CN103408990A - Nanoparticle super-hydrophobic self-cleaning wall paint and preparation method thereof - Google Patents
Nanoparticle super-hydrophobic self-cleaning wall paint and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method for hydrophobic nanometer titanium dioxide. The preparation method comprises the following steps: 1) adding nanometer titanium dioxide into distilled water accounting for 0.1 to 2% of the mass of nanometer titanium dioxide, uniformly mixing the above-mentioned components with stirring, then adding a silane coupling agent accounting for 0.1 to 0.5% of the mass of nanometer titanium dioxide, heating to a temperature of 80 to 100 DEG C and carrying out uniform mixing with stirring so as to obtain a mixture I; 2) adding a silicon-fluorine material accounting for 10 to 30% of the mass of the mixture I with slow stirring and continuing stirring until uniform mixing is realized so as to obtain a mixture II; and 3) adding an emulsifier accounting for 3 to 5% of the mass of the mixture II into the mixture II, carrying out high-speed emulsification at a temperature of 80 to 100 DEG C for 90 to 120 min and then carrying out cooling so as to obtain viscous nanometer titanium dioxide slurry, i.e., hydrophobic nanometer titanium dioxide. The invention further provides a nanoparticle super-hydrophobic self-cleaning wall paint containing hydrophobic nanometer titanium dioxide and a preparation method thereof. The nanoparticle super-hydrophobic self-cleaning wall paint has a good hydrophobic function, forms a stable contact angle of 150 DEG with water and a rolling contact angle of less than 5 DEG and has powerful and long-lasting self-cleaning capability.
Description
Technical field
The present invention relates to the wall paint technical field, particularly, relate to a kind of nanoparticle super-hydrophobic self-cleaning wall paint and preparation method thereof.
Background technology
According to bionics, the super-hydrophobic self-cleaning effect reason that lotus leaf surface forms has two: one, and lotus leaf surface is covered with the wax of a layered low-surface energy; The 2nd, there is the mastoid process of certain micro-nano binary roughness on its surface.Wherein the mastoid process of micro-nano binary roughness refers to following two kinds of submicroscopic structures: a kind of is micron-sized projection, and a kind of is nano level hair shape structure.Above-mentioned two kinds of submicroscopic structures of the generation of " lotus leaf effect " and lotus leaf are closely related, and the contact angle of finding after deliberation to contain the lotus leaf of two kinds of structures is 142 °, and the lotus leaf contact angle that only contains micrometer structure is 126 °.Scientist thinks accordingly, and nano level hair shape structure makes contact angle increase by 16 °.
Scientific research finds that water droplet can only contact with several mastoid process points on the lotus leaf face, and water is punctured into spherical under surface tension effects, can roll easily.And dust is while dropping on lotus leaf, dust is just on the salient point of lotus leaf, very little with the contact area of lotus leaf, thereby the adsorptive power of dust and lotus leaf is very little, and the contact area between dust and water droplet is large, stronger adsorptive power is arranged between dust particle and water droplet, just by water droplet, taken away so be easy to, reach self-cleaning function.
As can be seen here, hydrophobic effect will be got well, and the hydrophobic material not only needed prepares super hydrophobic surface, and need to form the nano level salient point at super hydrophobic surface." lotus leaf effect ", as a good model, for numerous areas, can facilitate the clean of house or building surface as the coating based on lotus leaf effect production.
Domestic have a lot of manufacturer production hydrophobic coatings, is all to adopt low-surface-energy material to form one deck hydrophobic surface at substrate surface.Organosilicon material and fluorine material are the confessed hydrophobic surface materials preferably for preparing of present stage.Yet silicone resin be take the Si-O key and is main chain, and has the organosilicon polymers of high side chain.Organosilicon polymer has advantages of excellent heat-resisting, weather resistance, has simultaneously the poor and poor shortcoming of solvent resistance of film forming properties.In the fluoro-resin structure, contain stable C-F key, the C-F key is large because of its strong energy, the characteristics such as little and polarizability key of F atomic radius is little, thereby has excellent weather resistance, weathering resistance and chemical proofing, good non-adhesive, low surface tension and low frictional properties, and hydrophobic, hate oil, the surface property that clean surfaces etc. are special, also there are some defects in the organic fluorine carbon polymer simultaneously, as when as coating, using, poor adhesive force with ground, to pigment, the wettability of filler is poor, the shortcoming such as lower temperature resistance is not good enough, these drawbacks limit applying of fluorine resin coating.
How overcoming the shortcoming of above-mentioned organosilicon material and organic fluorine material, in conjunction with their advantage, and be applied to prepare super hydrophobic coating, is focus and the difficult point of research at present.Simultaneously, prior art also rarely has report that a kind of coating is arranged, and can as lotus leaf, can form hydrophobic surface, can form the nano level salient point at hydrophobic surface again.
Summary of the invention
In order to overcome the deficiencies in the prior art, the application provides a kind of preparation method of hydrophobic nano-titanium dioxide, and contain nanoparticle super-hydrophobic self-cleaning wall paint of this hydrophobic nano-titanium dioxide and preparation method thereof, described nanoparticle super-hydrophobic self-cleaning wall paint, can form hydrophobic surface, can form the nano level salient point at hydrophobic surface again, make it have excellent ultra-hydrophobicity, the stable contact angle of itself and water is greater than 150 degree, the rolling contact angle is less than 5 degree, thereby also has very strong and permanent self-cleaning ability.
Technical scheme of the present invention is as follows: a kind of preparation method of hydrophobic nano-titanium dioxide comprises the steps:
1), nano titanium oxide is added in its quality 0.1%-2% distilled water, then add the silane coupling agent of nano titanium oxide quality 0.1%-0.5%, be warmed to 80-100 ℃, stir, obtain mixture one;
2), slowly stir the lower fluosilicic material that adds mixture one quality 10%-30%, and continue to be stirred to even mixing, obtain mixture two;
3), to the emulsifying agent that adds mixture two quality 3%-5% in mixture two, at 80-100 ℃ of lower emulsify at a high speed 90-120 minute, cooling, obtain the nano titania slurry of thickness, be hydrophobic nano-titanium dioxide.
Described nano titanium dioxide crystal form is rutile-type or Detitanium-ore-type.
Described fluosilicic material is organic silicon-fluorine polymkeric substance or epoxide modified fluosilicic polymkeric substance.
Described fluosilicic material is fluorine-containing poly-(methyl) acrylic ester emulsion with the polysiloxane-grafted modification of long-chain, seven fluorine butyl methyl acrylate as poly-as dimethyl siloxane-b-.
A kind of nanoparticle super-hydrophobic self-cleaning wall paint, comprise each component of following weight parts
The preparation method of described hydrophobic nano-titanium dioxide particle comprises the steps:
1), nano titanium oxide is added in its quality 0.1%-2% distilled water, then add the silane coupling agent of nano titanium oxide quality 0.1%-0.5%, be warmed to 80-100 ℃, stir, obtain mixture one;
2), slowly stir the lower fluosilicic material that adds mixture one quality 10%-30%, and continue to be stirred to even mixing, obtain mixture two;
3), to the emulsifying agent that adds mixture two quality 3%-5% in mixture two, at 80-100 ℃ of lower emulsify at a high speed 90-120 minute, cooling, obtain the nano titania slurry of thickness, be hydrophobic nano-titanium dioxide.
Described filler is any one or a few mixture in diatomite, calcium carbonate, kaolin, Magnesium Silicate q-agent or talcum powder.
Described film-forming resin is any one or a few mixture in epoxy resin, acrylic resin, resol, vibrin.
Described auxiliary agent comprises linking agent, initiator and promotor; Described linking agent is any one or a few the mixture in vinylbenzene, methyl methacrylate or dially phthalate; Described initiator is any one or a few the mixture in Benzoyl Peroxide, methylethyl ketone peroxide, tertbutyl peroxide or isopropyl hydrogen peroxide; Described promotor is any one or a few the mixture in triethylamine, xylidine or Diethyl Aniline.
The preparation method of described nanoparticle super-hydrophobic self-cleaning wall paint, comprise the steps:
1), by the described hydrophobic nano-titanium dioxide of formula weighing, titanium dioxide, filler, film-forming resin, auxiliary agent and distilled water;
2), under normal temperature, titanium dioxide, filler are slowly added in distilled water, be stirred to even mixing, obtain mixture three;
3), in mixture one, slowly add film-forming resin and auxiliary agent, and be stirred to even mixing, obtain mixture four;
4), in mixture four, slowly add hydrophobic nano-titanium dioxide, and be stirred to even mixing, obtain described nanoparticle super-hydrophobic self-cleaning wall paint.
The fluosilicic material contains F-C key, Si-O key and Si-C key, has lower surface energy, so have hydrophobic effect preferably.Therefore, with fluosilicic material parcel titanium dioxide nanoparticle, thereby give the hydrophobic performance that nano titanium oxide is good.
In nanoparticle super-hydrophobic self-cleaning wall paint of the present invention, when the filmogen in coating is dry, can shrink, thereby order is protruded in film coated surface through the titanium dioxide nanoparticle that the fluosilicic material wraps up.At this moment the formed film coated surface of the wall paint that purifies air of the present invention is very similar to lotus leaf surface, not only has super hydrophobic surface, and form the nano level salient point at super hydrophobic surface, thereby had an excellent super hydrophobic functional, after testing, with the stable contact angle of water, be greater than 150 degree, the rolling contact angle is less than 5 degree.
Beneficial effect of the present invention is: the present invention adopts fluosilicic material parcel nano titanium oxide, combine the advantage of organosilicon material and organic fluorine material, form stable hydrophobic nano-titanium dioxide particle, make it have lower surface energy, have preferably hydrophobic performance.The coating that contains fluosilicic material parcel nano titanium oxide shrinks when drying, make the titanium dioxide nanoparticle of fluosilicic material parcel protrude in film coated surface, thereby form the nano level salient point, reaches excellent super-hydrophobic self-cleaning function.Nanoparticle super-hydrophobic self-cleaning wall paint of the present invention nano titanium oxide used, fluosilicic material are tasteless, odorless, nontoxic, without harm, also can not cause other pollutions to human body; Raw materials cost is cheap, technique is simple, is applicable to suitability for industrialized production; The wall paint granule strength is higher, films that it is destroyed to be not easy, and has excellent weather resistance.。
Embodiment
Embodiment 1:
A kind of nanoparticle super-hydrophobic self-cleaning wall paint, comprise each component of following weight parts
Described filler is diatomite.
Described film-forming resin is epoxy resin.
Described auxiliary agent comprises linking agent, initiator and promotor; Described linking agent is vinylbenzene; Described initiator is Benzoyl Peroxide; Described promotor is triethylamine.
The preparation method of described hydrophobic nano-titanium dioxide particle is as follows:
1), the 10kg nano titanium oxide is added in 0.2kg distilled water, stir, then add the silane coupling agent of 0.05kg, be warmed to 80 ℃, stir, obtain mixture one;
2), slowly stir the fluosilicic material of lower interpolation mixture one quality 15%, and continue to be stirred to even mixing, obtain mixture two;
3), to the emulsifying agent that adds mixture two quality 3% in mixture two, 100 ℃ of lower emulsify at a high speed 100 minutes, cooling, obtain the nano titania slurry of thickness, be hydrophobic nano-titanium dioxide.
Described fluosilicic material is the organic silicon-fluorine polymkeric substance, and dimethyl siloxane-b-gathers seven fluorine butyl methyl acrylate; Described emulsifying agent is SDS.
The preparation method of described nanoparticle super-hydrophobic self-cleaning wall paint, comprise the steps:
1), by the described hydrophobic nano-titanium dioxide of formula weighing, titanium dioxide, filler, film-forming resin, auxiliary agent and distilled water;
2), under normal temperature, titanium dioxide, filler are slowly added in distilled water, be stirred to even mixing, obtain mixture three;
3), in mixture three, slowly add film-forming resin and auxiliary agent, and be stirred to even mixing, obtain mixture four;
4), in mixture four, slowly add hydrophobic nano-titanium dioxide, and be stirred to even mixing, obtain the described nano titanium dioxide photocatalysis wall paint that purifies air.
Embodiment 2
A kind of nanoparticle super-hydrophobic self-cleaning wall paint, comprise each component of following weight parts
Described filler is Magnesium Silicate q-agent and talcous mixture.
Described film-forming resin is resol.
Described auxiliary agent comprises linking agent, initiator and promotor; Described linking agent is vinylbenzene and methyl methacrylate; Described initiator is Benzoyl Peroxide and tertbutyl peroxide; Described promotor is Diethyl Aniline.
The preparation method of described hydrophobic nano-titanium dioxide particle is as follows:
1), the 10kg nano titanium oxide is added in 0.1kg distilled water, stir, then add the silane coupling agent of 0.03kg, be warmed to 90 ℃, stir, obtain mixture one;
2), slowly stir the fluosilicic material of lower interpolation mixture one quality 30%, and continue to be stirred to even mixing, obtain mixture two;
3), to the emulsifying agent SDS that adds mixture two quality 5% in mixture two, 80 ℃ of lower emulsify at a high speed 120 minutes, cooling, obtain the nano titania slurry of thickness, be hydrophobic nano-titanium dioxide.
Described fluosilicic material is epoxide modified fluosilicic polymkeric substance.
The preparation method of described nanoparticle super-hydrophobic self-cleaning wall paint, comprise the steps:
1), by the described hydrophobic nano-titanium dioxide of formula weighing, titanium dioxide, filler, film-forming resin, auxiliary agent and distilled water;
2), under normal temperature, titanium dioxide, filler are slowly added in distilled water, be stirred to even mixing, obtain mixture three;
3), in mixture three, slowly add film-forming resin and auxiliary agent, and be stirred to even mixing, obtain mixture four;
4), in mixture four, slowly add hydrophobic nano-titanium dioxide, and be stirred to even mixing, obtain the described nano titanium dioxide photocatalysis wall paint that purifies air.
Embodiment 3
A kind of nanoparticle super-hydrophobic self-cleaning wall paint, comprise each component of following weight parts
Described filler is talcum powder.
Described film-forming resin is acrylic resin.
Described auxiliary agent comprises linking agent, initiator and promotor; Described linking agent is dially phthalate; Described initiator is methylethyl ketone peroxide; Described promotor is the mixture of triethylamine and Diethyl Aniline.
The preparation method of described hydrophobic nano-titanium dioxide particle is as follows:
1), the 10kg nano titanium oxide is added in 0.01kg distilled water, stir, then add the silane coupling agent of 0.01kg, be warmed to 100 ℃, stir, obtain mixture one;
2), slowly stir the fluosilicic material of lower interpolation mixture one quality 10%, and continue to be stirred to even mixing, obtain mixture two;
3), to the emulsifying agent SDS that adds mixture two quality 5% in mixture two, 80 ℃ of lower emulsify at a high speed 120 minutes, cooling, obtain the nano titania slurry of thickness, be hydrophobic nano-titanium dioxide.
Described fluosilicic material is the organic silicon-fluorine polymkeric substance, and dimethyl siloxane-b-gathers seven fluorine butyl methyl acrylate.
The preparation method of described nanoparticle super-hydrophobic self-cleaning wall paint, comprise the steps:
1), by the described hydrophobic nano-titanium dioxide of formula weighing, titanium dioxide, filler, film-forming resin, auxiliary agent and distilled water;
2), under normal temperature, titanium dioxide, filler are slowly added in distilled water, be stirred to even mixing, obtain mixture one;
3), in mixture one, slowly add film-forming resin and auxiliary agent, and be stirred to even mixing, obtain mixture two;
4), in mixture two, slowly add hydrophobic nano-titanium dioxide, and be stirred to even mixing, obtain the described nano titanium dioxide photocatalysis wall paint that purifies air.
The present invention and existing super hydrophobic coating are compared to experiment, and experimental technique is as follows:
Coating is measured with JC2000C1 type contact angle measurement (middle morning digital technique equipment company limited) the static contact angle of water and rolling contact angle, and drop size is 5 μ L, measures according to preset angle configuration, and measuring result is as shown in the table.
Anti-staining property, measure according to the flyash method of GB/T 9780-1988 " anti-the staining property test method of building coating coating " regulation, estimates according to reflectivity, is divided into five grades, and measurement result is as shown in the table.
Concrete experimental result is as follows:
As seen from the above table, the present invention is except having: than the larger static contact angle of common super hydrophobic material and less roll angle, thereby have more good ultra-hydrophobicity; Has the better anti-performance that stains; Have better weathering resistance, tack, abrasion resistance and the advantage such as simple application property more.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by claims of submitting to.
Claims (10)
1. the preparation method of a hydrophobic nano-titanium dioxide, is characterized in that, comprises the steps:
1), nano titanium oxide is added in its quality 0.1%-2% distilled water, then add the silane coupling agent of nano titanium oxide quality 0.1%-0.5%, be warmed to 80-100 ℃, stir, obtain mixture one;
2), slowly stir the lower fluosilicic material that adds mixture one quality 10%-30%, and continue to be stirred to even mixing, obtain mixture two;
3), to the emulsifying agent that adds mixture two quality 3%-5% in mixture two, at 80-100 ℃ of lower emulsify at a high speed 90-120 minute, cooling, obtain the nano titania slurry of thickness, be hydrophobic nano-titanium dioxide.
2. the preparation method of hydrophobic nano-titanium dioxide as claimed in claim 1, is characterized in that, described nano titanium dioxide crystal form is rutile-type or Detitanium-ore-type.
3. the preparation method of hydrophobic nano-titanium dioxide as claimed in claim 1, is characterized in that, described fluosilicic material is organic silicon-fluorine polymkeric substance or epoxide modified fluosilicic polymkeric substance.
4. the preparation method of hydrophobic nano-titanium dioxide as claimed in claim 1 or 2, is characterized in that, described fluosilicic material is the poly-seven fluorine butyl methyl acrylate of dimethyl siloxane-b-.
5. the preparation method of hydrophobic nano-titanium dioxide as claimed in claim 1 or 2, described emulsifying agent is sodium lauryl sulphate.
6. a nanoparticle super-hydrophobic self-cleaning wall paint, is characterized in that, comprises each component of following weight parts
The preparation method of described hydrophobic nano-titanium dioxide particle comprises the steps:
1), nano titanium oxide is added in its quality 0.1%-2% distilled water, then add the silane coupling agent of nano titanium oxide quality 0.1%-0.5%, be warmed to 80-100 ℃, stir, obtain mixture one;
2), slowly stir the lower fluosilicic material that adds mixture one quality 10%-30%, and continue to be stirred to even mixing, obtain mixture two;
3), to the emulsifying agent that adds mixture two quality 3%-5% in mixture two, at 80-100 ℃ of lower emulsify at a high speed 90-120 minute, cooling, obtain the nano titania slurry of thickness, be hydrophobic nano-titanium dioxide.
7. nanoparticle super-hydrophobic self-cleaning wall paint as claimed in claim 6, is characterized in that, described filler is any one or a few mixture in diatomite, calcium carbonate, kaolin, Magnesium Silicate q-agent or talcum powder.
8. nanoparticle super-hydrophobic self-cleaning wall paint as claimed in claim 6, is characterized in that, described film-forming resin is any one or a few mixture in epoxy resin, acrylic resin, resol, vibrin.
9. nanoparticle super-hydrophobic self-cleaning wall paint as claimed in claim 6, is characterized in that, described auxiliary agent comprises linking agent, initiator and promotor; Described linking agent is any one or a few the mixture in vinylbenzene, methyl methacrylate or dially phthalate; Described initiator is any one or a few the mixture in Benzoyl Peroxide, methylethyl ketone peroxide, tertbutyl peroxide or isopropyl hydrogen peroxide; Described promotor is any one or a few the mixture in triethylamine, xylidine or Diethyl Aniline.
10. as the preparation method of the described nanoparticle super-hydrophobic self-cleaning of claim 6-9 any one wall paint, it is characterized in that, comprise the steps:
1), by the described hydrophobic nano-titanium dioxide of formula weighing, titanium dioxide, filler, film-forming resin, auxiliary agent and distilled water;
2), under normal temperature, titanium dioxide, filler are slowly added in distilled water, be stirred to even mixing, obtain mixture three;
3), in mixture one, slowly add film-forming resin and auxiliary agent, and be stirred to even mixing, obtain mixture four;
4), in mixture four, slowly add hydrophobic nano-titanium dioxide, and be stirred to even mixing, obtain described hydrophobic nano-titanium dioxide PHOTOCATALYTIC AIR-PURIFYING wall paint.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104017402A (en) * | 2014-05-23 | 2014-09-03 | 浙江鸿浩科技有限公司 | Flame retardation type exterior coating capable of automatically cleaning |
| CN104610787A (en) * | 2015-02-03 | 2015-05-13 | 安徽工业大学 | Neodymium aluminate nanowire multifunctional composite coating |
| CN104745025A (en) * | 2014-08-22 | 2015-07-01 | 赵杰 | Environment-friendly type multifunctional nano modified coating and spraying method thereof |
| CN105709404A (en) * | 2016-02-01 | 2016-06-29 | 浙江大学 | Drag-reducing and wear-resisting hydrophobic ski board |
| CN105907131A (en) * | 2016-04-27 | 2016-08-31 | 浙江工业大学 | Silane-modified titanium dioxide coating and application thereof |
| CN106554718A (en) * | 2016-11-29 | 2017-04-05 | 国网山东省电力公司电力科学研究院 | Phenolic resin integration super-amphiphobic anti-ultraviolet ageing coating and preparation method thereof |
| CN107057515A (en) * | 2017-06-01 | 2017-08-18 | 冯智勇 | A kind of red lead phenolic aldehyde protective paint coating |
| CN107189641A (en) * | 2017-07-25 | 2017-09-22 | 合肥嘉仕诚能源科技有限公司 | A kind of self-cleaning wall finiss of nano environmental protection and preparation method thereof |
| CN108822668A (en) * | 2018-06-04 | 2018-11-16 | 马爱连 | A kind of UV resistance hydrophobic coating agent and its preparation method and application |
| CN112250350A (en) * | 2020-09-30 | 2021-01-22 | 余明芳 | Preparation method of diatom ooze wall panel capable of self-cleaning and decontaminating |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017402A (en) * | 2014-05-23 | 2014-09-03 | 浙江鸿浩科技有限公司 | Flame retardation type exterior coating capable of automatically cleaning |
| CN104745025A (en) * | 2014-08-22 | 2015-07-01 | 赵杰 | Environment-friendly type multifunctional nano modified coating and spraying method thereof |
| CN104610787A (en) * | 2015-02-03 | 2015-05-13 | 安徽工业大学 | Neodymium aluminate nanowire multifunctional composite coating |
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| CN107189641A (en) * | 2017-07-25 | 2017-09-22 | 合肥嘉仕诚能源科技有限公司 | A kind of self-cleaning wall finiss of nano environmental protection and preparation method thereof |
| CN108822668A (en) * | 2018-06-04 | 2018-11-16 | 马爱连 | A kind of UV resistance hydrophobic coating agent and its preparation method and application |
| CN112250350A (en) * | 2020-09-30 | 2021-01-22 | 余明芳 | Preparation method of diatom ooze wall panel capable of self-cleaning and decontaminating |
| CN113201239A (en) * | 2021-04-30 | 2021-08-03 | 江苏理工学院 | Preparation method of biological adhesion-resistant super-hydrophobic suspension |
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