CN107325716A - A kind of solvent-borne type tin-antiomony oxide transparent heat insulating dope composition and its preparation method and application - Google Patents
A kind of solvent-borne type tin-antiomony oxide transparent heat insulating dope composition and its preparation method and application Download PDFInfo
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- CN107325716A CN107325716A CN201610283662.3A CN201610283662A CN107325716A CN 107325716 A CN107325716 A CN 107325716A CN 201610283662 A CN201610283662 A CN 201610283662A CN 107325716 A CN107325716 A CN 107325716A
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- solvent
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- transparent heat
- tin
- heat insulating
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K3/2279—Oxides; Hydroxides of metals of antimony
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/004—Reflecting paints; Signal paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2231—Oxides; Hydroxides of metals of tin
Abstract
The present invention relates to a kind of solvent-borne type tin-antiomony oxide transparent heat insulating dope composition and its preparation method and application, the solvent-borne type tin-antiomony oxide transparent heat insulating dope composition is made up of the nano antimony tin oxide slurry of 40~60 parts by weight and the solvent-borne type hybrid organic silicon resin of 40~60 parts by weight；The nano antimony tin oxide slurry of every 100 parts by weight includes nano antimony tin oxide powder, the dispersant of 1~6 parts by weight of 5~30 parts by weight, and surplus is alcoholic solvent；The solvent-borne type hybrid organic silicon resin is at least one of polyester modified organic silicon resin, phenol aldehyde modified organic siliconresin.Preparation technology of the present invention is simple, with low cost and environmental protection nonhazardous, it is adaptable to which factory mass produces.
Description
Technical field
The present invention relates to a kind of high rigidity, the solvent-borne type transparent heat insulating dope composition of high adhesion force, more particularly to contain
The preparation method of the transparent heat insulating dope of tin-antiomony oxide.
Background technology
With the increasingly depleted of global non-renewable energy especially oil and coal, save increasingly by global concern.
Large area uses windowpane and glass curtain wall so that the ratio that building energy consumption accounts for social total energy consumption is greatly increased therewith.China builds
Energy consumption in social total energy consumption proportion up to 30%.Root will be it was predicted that within following very short time, China's building energy consumption will increase
Grow to more than 35%.Building energy conservation has become the key subjects that China or even countries in the world are paid close attention to jointly, is that economic society can be held
The important leverage of supervention exhibition.In addition, with the lifting of people's living standard, the popularity rate of automobile also more and more higher, except
Outside to a large amount of consumption of the non-renewable resources such as oil, the environmental pollution brought is gradually obvious to the influence of society, such as this year
The problem of haze that everybody pays close attention to, a part of reason is vehicle exhaust.
Windowpane plays conclusive work as the main thoroughfare of energy exchange between human lives area and the external world to energy-conservation
With.The heat of common building about 40% is the exchange by window and extraneous progress, and is come for automobile and big curtain wall
Say, its proportion can be higher.But with the higher and higher demand to quality of life of people, window areas is raw in building etc.
Proportion shared by region living is by more and more higher, and how in the case where not influenceing glass window daylighting degree, reduction passes through window generation
Energy resource consumption turns into the emphasis of energy-conservation and environmental protection.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of high rigidity, high adhesion force solvent-borne type transparent heat insulating dope
Composition.
The invention provides a kind of solvent-borne type tin-antiomony oxide transparent heat insulating dope, the solvent-borne type tin-antiomony oxide is transparent heat-insulated to be applied
Feed composition is by the nano antimony tin oxide slurry of 40-60 parts by weight and the solvent-borne type hybrid organic silicon resin group of 40-60 parts by weight
Into；
The nano antimony tin oxide slurry of every 100 parts by weight includes the nano antimony tin oxide powder of 5-30 parts by weight, 1~6 parts by weight
Dispersant, surplus is alcoholic solvent；
The solvent-borne type hybrid organic silicon resin is at least one of polyester modified organic silicon resin, phenol aldehyde modified organic siliconresin.
Tin-antiomony oxide has the good transparency and spectral selection, is all widely used in transparent heat insulating dope all the time
Preparation in.The patent No. CN101108946, CN102559025A, CN104231909A, CN104556727A etc. are
Tin-antiomony oxide is applied and is described in detail in insulating moulding coating, but do not refer to the heat-proof quality of its insulating moulding coating, hardness and
The specific targets of adhesive force.The present invention carries out water proof guarantor using the solvent-borne type film forming agent with high-wearing feature to tin-antiomony oxide material
Shield, while film layer has very high intensity after film forming, can directly be coated on the transparent substrates such as glass surface, with good resistance to
Time property and wearability.Tin-antiomony oxide material has good dispersion effect in coating, it is ensured that can have good thermal insulation after film
Energy.
It is preferred that the particle diameter of the nano antimony tin oxide powder is 1-20nm, preferably 10nm.
It is preferred that the dispersant is a kind of cationic wetting dispersing agent (EFKA5010), the alkanol of block interpolymers
At least one of base ammonium salt.
It is preferred that the alcoholic solvent is at least one of absolute ethyl alcohol, isopropanol, n-butanol, ethyl acetate.
It is preferred that the solid content of the solvent-borne type hybrid organic silicon resin is 30-50%, solvent is ethanol, n-butanol, third
At least one of glycol methyl ether etc..
The present invention also additionally provides a kind of preparation method of above-mentioned solvent-borne type tin-antiomony oxide transparent heat insulating dope composition, including：
Add the nano antimony tin oxide powder after the dispersant is dissolved in the alcoholic solvent, it is ultrasonically treated after again ball-milling treatment obtain
To the nano antimony tin oxide slurry；
Gained nano antimony tin oxide slurry is saturating by the solvent-borne type tin-antiomony oxide is obtained after uniform mix with solvent-borne type hybrid organic silicon resin
Bright composition of insulating mold coating.
The present invention also additionally provides a kind of solvent-borne type tin-antiomony oxide transparent heat insulation diaphragm, transparent by above-mentioned solvent-borne type tin-antiomony oxide
Composition of insulating mold coating is coated on transparent substrates by spin-coating method or bar method, and the solvent-borne type tin-antiomony oxide is made in drying, cooling
Transparent heat insulation diaphragm.
It is preferred that the drying is to be incubated 20-50 minutes at 150-200 DEG C.
Can be applied to pass through solar energy or reflect of the present invention has the field of regulatory demand, include but are not limited to automobile and
The window of building, glass curtain wall, speculum etc..Technological merit is：Preparation technology is simple, with low cost and environmental protection
Nonhazardous, it is adaptable to which factory mass produces.After the coating film that the present invention is obtained in visible light transmissivity more than 77%,
Near-infrared rejection rate can reach more than 80%.The solar energy regulation and control efficiency high of film layer, coating hardness is higher (typically can reach 6H
More than), 0 grade of adhesive force, durability of coating is good, the prospect for having industrialized production.
Brief description of the drawings
Fig. 1 schemes for the TEM of ATO nano-powders；
Fig. 2 schemes for the TEM of nano antimony tin oxide slurry；
Fig. 3 is the preparation flow figure of solvent-borne type tin-antiomony oxide transparent heat insulating dope and film；
Fig. 4 is to pass through solvent-borne type tin-antiomony oxide transparent heat insulation diaphragm made from the nano antimony tin oxide slurry of different ATO powders solid contents
H103 resin；
Fig. 5 is the optics H103 resin of the solvent-borne type tin-antiomony oxide transparent heat insulation diaphragm of different wet-film thickness.
Embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this hair
It is bright, it is not intended to limit the present invention.
The present invention is raw material using tin-antiomony oxide, adds the alcoholic solvent acquisition nano antimony tin oxide for being dispersed with dispersant in advance
Slurry, then with solvent-borne type tin-antiomony oxide transparent heat insulating dope group is made as the solvent-borne type hybrid organic silicon mixed with resin of film forming agent
Compound can be used for prepares coating.Using the formula total amount of composition as 100 parts of agent, film forming matter can be 40-60 parts, tin-antiomony oxide slurry
It can be 40-60 parts.The film forming matter can be solvent-borne type hybrid organic silicon resin.Tin-antiomony oxide slurry can be wrapped by 100 parts of weight ratios
Include 5-30 parts of nano antimony tin oxide powders, 1-6 parts of dispersants, remaining be what alcoholic solvent was made.
Preparation method technique of the present invention is simple, and cost is relatively low, and environmental protection nonhazardous, it is adaptable to which factory gives birth on a large scale
Production.Illustrate to following exemplary the preparation method for the solvent-borne type tin-antiomony oxide transparent heat insulating dope composition that the present invention is provided, signal
Flow chart can be found in Fig. 3.
The preparation of nano antimony tin oxide slurry.Mass fraction according to nano antimony tin oxide powder, dispersant, alcoholic solvent claims
Content of starting materials, ultrasonically treated rear ball milling mixing obtains nano antimony tin oxide slurry.The present invention can refer to Fig. 3, first by dispersant and alcohol
Property solvent (for example, absolute ethyl alcohol) be prepared into ethanol solution, after again with nano antimony tin oxide powder (ATO powders) ultrasound
Ball milling mixing obtains nano antimony tin oxide slurry (ATO slurries) after processing.Referring to Fig. 1, it is known that nano antimony tin oxide powder can
For nanoscale, its particle diameter can be 1-20nm, preferably 10nm, and nano level ATO powders are more beneficial for it to visible ray
Through.First dispersant is uniformly dispersed in alcoholic solution and is conducive to ATO powders further disperseing in the solution.Dispersant can
Elect the conventional oxide powder of industry as and disperse surface modifier in oleaginous system, for example, can be a kind of cationic wetting dispersing agent
(EFKA5010), at least one of silane alcohol base ammonium salt of block interpolymers.It can be seen from Fig. 2, nanometer after slurry is prepared into
Tin-antiomony oxide diameter of particle is essentially unchanged, it is seen that the selection of dispersant causes nano antimony tin oxide powder to be uniformly dispersed, soilless sticking or
Block is present.Alcoholic solvent can be but be not limited only at least one of absolute ethyl alcohol, isopropanol, n-butanol, ethyl acetate.
As a detailed example, Step 1: 0.05-0.30g dispersants are added in 5g alcohol solvents, and stir
Uniformly.Step 2: 0.25-1.5g nano antimony tin oxide powders are added in stirring in above-mentioned solution, ultrasonic machine is subsequently placed in
Middle ultrasonic 3h.A few hours are sanded Step 3: being placed under 2500r/min rotating speeds, tin-antiomony oxide dispersion liquid is made.
The preparation of solvent-borne type tin-antiomony oxide transparent heat insulating dope composition.Gained nano antimony tin oxide slurry and solvent-borne type is miscellaneous
Change and the solvent-borne type tin-antiomony oxide transparent heat insulating dope combination is obtained after organic siliconresin is uniformly mixed according to mass fraction or percentage
Thing.The solvent-borne type hybrid organic silicon resin can be at least one in polyester modified organic silicon resin, phenol aldehyde modified organic siliconresin
Kind.The solid content of solvent-borne type hybrid organic silicon resin can be 30-50%, and solvent can be ethanol, n-butanol, propylene glycol monomethyl ether etc.
At least one of.As a detailed example, by tin-antiomony oxide dispersion liquid obtained above and modified organic silicone resin (or
Claim hybrid organic silicon resin, such as polyester modified organic silicon resin) with mass ratio 1：1 is well mixed, set aside for use.
Solvent-borne type tin-antiomony oxide transparent heat insulating dope is coated on transparent substrates, wet film by the present invention by spin-coating method or bar method
Thickness can be 2~30 μm, then be cooled to room temperature after being dried, and the transparent heat-insulated coating of solvent-borne type tin-antiomony oxide, film is made
Coating can be 0.1-1.5 μm.Wherein drying can be to be incubated 20-50 minutes at 150-200 DEG C.
As a detailed example, glass substrate is cleaned：By substrate of glass successively in deionized water, acetone, alcohol
Ultrasound ten minutes, is dried stand-by.Using bar method or spin-coating method film, dry, hardening.
The present invention measures film hardness by pencil hardometer.Film mist is measured by ultraviolet-visible-near infrared spectrometer
Degree, film visible light transmissivity, film near-infrared rejection rate.Adhesive force is measured by hundred lattice devices.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this hair
It is bright to be further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential modifications and adaptations that the above is made belong to protection scope of the present invention.Following specific technique ginsengs of example
Number etc. is also only an example in OK range, i.e. those skilled in the art can be done in suitable scope by this paper explanation
Selection, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
The preparation method of solvent-borne type tin-antiomony oxide transparent heat insulating dope composition is carried out in the steps below in this experiment method：
1) prepared by tin-antiomony oxide slurry：0.3g dispersants (EFKA5010) are dissolved in 5g ethanol and stirred, then 1.5g is received
Added in the powder stirring of rice tin-antiomony oxide, tin-antiomony oxide dispersion liquid is then both obtained after ultrasound 3h, 2500r/min ball milling a few hours
(solid content is 30wt%)；Use similar approach that solid content is made to treat for 5wt%, 10wt%, 20wt% tin-antiomony oxide slurry
With；
3g tin-antiomony oxide slurry (30wt%), 3g polyester modified organic silicon resins (solid content 50wt%) are mixed,
And 20min is stirred, obtain solvent-borne type transparent heat insulating dope composition；
The tin-antiomony oxide slurry replacement solid content that 5wt%, 10wt%, 20wt% is respectively adopted is made for 30wt% tin-antiomony oxide slurry
Coating composition is standby.
The preparation method of transparent heat-insulated coating：First by the substrate of glass successively ultrasound ten in deionized water, acetone, alcohol
Minute, after cleaning up, use solid content above-mentioned composition made from 30wt% tin-antiomony oxide slurry to be made using bar method
Wet-film thickness is respectively 2 μm, 10 μm, 15 μm, 22 μm, 30 μm of wet film, is placed in baking oven is warming up to afterwards
Be incubated after 150-200 DEG C, be cooled to room temperature, coating is made, coating layer thickness is respectively 0.1 μm, 0.5 μm, 0.75 μm,
1.1μm、1.5μm；
The Specifeca tion speeification of this experiment method product：
| Project | Performance |
| State in container | It is in uniform shape without lump, after stirring |
| Low-temperature stability | Never degenerate |
| Appearance of film | Normally |
| Drying temperature | 150-200℃ |
| Drying time | 20-50min |
| Hardness | More than 5H |
| Film mist degree (%) | ≤1 |
| Visible light transmissivity (%) | ≥90 |
| Near-infrared rejection rate (%) | ≥80 |
| Adhesive force | 0 grade |
Fig. 4 is transparent heat-insulated thin by solvent-borne type tin-antiomony oxide made from the nano antimony tin oxide slurry of different ATO solid contents
The H103 resin of film, with the raising of solid content, coating is gradually lifted to the rejection rate of near infrared region, it is seen that light transmission rate influences
It is smaller.Fig. 5 is the optics H103 resin of the transparent heat-insulated coating of solvent-borne type tin-antiomony oxide of different wet-film thickness, it can be seen that this hair
During visible light transmissivity more than 77% of bright obtained solvent-borne type tin-antiomony oxide transparent heat insulation diaphragm, infrared barrier rate be 80% with
On.
Claims (8)
1. a kind of solvent-borne type tin-antiomony oxide transparent heat insulating dope composition, it is characterised in that the solvent-borne type tin-antiomony oxide transparent heat insulating dope composition is made up of the nano antimony tin oxide slurry of 40~60 parts by weight and the solvent-borne type hybrid organic silicon resin of 40~60 parts by weight；
The nano antimony tin oxide slurry of every 100 parts by weight includes nano antimony tin oxide powder, the dispersant of 1~6 parts by weight of 5~30 parts by weight, and surplus is alcoholic solvent；
The solvent-borne type hybrid organic silicon resin is at least one of polyester modified organic silicon resin, phenol aldehyde modified organic siliconresin.
2. solvent-borne type tin-antiomony oxide transparent heat insulating dope composition according to claim 1, it is characterised in that the particle diameter of the nano antimony tin oxide powder is 1~20nm, preferably 10nm.
3. solvent-borne type tin-antiomony oxide transparent heat insulating dope composition according to claim 1 or 2, it is characterised in that the dispersant is a kind of cationic wetting dispersing agent（EFKA5010）, block interpolymers at least one of silane alcohol base ammonium salt.
4. the solvent-borne type tin-antiomony oxide transparent heat insulating dope composition according to any one of claim 1-3, it is characterised in that the alcoholic solvent is at least one of absolute ethyl alcohol, isopropanol, n-butanol, ethyl acetate.
5. the solvent-borne type tin-antiomony oxide transparent heat insulating dope composition according to any one of claim 1-4, it is characterised in that the solid content of the solvent-borne type hybrid organic silicon resin is 30~50%, solvent is at least one of ethanol, n-butanol, propylene glycol monomethyl ether.
6. a kind of preparation method of the solvent-borne type tin-antiomony oxide transparent heat insulating dope composition as any one of claim 1-5, it is characterised in that including：
Add the nano antimony tin oxide powder after the dispersant is dissolved in the alcoholic solvent, it is ultrasonically treated after again ball-milling treatment obtain the nano antimony tin oxide slurry；
The solvent-borne type tin-antiomony oxide transparent heat insulating dope composition is obtained after gained nano antimony tin oxide slurry is uniformly mixed with solvent-borne type hybrid organic silicon resin.
7. a kind of solvent-borne type tin-antiomony oxide transparent heat insulation diaphragm, it is characterized in that, transparent substrates are imposed on by spin-coating method or bar method as the solvent-borne type tin-antiomony oxide transparent heat insulating dope composition any one of claim 1 to 5, the solvent-borne type tin-antiomony oxide transparent heat insulation diaphragm is made in drying, cooling.
8. solvent-borne type tin-antiomony oxide transparent heat insulation diaphragm according to claim 7, it is characterised in that the drying is to be incubated 20~50 minutes at 150~200 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110564294A (en) * | 2019-09-12 | 2019-12-13 | 广东沐峰节能创新科技有限公司 | heat-preservation and heat-insulation coating and preparation method thereof |
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| KR101045351B1 (en) * | 2010-09-30 | 2011-06-30 | 주식회사 솔라메이트 | Multi-functional coating composition and biface coating method using the composition |
| CN102391778A (en) * | 2011-09-05 | 2012-03-28 | 北京首创纳米科技有限公司 | Colored transparent heat insulation glass coating and preparation method thereof |
| CN102876197A (en) * | 2012-07-04 | 2013-01-16 | 中南大学 | Heat-insulating self-cleaning glass coating |
| CN103102083A (en) * | 2013-02-26 | 2013-05-15 | 杭州电子科技大学 | Preparation method of nano antimony tin oxide transparent insulation film |
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| CN101219859A (en) * | 2007-11-30 | 2008-07-16 | 华南理工大学 | Nano-oiliness ATO heat-insulating slurry, production method and uses thereof |
| KR101045351B1 (en) * | 2010-09-30 | 2011-06-30 | 주식회사 솔라메이트 | Multi-functional coating composition and biface coating method using the composition |
| CN102391778A (en) * | 2011-09-05 | 2012-03-28 | 北京首创纳米科技有限公司 | Colored transparent heat insulation glass coating and preparation method thereof |
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| CN103102083A (en) * | 2013-02-26 | 2013-05-15 | 杭州电子科技大学 | Preparation method of nano antimony tin oxide transparent insulation film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110564294A (en) * | 2019-09-12 | 2019-12-13 | 广东沐峰节能创新科技有限公司 | heat-preservation and heat-insulation coating and preparation method thereof |
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