film obtained has good surface texture stability, and before and after experiment, film is constant with the contact angle of water.
Embodiment 2
Weigh 17.6mg iPP-b-PEG (wherein the number-average molecular weight of iPP segment is 6500g/mol), the number-average molecular weight of PEG chain segment is 2300g/mol, it is placed in 5mL volumetric flask, add normal octane to scale, being heated to 110 DEG C makes polymer be completely dissolved, and then uses spin coating instrument that polymer solution is spin-coated on clean polypropylene film surface (water contact angle of polypropylene film itself is 100 °).Finally it is placed on the polypropylene film through surface modification in vacuum drying oven to vacuumize and is dried and reclaims the solvent evaporated, obtain super-hydrophobic polypropylene film.Using OCAH200 contact angle tester to test the wetability of this film surface, result shows that this surface is 151 ° with the contact angle of water, and roll angle is less than 10 °.Hot mist test result indicate that, the super-hydrophobic polypropylene film obtained has good surface texture stability.
Embodiment 3
Weigh 17.6mg iPP-b-PEG (wherein the number-average molecular weight of iPP segment is 5500g/mol), the number-average molecular weight of PEG chain segment is 2300g/mol, it is placed in 5mL volumetric flask, add normal octane to scale, being heated to 110 DEG C makes polymer be completely dissolved, and then uses spin coating instrument that polymer solution is spin-coated on clean polypropylene film surface (water contact angle of polypropylene film itself is 100 °).Finally it is placed on the polypropylene film through surface modification in vacuum drying oven to vacuumize and is dried and reclaims the solvent evaporated, obtain super-hydrophobic polypropylene film.Using OCAH200 contact angle tester to test the wetability of this film surface, result shows that this surface is 146 ° with the contact angle of water, and roll angle is less than 10 °.Hot mist test result indicate that, the super-hydrophobic polypropylene film obtained has good surface texture stability.
Embodiment 4
Weigh 17.6mg iPP-b-PEG (wherein the number-average molecular weight of iPP segment is 4400g/mol), the number-average molecular weight of PEG chain segment is 2300g/mol, it is placed in 5mL volumetric flask, add normal octane to scale, being heated to 110 DEG C makes polymer be completely dissolved, and then uses spin coating instrument that polymer solution is spin-coated on clean polypropylene film surface (water contact angle of polypropylene film itself is 100 °).Finally it is placed on the polypropylene film through surface modification in vacuum drying oven to vacuumize and is dried and reclaims the solvent evaporated, obtain super-hydrophobic polypropylene film.Using OCAH200 contact angle tester to test the wetability of this film surface, result shows that this surface is 145 ° with the contact angle of water, and roll angle is less than 10 °.Hot mist test result indicate that, the super-hydrophobic polypropylene film obtained has good surface texture stability.
Embodiment 5
Weigh 17.6mg iPP-b-PEG (wherein the number-average molecular weight of iPP segment is 9500g/mol), the number-average molecular weight of PEG chain segment is 2300g/mol, it is placed in 5mL volumetric flask, add normal octane to scale, being heated to 110 DEG C makes polymer be completely dissolved, and then uses spin coating instrument that polymer solution is spin-coated on clean polypropylene film surface (water contact angle of polypropylene film itself is 100 °).Finally it is placed on the polypropylene film through surface modification in vacuum drying oven to vacuumize and is dried and reclaims the solvent evaporated, obtain super-hydrophobic polypropylene film.Using OCAH200 contact angle tester to test the wetability of this film surface, result shows that this surface is 142 ° with the contact angle of water, and roll angle is less than 10 °.Hot mist test result indicate that, the super-hydrophobic polypropylene film obtained has good surface texture stability.
Embodiment 6
Weigh 250mg iPP-b-PEG (wherein the number-average molecular weight of iPP segment is 1000g/mol), the number-average molecular weight of PEG chain segment is 300g/mol, it is placed in 5mL volumetric flask, add normal heptane to scale, being heated to 100 DEG C makes polymer be completely dissolved, and then uses spin coating instrument that polymer solution is spin-coated on clean polypropylene film surface (water contact angle of polypropylene film itself is 100 °).Finally it is placed on the polypropylene film through surface modification in vacuum drying oven to vacuumize and is dried and reclaims the solvent evaporated, obtain super-hydrophobic polypropylene film.Using OCAH200 contact angle tester to test the wetability of this film surface, result shows that this surface is 157 ° with the contact angle of water, and roll angle is less than 10 °.Hot mist test result indicate that, the super-hydrophobic polypropylene film obtained has good surface texture stability.
Embodiment 7
Weigh 5mg iPP-b-PEG (wherein the number-average molecular weight of iPP segment is 15000g/mol), the number-average molecular weight of PEG chain segment is 5300g/mol, it is placed in 5mL volumetric flask, add normal octane to scale, being heated to 120 DEG C makes polymer be completely dissolved, and then uses spin coating instrument that polymer solution is spin-coated on clean polypropylene film surface (water contact angle of polypropylene film itself is 100 °).Finally it is placed on the polypropylene film through surface modification in vacuum drying oven to vacuumize and is dried and reclaims the solvent evaporated, obtain super-hydrophobic polypropylene film.Using OCAH200 contact angle tester to test the wetability of this film surface, result shows that this surface is 141 ° with the contact angle of water, and roll angle is less than 10 °.Hot mist test result indicate that, the super-hydrophobic polypropylene film obtained has good surface texture stability.
It is only the specific embodiment of the present invention finally it should be noted that listed above.It is clear that the invention is not restricted to above example, it is also possible to there is many variations.All deformation that those of ordinary skill in the art can directly derive from present disclosure or associate, are all considered as protection scope of the present invention.
Claims (6)
1. a super-hydrophobic polypropylene film, main body is polypropylene film, it is characterised in that gather with isotactic polypropylene-b-
Ethylene glycol two block thing, i.e. iPP-b-PEG is surface modifier, and the surface construction at polypropylene film has micro-nano compound
Structure；
Described micron and nanometer composite structure, i.e. utilizes iPP segment and PEG chain segment in iPP-b-PEG to be easy crystalline segment,
When separating out in the solution, respective distinct crystalline and the micron and nanometer composite structure that formed.
A kind of super-hydrophobic polypropylene film the most according to claim 1, it is characterised in that described super-hydrophobic poly-third
Alkene film surface is 141～157 ° with the contact angle of water, and the water droplet roll angle on super-hydrophobic polypropylene film surface is less than
10°。
3. the method for super-hydrophobic polypropylene film described in preparation claim 1, it is characterised in that specifically include following step
Rapid:
Isotactic polypropylene-b-polyethylene glycol two block thing is dissolved in alkane solvent, obtains polymer solution；Then will be poly-
Polymer solution is spin-coated on polypropylene film surface, and polypropylene film is carried out surface modification；Again by gathering through surface modification
Polypropylene film is placed in vacuum drying oven, vacuumizes and is dried and reclaims the solvent evaporated, i.e. obtains super-hydrophobic polypropylene thin
Film.
Preparation method the most according to claim 3, it is characterised in that described when preparing polymer solution, uses
Weigh iPP-b-PEG when joining in alkane solvent, temperature is risen to 100 DEG C～120 DEG C, under magnetic stirring, is formed
Concentration is the polymer solution of 1～50mg/mL.
Preparation method the most according to claim 3, it is characterised in that described alkane solvent uses normal octane or just
Heptane.
Preparation method the most according to claim 3, it is characterised in that the number of iPP segment in described iPP-b-PEG
Average molecular weight is 1000～15000g/mol, and the number-average molecular weight of PEG chain segment is 300～5300g/mol.
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Cited By (7)
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| CN106496621A (en) * | 2016-10-03 | 2017-03-15 | 浙江大学 | A kind of method of polyethylene surface super-hydrophobicization |
| CN106540551A (en) * | 2016-10-06 | 2017-03-29 | 浙江大学 | High hydrophobicity polyethylene flat plate porous film and preparation method thereof |
| WO2018193094A1 (en) * | 2017-04-21 | 2018-10-25 | Technische Universität Darmstadt | Regenerative superhydrophobic coating |
| CN111944379A (en) * | 2020-08-25 | 2020-11-17 | 上海大学 | Application of carbohydrate-based block copolymer self-assembled micro-nano structure in anti-icing |
| CN112126092A (en) * | 2020-09-16 | 2020-12-25 | 彭军文 | Super-hydrophobic antibacterial polypropylene film and preparation method thereof |
| CN114504954A (en) * | 2020-11-16 | 2022-05-17 | 中国石油化工股份有限公司 | Multilayer super-hydrophobic composite membrane and preparation method thereof |
| CN115926229A (en) * | 2022-12-30 | 2023-04-07 | 湖南工业大学 | Polypropylene film with super-hydrophobicity and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106496621A (en) * | 2016-10-03 | 2017-03-15 | 浙江大学 | A kind of method of polyethylene surface super-hydrophobicization |
| CN106496621B (en) * | 2016-10-03 | 2019-06-14 | 浙江大学 | A kind of method of polyethylene surface super-hydrophobicization |
| CN106540551A (en) * | 2016-10-06 | 2017-03-29 | 浙江大学 | High hydrophobicity polyethylene flat plate porous film and preparation method thereof |
| CN106540551B (en) * | 2016-10-06 | 2019-08-23 | 浙江大学 | High hydrophobicity polyethylene flat plate porous film and preparation method thereof |
| WO2018193094A1 (en) * | 2017-04-21 | 2018-10-25 | Technische Universität Darmstadt | Regenerative superhydrophobic coating |
| CN111944379A (en) * | 2020-08-25 | 2020-11-17 | 上海大学 | Application of carbohydrate-based block copolymer self-assembled micro-nano structure in anti-icing |
| CN111944379B (en) * | 2020-08-25 | 2021-11-16 | 上海大学 | Application of carbohydrate-based block copolymer self-assembled micro-nano structure in anti-icing |
| CN112126092A (en) * | 2020-09-16 | 2020-12-25 | 彭军文 | Super-hydrophobic antibacterial polypropylene film and preparation method thereof |
| CN114504954A (en) * | 2020-11-16 | 2022-05-17 | 中国石油化工股份有限公司 | Multilayer super-hydrophobic composite membrane and preparation method thereof |
| CN114504954B (en) * | 2020-11-16 | 2023-03-28 | 中国石油化工股份有限公司 | Multilayer super-hydrophobic composite membrane and preparation method thereof |
| CN115926229A (en) * | 2022-12-30 | 2023-04-07 | 湖南工业大学 | Polypropylene film with super-hydrophobicity and preparation method thereof |
| CN115926229B (en) * | 2022-12-30 | 2024-03-29 | 湖南工业大学 | Polypropylene film with superhydrophobicity and preparation method thereof |
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