CN106467706A - A kind of preparation method of environmentally friendly organic inorganic hybridization preservative protective film - Google Patents

A kind of preparation method of environmentally friendly organic inorganic hybridization preservative protective film Download PDF

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Publication number
CN106467706A
CN106467706A CN201610841918.8A CN201610841918A CN106467706A CN 106467706 A CN106467706 A CN 106467706A CN 201610841918 A CN201610841918 A CN 201610841918A CN 106467706 A CN106467706 A CN 106467706A
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protective film
preparation
environmentally friendly
mass ratio
silsesquioxane
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王文庆
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a kind of preparation method of environmentally friendly organic inorganic hybridization preservative protective film, the mixture initially with sol-gal process hydrolytic condensation γ aminopropyl triethoxysilane, tetraethyl orthosilicate to prepare SiO2Silsesquioxane, then to SiO2Silsesquioxane system in add ethanol, initiator and ATMP, after mix homogeneously, size according to film thing using the coating method of leaching film, spraying or brushing, then solidifies 5 10h at 100 120 DEG C, obtains organic inorganic hybridization preservative protective film.The protecting film that the present invention is obtained, wear-resisting scratch resistance performance is good, excellent anti-corrosion performance, and antiseptic property is good, and mechanical property is good, nontoxic, and preparation method is simple, low cost.

Description

A kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film
Technical field：
The present invention relates to technical field of material, it is specifically related to a kind of environmentally friendly hybrid inorganic-organic anti-corrosion The preparation method of protecting film.
Background technology：
With scientific and technical development, people's also more and more higher of the requirement to material, different types of material is passed through one Fixed process makes composite, it can be made to retain the advantage of original component, overcome the deficiency, and show some new property Energy.Inorganic-Organic Hybrid Material combines the good characteristic of inorganic material and organic material, is a kind of uniform heterogeneous material, In nanoscale, nanometer is alternate with other (covalent bond, to be joined at least one dimension of size that wherein must have a phase by chemistry Position key) act on physics (hydrogen bond etc.), compound on nanometer level.Inorganic-Organic Hybrid Material has the little chi of nano material The properties such as very little effect, skin effect, quantum size effect.In addition, the form of this material and performance can be in sizable scopes Interior regulation, makes the performance of material assume variation.
Inorganic-Organic Hybrid Material is primarily present following shortcoming at present：(1) nano-particle specific surface area is big, in system Easily reunite, dispersion is poor, thus losing its nano-meter characteristic；(2) the Inorganic-Organic Hybrid Material corrosion resistance being obtained Energy, antiseptic property are poor.
Content of the invention：
It is an object of the invention to provide a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film, should The preservative protective film corrosion resistance and good that method is obtained, heat-resistant antifriction excellent performance, excellent in mechanical performance, hardening time is short, nontoxic, And preparation method is simple, low cost.
For achieving the above object, the present invention employs the following technical solutions：
A kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film, comprises the following steps：
(1) SiO is prepared using sol-gal process2Silsesquioxane, sequentially add γ-ammonia first in organic solvent Propyl-triethoxysilicane, tetraethyl orthosilicate, after being uniformly mixed, are warming up to 30-60 DEG C, Deca citric acid and glacial acetic acid Mixture, continue reaction, in course of reaction, its mean molecule quantity surveyed using gel chromatography, determine and generate SiO2Sesquialter silicon Oxygen alkane；
(2) SiO being obtained to step (1)2Silsesquioxane system in add ethanol, initiator to stir after, so Add ATMP afterwards, be uniformly mixed, then the size according to membrane attached matter is using the painting of leaching film, spraying or brushing Embrane method, then solidifies 5-10h at 100-120 DEG C, obtains hybrid inorganic-organic preservative protective film.
Preferred as technique scheme, in step (1), described organic solvent be acetone, oxolane, dimethylbenzene, One or more of ethanol, ethyl acetate mix.
Preferred as technique scheme, in step (1), described gamma-aminopropyl-triethoxy-silane, positive silicic acid tetrem The mass ratio of ester is (5-15)：1.
Preferred as technique scheme, in step (1), described organic solvent and gamma-aminopropyl-triethoxy-silane, The mass ratio of tetraethyl orthosilicate mixture is (2-8)：1.
Preferred as technique scheme, in step (1), in the mixture of described citric acid and glacial acetic acid, citric acid Mass ratio with glacial acetic acid is 1：(3-5).
Preferred as technique scheme, in step (1), described citric acid, the mixture of glacial acetic acid and organic solvent Mass ratio be (0.05-0.1)：1.
Preferred as technique scheme, in step (2), described ethanol, ATMP, SiO2 silsesquioxane Alkane, the mass ratio of initiator are (8-15)：(1-2)：3:1.
Preferred as technique scheme, in step (2), described initiator is di-cyclohexylperoxy di-carbonate, mistake Oxidation (2 ethyl hexanoic acid) tert-butyl ester, benzoyl peroxide, double (3,5,5- trimethyl -1- oxo-hexyl) peroxide, peroxide Change the mixing of one or more of benzoic acid tert-butyl ester.
Compared with prior art, the present invention has advantages below：
The present invention carrys out the mixing of hydrolytic condensation gamma-aminopropyl-triethoxy-silane, tetraethyl orthosilicate in sol-gal process During thing, the mixture of appropriate Deca citric acid and glacial acetic acid, and rationally control the consumption of the two, effectively facilitate γ-ammonia The hydrolysis property of propyl-triethoxysilicane, substantially reduces the response time, prepared SiO2Silsesquioxane stable system Property is good；
The present invention adds appropriate ATMP in the treatment fluid before film, effectively increases its film Can, the protecting film decay resistance obtaining is more excellent, and Wear-resistant scratch-resistant performance is good, and this preparation method is simple, low production cost.
Specific embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving Release the present invention, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film, comprises the following steps：
(1) SiO is prepared using sol-gal process2Silsesquioxane, sequentially add γ-aminopropyl first in acetone Triethoxysilane, tetraethyl orthosilicate, after being uniformly mixed, are warming up to 45 DEG C, the mixing of Deca citric acid and glacial acetic acid Thing, continues reaction, surveys its mean molecule quantity using gel chromatography in course of reaction, determines and generates SiO2Silsesquioxane, Wherein, gamma-aminopropyl-triethoxy-silane, the mass ratio of tetraethyl orthosilicate are 5：1, acetone and gamma-aminopropyl-triethoxy Silane, the mass ratio of tetraethyl orthosilicate mixture are 2：1, in the mixture of citric acid and glacial acetic acid, citric acid and glacial acetic acid Mass ratio be 1：3, the mass ratio of citric acid, the mixture of glacial acetic acid and organic solvent is 0.05：1；
(2) SiO being obtained to step (1)2Silsesquioxane system in add ethanol, di-cyclohexylperoxy di-carbonate After stirring, be subsequently adding ATMP, be uniformly mixed, then according to the size of membrane attached matter using leaching film, Spraying or the coating method brushed, then solidify 10h at 100 DEG C, obtain hybrid inorganic-organic preservative protective film, wherein, ethanol, ATMP, SiO2 silsesquioxane, the mass ratio of di-cyclohexylperoxy di-carbonate are 8：1：3:1.
Embodiment 2
A kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film, comprises the following steps：
(1) SiO is prepared using sol-gal process2Silsesquioxane, sequentially add γ-ammonia first in oxolane Propyl-triethoxysilicane, tetraethyl orthosilicate, after being uniformly mixed, are warming up to 60 DEG C, Deca citric acid and glacial acetic acid Mixture, continues reaction, surveys its mean molecule quantity using gel chromatography in course of reaction, determines and generates SiO2Silsesquioxane Alkane, wherein, gamma-aminopropyl-triethoxy-silane, the mass ratio of tetraethyl orthosilicate are 15：1, oxolane and γ-aminopropyl Triethoxysilane, the mass ratio of tetraethyl orthosilicate mixture are 8：1, in the mixture of citric acid and glacial acetic acid, citric acid Mass ratio with glacial acetic acid is 1：5, the mass ratio of citric acid, the mixture of glacial acetic acid and organic solvent is 0.1：1；
(2) SiO being obtained to step (1)2Silsesquioxane system in add ethanol, peroxidating (2 ethyl hexanoic acid) uncle After butyl ester stirs, it is subsequently adding ATMP, is uniformly mixed, then the size according to membrane attached matter is using leaching The coating method of film, spraying or brushing, then solidifies 5h at 120 DEG C, obtains hybrid inorganic-organic preservative protective film, wherein, second Alcohol, ATMP, SiO2 silsesquioxane, the mass ratio of peroxidating (2 ethyl hexanoic acid) tert-butyl ester are 15：2：3:1.
Embodiment 3
A kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film, comprises the following steps：
(1) SiO is prepared using sol-gal process2Silsesquioxane, sequentially add γ-ammonia third first in dimethylbenzene Ethyl triethoxy silicane alkane, tetraethyl orthosilicate, after being uniformly mixed, are warming up to 50 DEG C, and Deca citric acid is mixed with glacial acetic acid Compound, continues reaction, surveys its mean molecule quantity using gel chromatography in course of reaction, determines and generates SiO2Silsesquioxane Alkane, wherein, gamma-aminopropyl-triethoxy-silane, the mass ratio of tetraethyl orthosilicate are 7：1, dimethylbenzene and γ-aminopropyl three second TMOS, the mass ratio of tetraethyl orthosilicate mixture are 4：1, in the mixture of citric acid and glacial acetic acid, citric acid and ice The mass ratio of acetic acid is 1：3.5, the mass ratio of citric acid, the mixture of glacial acetic acid and organic solvent is 0.06：1；
(2) SiO being obtained to step (1)2Silsesquioxane system in add ethanol, benzoyl peroxide to stir Afterwards, it is subsequently adding ATMP, is uniformly mixed, then the size according to membrane attached matter is using leaching film, spraying or brush The coating method applying, then solidifies 6h at 105 DEG C, obtains hybrid inorganic-organic preservative protective film, wherein, ethanol, amino three methene Phosphonic acids, SiO2 silsesquioxane, the mass ratio of benzoyl peroxide are 10：1.2：3:1.
Embodiment 4
A kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film, comprises the following steps：
(1) SiO is prepared using sol-gal process2Silsesquioxane, sequentially add γ-aminopropyl first in ethanol Triethoxysilane, tetraethyl orthosilicate, after being uniformly mixed, are warming up to 50 DEG C, the mixing of Deca citric acid and glacial acetic acid Thing, continues reaction, surveys its mean molecule quantity using gel chromatography in course of reaction, determines and generates SiO2Silsesquioxane, Wherein, gamma-aminopropyl-triethoxy-silane, the mass ratio of tetraethyl orthosilicate are 9：1, ethanol and gamma-aminopropyl-triethoxy Silane, the mass ratio of tetraethyl orthosilicate mixture are 5：1, in the mixture of citric acid and glacial acetic acid, citric acid and glacial acetic acid Mass ratio be 1：4, the mass ratio of citric acid, the mixture of glacial acetic acid and organic solvent is 0.07：1；
(2) SiO being obtained to step (1)2Silsesquioxane system in add ethanol, double (3,5,5- trimethyl -1- oxygen For hexyl) after peroxide stirs, it is subsequently adding ATMP, is uniformly mixed, then according to membrane attached matter Size using the coating method of leaching film, spraying or brushing, then solidify 7h at 110 DEG C, obtain hybrid inorganic-organic anti-corrosion protection Film, wherein, ethanol, ATMP, SiO2 silsesquioxane, double (3,5,5- trimethyl -1- oxo-hexyl) peroxidating The mass ratio of thing is 12：1.4：3:1.
Embodiment 5
A kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film, comprises the following steps：
(1) SiO is prepared using sol-gal process2Silsesquioxane, sequentially add γ-ammonia first in ethyl acetate Propyl-triethoxysilicane, tetraethyl orthosilicate, after being uniformly mixed, are warming up to 55 DEG C, Deca citric acid and glacial acetic acid Mixture, continues reaction, surveys its mean molecule quantity using gel chromatography in course of reaction, determines and generates SiO2Silsesquioxane Alkane, wherein, gamma-aminopropyl-triethoxy-silane, the mass ratio of tetraethyl orthosilicate are 11：1, ethyl acetate and γ-aminopropyl Triethoxysilane, the mass ratio of tetraethyl orthosilicate mixture are 6：1, in the mixture of citric acid and glacial acetic acid, citric acid Mass ratio with glacial acetic acid is 1：4.5, the mass ratio of citric acid, the mixture of glacial acetic acid and organic solvent is 0.08：1；
(2) SiO being obtained to step (1)2Silsesquioxane system in add ethanol, perbenzoic acid tributyl After stirring, be subsequently adding ATMP, be uniformly mixed, then according to the size of membrane attached matter using leaching film, Spraying or the coating method brushed, then solidify 8h at 115 DEG C, obtain hybrid inorganic-organic preservative protective film, wherein, ethanol, ammonia Base three methylenephosphonic acid, SiO2 silsesquioxane, the mass ratio of perbenzoic acid tributyl are 13：1.8：3:1.
Embodiment 6
A kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film, comprises the following steps：
(1) SiO is prepared using sol-gal process2Silsesquioxane, sequentially add γ-ammonia first in ethyl acetate Propyl-triethoxysilicane, tetraethyl orthosilicate, after being uniformly mixed, are warming up to 60 DEG C, Deca citric acid and glacial acetic acid Mixture, continues reaction, surveys its mean molecule quantity using gel chromatography in course of reaction, determines and generates SiO2Silsesquioxane Alkane, wherein, gamma-aminopropyl-triethoxy-silane, the mass ratio of tetraethyl orthosilicate are 13：1, organic solvent and γ-aminopropyl Triethoxysilane, the mass ratio of tetraethyl orthosilicate mixture are 7：1, in the mixture of citric acid and glacial acetic acid, citric acid Mass ratio with glacial acetic acid is 1：5, the mass ratio of citric acid, the mixture of glacial acetic acid and organic solvent is 0.09：1；
(2) SiO being obtained to step (1)2Silsesquioxane system in add ethanol, double (3,5,5- trimethyl -1- oxygen For hexyl) after peroxide stirs, it is subsequently adding ATMP, is uniformly mixed, then according to membrane attached matter Size using the coating method of leaching film, spraying or brushing, then solidify 5-10h at 100-120 DEG C, obtain hybrid inorganic-organic Preservative protective film, wherein, ethanol, ATMP, SiO2 silsesquioxane, double (3,5,5- trimethyl -1- oxos oneself Base) peroxide mass ratio be 13：1.8：3:1.

Claims (8)

1. a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film is it is characterised in that include following walking Suddenly：
(1) SiO is prepared using sol-gal process2Silsesquioxane, sequentially add γ-aminopropyl first in organic solvent Triethoxysilane, tetraethyl orthosilicate, after being uniformly mixed, are warming up to 30-60 DEG C, and Deca citric acid is mixed with glacial acetic acid Compound, continues reaction, surveys its mean molecule quantity using gel chromatography in course of reaction, determines and generates SiO2Silsesquioxane Alkane；
(2) SiO being obtained to step (1)2Silsesquioxane system in add ethanol, initiator to stir after, be subsequently adding ATMP, is uniformly mixed, and then the size according to membrane attached matter adopts the coating method of leaching film, spraying or brushing, Then solidify 5-10h at 100-120 DEG C, obtain hybrid inorganic-organic preservative protective film.
2. a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film as claimed in claim 1, its feature It is：In step (1), described organic solvent is one or more of acetone, oxolane, dimethylbenzene, ethanol, ethyl acetate Mixing.
3. a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film as claimed in claim 1, its feature It is：In step (1), described gamma-aminopropyl-triethoxy-silane, the mass ratio of tetraethyl orthosilicate are (5-15)：1.
4. a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film as claimed in claim 1, its feature It is：In step (1), described organic solvent and gamma-aminopropyl-triethoxy-silane, the mass ratio of tetraethyl orthosilicate mixture For (2-8)：1.
5. a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film as claimed in claim 1, its feature It is：In step (1), in the mixture of described citric acid and glacial acetic acid, citric acid is 1 with the mass ratio of glacial acetic acid：(3-5).
6. a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film as claimed in claim 1, its feature It is：In step (1), the mass ratio of described citric acid, the mixture of glacial acetic acid and organic solvent is (0.05-0.1)：1.
7. a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film as claimed in claim 1, its feature It is：In step (2), described ethanol, ATMP, SiO2 silsesquioxane, the mass ratio of initiator are (8-15)： (1-2)：3:1.
8. a kind of preparation method of environmentally friendly hybrid inorganic-organic preservative protective film as claimed in claim 1, its feature It is：In step (2), described initiator is di-cyclohexylperoxy di-carbonate, peroxidating (2 ethyl hexanoic acid) tert-butyl ester, peroxide Change one of benzoyl, double (3,5,5- trimethyl -1- oxo-hexyl) peroxide, perbenzoic acid tributyl or many Plant mixing.
CN201610841918.8A 2016-09-21 2016-09-21 A kind of preparation method of environmentally friendly organic inorganic hybridization preservative protective film Pending CN106467706A (en)

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CN107418374A (en) * 2017-07-24 2017-12-01 杨洁磊 A kind of preparation method of anticorrosive metal epoxy coating
CN110669222A (en) * 2019-09-02 2020-01-10 武汉华星光电半导体显示技术有限公司 Optically transparent material and preparation method thereof, polymer film and manufacturing method thereof

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CN107418374A (en) * 2017-07-24 2017-12-01 杨洁磊 A kind of preparation method of anticorrosive metal epoxy coating
CN110669222A (en) * 2019-09-02 2020-01-10 武汉华星光电半导体显示技术有限公司 Optically transparent material and preparation method thereof, polymer film and manufacturing method thereof
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