CN101987941A - Method for preparing nanometer hardened organic silicon coating - Google Patents
Method for preparing nanometer hardened organic silicon coating Download PDFInfo
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- CN101987941A CN101987941A CN2009101091651A CN200910109165A CN101987941A CN 101987941 A CN101987941 A CN 101987941A CN 2009101091651 A CN2009101091651 A CN 2009101091651A CN 200910109165 A CN200910109165 A CN 200910109165A CN 101987941 A CN101987941 A CN 101987941A
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Abstract
The invention provides a method for preparing a nanometer hardened organic silicon coating. The method is mainly characterized by comprising the following steps of: mixing ethyl orthosilicate, deionized water and various silane coupling agents (such as KH560, methyl triethoxysilane and the like) according to a proportion; adding absolute ethyl alcohol, stirring by using a magnetic stirrer, and adding an inorganic acid catalyst during the stirring; and heating and condensing the solution to obtain organic silicon composite coating solution. The solution can be used for coatings on the surface of substrates such as glass, metal, plastic and the like, and a coating is obtained by a pulling process. The obtained coating has high hardness, wear resistance and weather resistance and can be used for protecting the surface of various substrates. The method has the characteristics that: the preparation process is simple; and feasible and mass production can be realized.
Description
Technical field
The present invention relates to the preparation method of nanometer stiffened organic silicon coating, can be used for preparing the nano hybridization coating of high rigidity, belong to the organic-inorganic hybrid material field.
Background technology
Nanometer stiffened organic silicon coating can be widely used in ophthalmic lens, automobile front truck lampshade, dial of meter plate, CD and special building with surfaces such as window glasss, and substrate is protected, and has simultaneously to increase hard attrition resistant performance, prolongs the work-ing life of substrate.
Traditional material surface coating mainly is to be prepared from by resin synthetic coating such as aminoresin, urethane resin, Synolac, thermal-curable acrylic resin, resol, and main component is an organism.Coating generally has wear resistance and weathering resistance is poor, shortcomings such as non-refractory.Organic silicon coating is better than other organic polymers increasing on the hard wear resisting property, study morely both at home and abroad, all belongs to imported product but the high-performance of domestic present appearance increases hard wear-resistant paint, and domestic organic silicon rigidity-increasing dope performance is not good.Though the inorganic hard coat that increases has advantages such as high temperature resistant, anti-aging, but the deficiency that also exists at aspects such as shock resistance, visible light transmissivities.Organic and inorganic composite hybridization coating is that nano material is combined with traditional top coat technology, can obtain nano-composite coating.Advantage such as nano-composite coating has the hardness height, wear resistance is good, toughness is high, high temperature resistant, oxidation-resistance, corrosion prevention ability are good.
It is to adopt mechanical blending method or situ aggregation method that inorganic nano-particle is dispersed in coating or the resin that general nanoparticle is applied in resin and the coating, the nano-resin or the coating of this method preparation can not make the nanoparticle homodisperse, cause easily to be separated, little to the performance raising of coating or resin.And sol-gel method is by being precursor with inorganic salt or metal alkoxide, be dissolved in and form uniform solution in the solvent, add other component then, at a certain temperature, solute and solvent produce hydrolysis or alcoholysis reaction, reaction product is gathered into the particle about several nanometers and forms colloidal sol, and material requested is made in processing such as drying and sintering again.Organic and inorganic component in the hybrid material that this method obtains is through chemical bonding, and nothing is separated, and has very excellent thermotolerance, and simple to operate, and temperature of reaction is low, and energy consumption is low.Adopt sol-gel method with inorganic silica system and organosilane system bonding reaction, preparation nanometer composite organic material can realize that phase-splitting does not appear in matrix material, also can increase substantially the mechanical property of silicone resin.
The nanometer stiffened organic silicon coating of external report is more, adopt multiple organosilane monomer and tetraethoxy to carry out crosslinked as people such as Wu, add hard coat in the polycarbonate surface preparation, form firm chemical bond through polycarbonate surface and the hybrid coating of handling, increased adhesive force of coatings and stability, the hardness of coating reaches as high as 8H.Domestic organosilicon for nano modification adds hard coat report seldom, and performance with compare the external segment distance that also has.The Lu Jingjuan of Zhejiang University adopts sol-gel method with the condensation that is hydrolyzed of KH570 and tetraethoxy, the transparent wear-resistance thin film of preparation on the PC plate, coating has antireflective effect to substrate, pencil hardness is brought up to H～5H from B, hardness is along with the content of tetraethoxy increases, but inorganic component is too high, causes adhesive force of coatings to descend, and coating adhesion and hardness performance can not get both.
Summary of the invention
The technical issues that need to address of the present invention are the preparation methods that disclose a kind of nanometer stiffened organic silicon coating.
Method of the present invention comprises the steps:
Tetraethoxy, organosilane monomer and dehydrated alcohol are mixed, be heated to 80～100 ℃, the mixing solutions of dropping inorganic acid and deionized water under stirring condition, keep this temperature to reflux and stir the condensation reaction 60～600 minutes that is hydrolyzed, obtain transparent and uniform nanometer stiffened organic silicon sol.Adopt crystal pulling method to prepare coating.With coating standing and drying 10～30 minutes in air, put into baking oven then, treatment temp is 80～120 ℃, and heat treatment time is 30～120 minutes.
Described mineral acid is any of following mineral acid: hydrochloric acid or acetic acid;
Described organosilane monomer be a kind of among monomethyl triethoxyl silane, KH570 (γ-methacryloxypropyl trimethoxy silane) and the KH792 (N-β-(aminoethyl)-γ-An Bingjisanjiayangjiguiwan) or wherein two or more.
This shows that concrete enforcement divides two to go on foot greatly:
The first step is the preparation of nanometer stiffened organic silicon sol, and second step was the preparation of high hardness nanocomposite stiffened organic silicon coating.Now details are as follows respectively:
(1) preparation of organic silicon sol
Tetraethoxy, organosilane monomer and dehydrated alcohol are mixed, be heated to 80～100 ℃, the mixing solutions of dropping inorganic acid and deionized water under stirring condition, keep this temperature to reflux and stir the condensation reaction 60～600 minutes that is hydrolyzed, obtain transparent and uniform nanometer stiffened organic silicon sol.
(2) preparation of hard organosilicon coating
Nanometer stiffened organic silicon sol was left standstill 60～400 minutes, pour in the container and seal, after 12～24 hours, solution is used for coating.Coating adopts the crystal pulling method preparation, and pull rate is 5～20cm/ minute, and lifting number of times is 1～15 time, and lifting the gap is 1～10 minute.With coating standing and drying 10～30 minutes in air, put into heat treatment furnace then, temperature is 80～120 ℃, and heat treatment time is 30～120 minutes.
Ultimate principle of the present invention is as described below:
The characteristics of the making method of nanometer stiffened organic silicon coating provided by the invention are that KH570 contains three alkoxyl groups, the monomethyl triethoxyl silane contains three organoalkoxysilanes, when hydrolysis, hydroxyl on the siloxanes and the condensation of teos hydrolysis thing form and have rigidity and flexible network-like structure concurrently.Adopt the nano-organosilicon composite coating of method preparation of the present invention to have very high hardness, wear resistance and weather resisteant.Show that through experiment test the surperficial pencil hardness of nano-organosilicon composite coating sample is greater than 6H, erosion resistance is good.
Embodiment
Embodiment 1
Proportioning raw materials is: tetraethoxy 27 grams, KH570 (γ-methacryloxypropyl trimethoxy silane) 18 grams, dehydrated alcohol 100 grams, deionized water 10 grams, hydrochloric acid 0.1 gram.Use magnetic stirrer 60 minutes after mixing,, after 24 hours solution is heated to 80 ℃ and refluxed 120 minutes, continue heating, treat that being incubated 60 minutes after solution is warming up to 100 ℃ promptly gets nanometer stiffened organic silicon sol the mixing solutions sealing and standing.This colloidal sol is adopted the crystal pulling method coating preparation, and pull rate is 10cm/ minute, and lifting number of times is 10 times, and lifting the gap is 5 minutes.Then coating is put into baking oven and heat-treat, treatment temp is 80 ℃, and heat treatment time is 30 minutes.Show that after tested the coating pencil hardness is greater than 5H, sticking power and erosion resistance are good.
Embodiment 2
Proportioning raw materials is: tetraethoxy 27 grams, monomethyl triethoxyl silane 10 grams, KH570 (γ-methacryloxypropyl trimethoxy silane) 4 grams, dehydrated alcohol 100 grams, deionized water 10 grams, hydrochloric acid 0.1 gram.Use magnetic stirrer 60 minutes after mixing,, after 24 hours solution is heated to 80 ℃ and refluxed 120 minutes, continue heating, treat that being incubated 60 minutes after solution is warming up to 100 ℃ promptly gets nanometer stiffened organic silicon sol the mixing solutions sealing and standing.This colloidal sol is adopted the crystal pulling method coating preparation, and pull rate is 10cm/ minute, and lifting number of times is 10 times, and lifting the gap is 5 minutes.Then coating is put into baking oven and heat-treat, treatment temp is 80 ℃, and heat treatment time is 30 minutes.Show that after tested the coating pencil hardness is greater than 6H, sticking power and erosion resistance are good.
Embodiment 3
Proportioning raw materials is: tetraethoxy 27 grams, monomethyl triethoxyl silane 10 grams, KH570 (γ-methacryloxypropyl trimethoxy silane) 4 grams, dehydrated alcohol 100 grams, deionized water 10 grams, acetic acid 0.2 gram.Use magnetic stirrer 60 minutes after mixing,, after 24 hours solution is heated to 80 ℃ and refluxed 120 minutes, continue heating, treat that being incubated 60 minutes after solution is warming up to 100 ℃ promptly gets nanometer stiffened organic silicon sol the mixing solutions sealing and standing.This colloidal sol is adopted the crystal pulling method coating preparation, and pull rate is 10cm/ minute, and lifting number of times is 10 times, and lifting the gap is 5 minutes.Then coating is put into baking oven and heat-treat, treatment temp is 80 ℃, and heat treatment time is 30 minutes.Show that after tested the coating pencil hardness is greater than 6H, sticking power and erosion resistance are good.
Claims (9)
1. the preparation method of a nanometer stiffened organic silicon coating, it is characterized in that: tetraethoxy, organosilane monomer and dehydrated alcohol are mixed, be heated to 80～100 ℃, the mixing solutions of dropping inorganic acid and deionized water under stirring condition, keep this temperature to reflux and stir the condensation reaction 60～600 minutes that is hydrolyzed, obtain transparent and uniform nanometer stiffened organic silicon sol.This colloidal sol can be used for the coating of substrate surfaces such as glass, metal, plastics, obtains coating by crystal pulling method.The coating that is obtained has very high hardness, wear resistance and weather resisteant, can be used for the protection of multiple substrate surface.Present method has preparation technology's simple possible, the characteristics that can be mass-produced.
2. according to the described preparation method of claim 1, it is characterized in that: the mass ratio of the synthesis material tetraethoxy of preparation nanometer stiffened organic silicon sol is 40%～65%.
3. according to the described preparation method of claim 1, it is characterized in that: the synthesis material of preparation nanometer stiffened organic silicon sol adopts organosilane monomer, comprise a kind of among monomethyl triethoxyl silane, KH570 (γ-methacryloxypropyl trimethoxy silane) or the KH792 (N-β-(aminoethyl)-γ-An Bingjisanjiayangjiguiwan) or wherein two or more, and deionized water.Wherein the mass ratio of monomethyl triethoxyl silane is 0%～40%, the mass ratio of KH570 (γ-methacryloxypropyl trimethoxy silane) is 5%～50%, the mass ratio of KH792 (N-β-(aminoethyl)-γ-An Bingjisanjiayangjiguiwan) is 0%～20%, and deionized water quality ratio is 5%～35%.
4. according to the described preparation method of claim 1, it is characterized in that: it is catalyzer that preparation nanometer stiffened organic silicon sol adopts mineral acid, and the mineral acid of interpolation is following any: hydrochloric acid or acetic acid, its consumption accounts for 0.1%～3% of total amount ratio.The pH value scope is controlled at 4～8.
5. according to the described preparation method of claim 1, it is characterized in that: preparation nanometer stiffened organic silicon sol solvent adopts dehydrated alcohol, and the consumption of dehydrated alcohol is tetraethoxy and various silane coupling agent total amounts 1～100 times.
6. according to the described preparation method of claim 1, it is characterized in that: preparation nanometer stiffened organic silicon sol temperature of reaction is 80～100 ℃, and the reaction times is 60～600 minutes.
7. according to the described preparation method of claim 1, it is characterized in that: nanometer stiffened organic silicon sol was left standstill 60～400 minutes, pour in the container and seal, after 12～24 hours, colloidal sol is used for coating.
8. according to the described preparation method of claim 1, it is characterized in that: preparation nanometer stiffened organic silicon coating adopts the crystal pulling method preparation, and pull rate is 5～20cm/ minute, and lifting number of times is 1～15 time, and lifting the gap is 1～10 minute.
9. according to the described preparation method of claim 1, it is characterized in that: preparation nanometer stiffened organic silicon coating is through Temperature Treatment, and temperature is 80～120 ℃, and heat treatment time is 30～120 minutes.
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| CN102703089A (en) * | 2012-05-28 | 2012-10-03 | 广州市翰瑞文物保护设计研究中心 | Organic silicon modified composite material for reinforcing and protecting site soil in damp environment, and preparation method of organic silicon modified composite material |
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Application publication date: 20110323 |