CN103421423A - Method for preparing high-temperature-resistant super-hydrophobic coating in situ - Google Patents
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Abstract
The invention discloses a method for preparing a high-temperature-resistant super-hydrophobic coating in situ. The method comprises the following steps: (1) conducting in-situ copolymerization of organosilicon monomers and nano silicon dioxide particles; (2) preparing sol nano particles; (3) preparing a coating solution; (4) preparing a super-hydrophobic surface; (5) performing thermal treatment on a coating. The method solves the problems of small adhesive force, complex technology, high cost, expensive raw materials and the like of the conventional super-hydrophobic coating. The contact angle between water and the super-hydrophobic coating prepared in the invention is 150-160 degrees, the rolling angle is smaller than or equal to than 5 degrees, and the adhesive force can reach the first grade; the super-hydrophobic coating can keep a super-hydrophobic property even after being heated at 450 DEG C, and has unique properties of self cleaning, corrosion resistance and super hydrophobicity. The method is simple in process, and convenient to operate,. The super-hydrophobic coating is suitable for large-area construction, and has a potential and wide application value in various fields such as the industry, construction, national defense and medicine.
Description
Technical field
The present invention relates to the preparation method of hydrophobic coating, particularly a kind of in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat.
Background technology
People are to derive from nature for the understanding of super-hydrophobic phenomenon at first, as lotus leaf can go out mud and not dye, are due to surperficial super-hydrophobicity, and its key reason is on blade face, to have a large amount of micro nano structure papilla things and lip-deep wax jointly to cause.This phenomenon and reason have caused investigation of materials person's very big interest, prepare multiple super-hydrophobic coating material.
Chinese patent (CN1544482) is by carrying out fluorochemical monomer
60Co irradiation, in the atmosphere of non-fluorine-containing alkene, aggregate into super hydrophobic film, prepare fluorine-containing multipolymer, the contact angle of film is greater than 130 °, and the method gained surface water contact angle is relatively low, contain fluorine in raw material, material expensive, and operation easier is large relatively, to environment and operator, requires high.Chinese patent (CN1272114C) has been reported and has been utilized the phase separation method of amorphism polymer in the volatilization process of poor solvent to form coarse super hydrophobic surface to reach super-hydrophobic phenomenon, the coatingsurface sticking power extreme difference that the method makes, poisonous (the toluene of while part reagent, benzene etc.), be unfavorable for environmental protection and person health.The primary structure of the columnar arrays that it is same material that Chinese patent (CN102553812A) adopts the method for etching to prepare with substrate material on polymer substrate surface, again in the surface deposition zinc oxide seed layer of the primary structure of columnar arrays, but subsequently substrate is put into to the growth media of growth of zinc oxide nano linear array, make the surface growth of primary structure go out the secondary structure of zinc oxide nano-wire array, the polymer substrate that will prepare again the firsts and seconds structure immerses the solution that is dissolved with hydrophobic substance, after making the surface of the firsts and seconds structure on the polymer substrate adhere to hydrophobic substance fully, the polymer substrate is taken out, dry, obtain needed super hydrophobic surface, this process device complicated (laser radiation etc.), can not big area operate, thereby apply limited.Chinese patent (CN102795786A) directly is dispersed in blend in ethanol or cyclohexane to silicone resin and Nano particles of silicon dioxide, and then spraying obtains super hydrophobic surface, but coating adhesion extreme difference prepared by the method, and surface becomes powder.
Summary of the invention
With not enough, the object of the present invention is to provide a kind of in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat for the above-mentioned shortcoming that overcomes prior art, possess skills easy, physical strength is high, cost is low, formula is simple, raw material and the advantage such as product is nontoxic.
Purpose of the present invention is achieved through the following technical solutions:
A kind of in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat comprises the following steps:
(1) organosilane monomer and the copolymerization of nano-silicon dioxide particle in-situ method: nano-silicon dioxide particle is added in aqueous ethanolic solution, the composite organic monomer is added, and dropping hydrochloric acid is made catalyzer, increase the temperature to 70 ℃~80 ℃, stir copolycondensation 16h~21h, make the organic and inorganic system; The mass ratio of described nano-silicon dioxide particle and composite organic monomer is (0.05~0.10): 1;
(2) preparation of colloidal sol nanoparticle: tetraethoxy is added drop-wise in the alkaline alcohol solution of 50 ℃~70 ℃, insulation reaction 3h~5h makes colloidal sol nanoparticle that can stable existence;
(3) preparation of coating solution: the colloidal sol nanoparticle is joined to the organic and inorganic system, in 60 ℃~70 ℃ lower stirring reaction 3h~5h, obtain coating solution;
(4) preparation of super hydrophobic surface: coating solution is arrived to substrate surface with spray gun spraying, obtain being coated with the base material of micro-nano compound coating; Spray gun pressure 0.5MPa~1.5MPa wherein, spray gun is apart from substrate surface 4cm~10cm, and spray gun and substrate surface are 70 °~90 ° angles;
(5) thermal treatment of coating: the base material that is coated with micro-nano compound coating that step (4) is obtained is placed at the temperature of 140 ℃~160 ℃ and toasts 3h~5h, at substrate surface, obtains resistant to elevated temperatures super-hydrophobic coat.
Described nano-silicon dioxide particle is nano-silicon dioxide particle prepared by vapor phase process.
The size of described nano-silicon dioxide particle is 10nm~30nm.
Described composite organic monomer comprises methyltrimethoxy silane, propyl trimethoxy silicane and dimethoxydiphenylsilane, methyltrimethoxy silane wherein, propyl trimethoxy silicane, the mol ratio of dimethoxydiphenylsilane: (4.0~4.3): 1.0:(1.2~1.4).
Described the composite organic monomer is added, is specially:
First add dimethoxydiphenylsilane reaction 3h~5h, then add propyl trimethoxy silicane reaction 2h~4h, last methylate Trimethoxy silane reaction 10h~12h.
Described alkaline alcohol solution is (0.04~0.1) by ammoniacal liquor and ethanol by volume: 1 forms.
The volume ratio of described tetraethoxy and alkaline alcohol solution is (0.04~0.08): 1.
Described aqueous ethanolic solution forms by ethanol is water-soluble, ethanol: water: the mass ratio of composite organic monomer is (1.18~2.37): (0.2~0.4): 1.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention uses nontoxic siloxanes raw material, and preparation process is polluted little, and product has farthest reduced the injury to human body and environment, and the environmental protection degree is high, compares the monomers such as silicon fluoride, wide material sources, low price simultaneously; Compound siloxanyl monomers hydrolysis condensation reaction technique is simple, easy to prepare, and the reaction process gentleness is therefore easy to control.
(2) coating that the present invention makes possesses good sticking power than other super-hydrophobic coat, because there are a large amount of silicon hydroxyls in coating, and the quite effect of coupling agent.Can under the environment such as soda acid, use at high temperature, because coatingsurface is mainly the Si-O key simultaneously, its bond energy is very high, forms tridimensional network simultaneously, does not contain polar substituent, and coating has a small amount of Si-C key, makes it at normal temperatures, there is good acidproof, alkaline-resisting performance.
(3) the present invention can operate by spraying method on multiple base material, solidify and make and 150 °~160 ° of water contact angles, roll angle≤5 °, sticking power reaches one-level, the coating that also possesses super-hydrophobicity after 450 ℃ of barbecues, the performance that its surface has many uniquenesses is as automatically cleaning, protection against corrosion, super-hydrophobic etc.This preparation method's technique is simple, easy to operate, can large-area construction, therefore in a lot of fields as industry, building, national defence, medicine etc. has potential and using value widely.
The accompanying drawing explanation
The surface topography map of the resistant to elevated temperatures super-hydrophobic coat that Fig. 1 is embodiment 2 preparations.
The sticking power data plot of the resistant to elevated temperatures super-hydrophobic coat that Fig. 2 is embodiment 1~3 preparation.
The resistance to elevated temperatures data plot of the resistant to elevated temperatures super-hydrophobic coat that Fig. 3 is embodiment 3 preparations.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
The in-situ preparation method of the resistant to elevated temperatures super-hydrophobic coat of the present embodiment comprises the following steps:
(1) organosilane monomer and the copolymerization of inorganic particulate in-situ method: the 0.5g Nano particles of silicon dioxide is added in the 15ml ethanolic soln containing 2ml water and is warmed up to 80 ℃, 1.50g phenylbenzene dimethoxysiloxane monomer is added and drips several hydrochloric acid and make catalyzer stirring reaction 3h, then add 0.82g propyl trimethoxy siloxanyl monomers to react 3h in above-mentioned system, finally add 2.68g methyl trimethoxy oxygen base oxygen alkane monomer reaction 10h, make the organic and inorganic mixed system;
(2) preparation of colloidal sol nanoparticle: the 4ml tetraethoxy is added drop-wise to 60 ℃ containing in the 5ml ethanolic soln of 2ml ammoniacal liquor, and insulation reaction 3h makes the colloidal sol nanoparticle of energy stable existence;
(3) preparation of coating solution: colloidal sol nanoparticle prepared by step (2) joins in organic and inorganic system prepared by step (1), at 60 ℃ of stirring reaction 3h, prepares coating solution;
(4) preparation of super hydrophobic surface: coating solution is arrived to sheet glass base material (or iron plate base material) surface with spray gun spraying, obtain being coated with the base material of micro-nano compound coating; Control spray gun pressure 1.5MPa, spray gun is apart from the surperficial 10cm of sheet glass base material (or iron plate base material), and spray gun and substrate surface are 90 ° of angles and are sprayed into coating;
(5) base material that is coated with micro-nano compound coating step (4) obtained is placed at the temperature of 140 ℃ and toasts 5h, makes that coating is full cross-linked solidifies, to improve the sticking power of coating, thermostability.
The sticking power data of resistant to elevated temperatures super-hydrophobic coat prepared by the present embodiment (take the sheet glass base material as example) are shown in Fig. 2, and known energy is realized very good sticking power, reaches one-level.Resistant to elevated temperatures super-hydrophobic coat prepared by the present embodiment is 153 ° at contact angle on glass, and roll angle is 2 °; Contact angle on tinsel is 155 °, and roll angle is about 1 °, at tinsel with on glassly can realize superhydrophobic property.
The in-situ preparation method of the resistant to elevated temperatures super-hydrophobic coat of the present embodiment comprises the following steps:
(1) organosilane monomer and the copolymerization of inorganic particulate in-situ method: the 0.6g Nano particles of silicon dioxide is added in the 20ml ethanolic soln containing 3ml water and is raised to temperature to 70 ℃, 1.70g phenylbenzene dimethoxysiloxane monomer is added and drips several hydrochloric acid and make catalyzer stirring reaction 4h, then add 1.00g propyl trimethoxy siloxanyl monomers to stirring reaction 4h in above-mentioned system, finally add 3.00g methyl trimethoxy oxygen base oxygen alkane monomer stirring reaction 12h, make the organic and inorganic mixed system.
(2) preparation of colloidal sol nanoparticle: the 3ml tetraethoxy is added drop-wise to 50 ℃ containing in the 50ml ethanolic soln of 3ml ammoniacal liquor, and insulated and stirred reaction 5h makes the colloidal sol nanoparticle of energy stable existence;
(3) preparation of coating solution: colloidal sol nanoparticle prepared by step (2) joins in organic and inorganic system prepared by step (1), at 70 ℃ of stirring reaction 4h;
(4) preparation of super hydrophobic surface: coating solution to sheet glass base material surface, obtains being coated with the base material of micro-nano compound coating with spray gun spraying; Control spray gun pressure 1.0MPa, spray gun is apart from sheet glass base material surface 7cm, and spray gun and substrate surface are 80 ° of angles and are sprayed into coating.
(5) base material that is coated with micro-nano compound coating step (4) obtained is placed at the temperature of 160 ℃ and toasts 3h, makes that coating is full cross-linked solidifies, to improve the sticking power of coating, thermostability.
The sticking power data of resistant to elevated temperatures super-hydrophobic coat prepared by the present embodiment are shown in Fig. 2, also can reach secondary, meet industrial application; Its surface topography is shown in Fig. 1, known surface irregularity injustice, and as the coral structure, this is most important for realizing superhydrophobic property.
The in-situ preparation method of the resistant to elevated temperatures super-hydrophobic coat of the present embodiment comprises the following steps:
(1) organosilane monomer and the copolymerization of inorganic particulate in-situ method: the 1.0g Nano particles of silicon dioxide is added in the 30ml ethanolic soln containing 4ml water, be warmed up to 75 ℃, 3.1g phenylbenzene dimethoxysiloxane monomer is added and drips several hydrochloric acid and make catalyzer stirring reaction 5h, then add 1.5g propyl trimethoxy siloxanyl monomers to react 3h in above-mentioned system, finally add 5.4g methyl trimethoxy oxygen base oxygen alkane monomer stirring reaction 12h, make the organic and inorganic system.
(2) preparation of colloidal sol nanoparticle: the 2ml tetraethoxy is added drop-wise to 70 ℃ containing in the 50ml ethanolic soln of 4ml ammoniacal liquor, and insulated and stirred reaction 4h makes the colloidal sol nanoparticle of energy stable existence;
(3) preparation of coating solution: colloidal sol nanoparticle prepared by step (2) joins in organic and inorganic system prepared by step (1), at 60 ℃ of stirring reaction 5h;
(4) preparation of super hydrophobic surface: coating solution to sheet glass base material surface, obtains being coated with the base material of micro-nano compound coating with spray gun spraying; Control spray gun pressure 0.5MPa, spray gun is apart from sheet glass base material surface 4cm, and spray gun and substrate surface are 70 ° of angles and are sprayed into coating;
(5) base material that is coated with micro-nano compound coating step (4) obtained is placed at the temperature of 160 ℃ and toasts 3h, makes that coating is full cross-linked solidifies, to improve the sticking power of coating, thermostability.
The sticking power data of resistant to elevated temperatures super-hydrophobic coat prepared by the present embodiment are shown in Fig. 2, and sticking power may descend a little, but still can meet utilization to a certain extent; Its high temperature resistant ultra-hydrophobicity is shown in Fig. 3, as shown in Figure 3, up to 450 ℃, also can realize super-hydrophobicity.
In above-described embodiment:
Surface topography map is obtained by scanning electronic microscope.
Contact angle is recorded by the video contact angle measurement.
Resistance to elevated temperatures is under differing temps, after baking 1.5h, to be cooled to the contact angle reading that room temperature obtains at retort furnace.
The sticking power data are measured and are obtained according to GB GB-T9286-1998.
Nano particles of silicon dioxide prepared by the vapor phase process used in embodiment, the trade mark is REOLOSILQS-102, manufacturer is a day Bender mountain TOKUYAMA.
The methyl trimethoxy oxygen radical siloxane monomer used in embodiment, the trade mark is JH-N311, manufacturer is Jing Zhou, Hubei Province Jiang-Han Area Fine Chemical Co., Ltd.
The phenylbenzene dimethoxysiloxane monomer used in embodiment, the trade mark is JH-N620, manufacturer is all Jing Zhou, Hubei Province Jiang-Han Area Fine Chemical Co., Ltd.
The propyl trimethoxy siloxanyl monomers used in embodiment, the trade mark is JH-N313, manufacturer is Jing Zhou, Hubei Province Jiang-Han Area Fine Chemical Co., Ltd.
The dehydrated alcohol used in embodiment, tetraethoxy, ammoniacal liquor (W25%) is all analytical pure, manufacturer is Chemical Reagent Co., Ltd., Sinopharm Group.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not limited by the examples; as; composite organic monomer of the present invention can also comprise dimethyldimethoxysil,ne; phenyltrimethoxysila,e etc.; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify, and all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (8)
1. the in-situ preparation method of a resistant to elevated temperatures super-hydrophobic coat, is characterized in that, comprises the following steps:
(1) organosilane monomer and the copolymerization of nano-silicon dioxide particle in-situ method: nano-silicon dioxide particle is added in aqueous ethanolic solution, the composite organic monomer is added, and dropping hydrochloric acid is made catalyzer, increase the temperature to 70 ℃~80 ℃, stir copolycondensation 16h~21h, make the organic and inorganic system; The mass ratio of described nano-silicon dioxide particle and composite organic monomer is (0.05~0.10): 1;
(2) preparation of colloidal sol nanoparticle: tetraethoxy is added drop-wise in the alkaline alcohol solution of 50 ℃~70 ℃, insulation reaction 3h~5h makes colloidal sol nanoparticle that can stable existence;
(3) preparation of coating solution: the colloidal sol nanoparticle is joined to the organic and inorganic system, in 60 ℃~70 ℃ lower stirring reaction 3h~5h, obtain coating solution;
(4) preparation of super hydrophobic surface: coating solution is arrived to substrate surface with spray gun spraying, obtain being coated with the base material of micro-nano compound coating; Spray gun pressure 0.5MPa~1.5MPa wherein, spray gun is apart from substrate surface 4cm~10cm, and spray gun and substrate surface are 70 °~90 ° angles;
(5) thermal treatment of coating: the base material that is coated with micro-nano compound coating that step (4) is obtained is placed at the temperature of 140 ℃~160 ℃ and toasts 3h~5h, at substrate surface, obtains resistant to elevated temperatures super-hydrophobic coat.
2. the in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat according to claim 1, is characterized in that, described nano-silicon dioxide particle is nano-silicon dioxide particle prepared by vapor phase process.
3. the in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat according to claim 1 and 2, is characterized in that, the size of described nano-silicon dioxide particle is 10nm~30nm.
4. the in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat according to claim 1, it is characterized in that, described composite organic monomer comprises methyltrimethoxy silane, propyl trimethoxy silicane and dimethoxydiphenylsilane, methyltrimethoxy silane wherein, propyl trimethoxy silicane, the mol ratio of dimethoxydiphenylsilane: (4.0~4.3): 1.0:(1.2~1.4).
5. the in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat according to claim 4, is characterized in that, described the composite organic monomer added, and is specially:
First add dimethoxydiphenylsilane reaction 3h~5h, then add propyl trimethoxy silicane reaction 2h~4h, last methylate Trimethoxy silane reaction 10h~12h.
6. the in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat according to claim 1, is characterized in that, described alkaline alcohol solution is (0.04~0.1) by ammoniacal liquor and ethanol by volume: 1 forms.
7. the in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat according to claim 6, is characterized in that, the volume ratio of described tetraethoxy and alkaline alcohol solution is (0.04~0.08): 1.
8. the in-situ preparation method of resistant to elevated temperatures super-hydrophobic coat according to claim 1, it is characterized in that, described aqueous ethanolic solution forms by ethanol is water-soluble, ethanol: water: the mass ratio of composite organic monomer is (1.18~2.37): (0.2~0.4): 1.
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