CN106118459A - A kind of casein modified film coating and preparation method thereof - Google Patents
A kind of casein modified film coating and preparation method thereof Download PDFInfo
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- CN106118459A CN106118459A CN201610516192.0A CN201610516192A CN106118459A CN 106118459 A CN106118459 A CN 106118459A CN 201610516192 A CN201610516192 A CN 201610516192A CN 106118459 A CN106118459 A CN 106118459A
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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
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of casein modified film coating, it is made up of the raw material of following weight parts: Afluon (Asta) 12, trithiocyanuric acid 0.7 1, HMPA 0.4 1, casein 12, polytetrafluoroethylwax wax 23, aluminium dihydrogen phosphate 0.3 1, ammonium hydrogen carbonate 45, hydrated sulfuric acid vanadyl 1 1.5, Disodium tungstate (Na2WO4) dihydrate 67, silane coupler KH57020 30, the ammonia spirit 60 70 of MTES 57,2 3%, aminopropyl triethoxysilane 0.3 0.4, nonyl phenol 0.1 0.2, calcium palmitate 12, propylgallate 0.1 0.2.The present invention uses silane coupler KH570 modification, is grafted to mix on tungsten hypovanadic oxide powder granule by silane coupler KH570 molecule, effectively raises the hydrophobicity of modified particle, also further increase the surface strength of film.
Description
Technical field
The present invention relates to film coating technical field, particularly relate to a kind of casein modified film coating and preparation side thereof
Method.
Background technology
Inorganic nano-particle can play mechanics in coating to be strengthened or gives the effect of coating New function and be subject to extensively
Pay close attention to.The dispersion of nanoparticle is even more important for the realization of its function, special high transparent organic-inorganic hybrid nanocomposite coating
Preparation.
Vanadium dioxide has huge application prospect in terms of intelligence heat-insulating and energy-saving coating, but due to its preparation method and work
The restriction of skill, and the strong absorption that vanadium dioxide metal phase and quasiconductor are in short wave ranges, vanadium dioxide film is usual
There is relatively low optical clear, significantly limit its actual application.Therefore, the anti-reflection of vanadium dioxide film is increasingly becoming research
One of focus.
Due to the peculiar property of inorganic nano-particle, it is frequently used to join organic as enhancing phase or functional stuffing
In coating, improve coating tradition performance, give coating specific function characteristic.The nanoparticle being presently used for coating mainly has gold
Belong to oxide (such as TiCh, Si02, Sn02, ZnO etc.), nano metal powder (such as nanometer A1, Co, Ti, Cr, Nd, Mo etc.) and
Nano metal salt (such as CaCO), BaS04) etc..The function of inorganic particulate in hybrid coating to be given full play to, needs the uniform of particle
Fine dispersion, the when that particularly the transparency to composite coating having higher requirements；
, due to its manufacturing process, usually there is reunion stronger between particle in commercially available inorganic particle, is difficult to directly application
In preparing composite coating.In organic coating field, usually the various physics of integrated application and chemical dispersion techniques, enter nano-powder
Row is modified and dispersion, and carries out compound preparing nanocomposite coating with organic resin.Very difficult preparation is provided simultaneously with the visible transparency
The composite membrane strong with infrared barrier；
Vanadium dioxide has thermochromic function, reduces phase transition temperature by doping and makes it possess the potentiality of actual application.To the greatest extent
Pipe it has been reported the preparation method of a lot of vanadium dioxide and doped vanadium dioxide powder and thin film at present, but actual apart from it
Application, still has a segment distance.First, conventional the preparation technology such as apparatus expensive such as magnetron sputtering, vapour deposition, cost is high, relatively
Difficulty realizes large area and covers with paint, lacquer, colour wash, etc.;Secondly, traditional preparation method is due to the limitation of itself, the vanadium dioxide of preparation or dioxy
The visible region transparency changing vanadium (W) thin film is poor, does not substantially have the possibility of actual application.Although having done much at anti-reflection aspect
Attempt, such as doping, coat anti-reflection film, but the raising of the transparency still ratio is relatively limited;Again, the report that oneself has at present is substantially
Concentrate on vanadium dioxide or the preparation of vanadium dioxide (W) pure film, and seldom dabble organic coating route to prepare vanadium dioxide heat
Cause discoloration coating.4th, the research about hypovanadic oxide powder or the stability of thin film (including composite membrane) is reported very at present
Few.Therefore, preparation has the vanadium dioxide film of the relatively high visible district transparency or compound with vanadium dioxide as functional stuffing
Film, and investigate its stability, there is important practical significance；
On the other hand, the dispersion of nanoparticle and stabilization technique are more used for the preparation of organic-inorganic nanocomposite materials the sixth of the twelve Earthly Branches,
Disperse uniformly reaching it, fully realize its function as implant.Common step is to first pass through physical chemistry dispersion
Technology prepares the nano dispersion fluid of inorganic particulate, then dispersion liquid and organic resin is being combined.In organic coating field, first
Step often utilizes the scattered method of ball milling (having under dispersant existence condition) that inorganic particle particle is carried out de-agglomerated.At said process
In the middle of, the compatibility between the compatibility and nanoparticle and organic resin between nanoparticle and disperse medium may be produced
Raw contradiction, if the organic molecule of grafting and resin compatible are the best, during resin solidification is dried, it is possible that receive
Being separated between rice corpuscles and organic facies, causes the decline of the nano-composite coating transparency.Therefore, the purpose of the present invention is exactly
Prepare the nanoparticle that dispersibility is higher, join in organic coating, play the effect of enhancing.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of casein modified film coating and system thereof
Preparation Method.
The present invention is achieved by the following technical solutions:
A kind of casein modified film coating, it is made up of the raw material of following weight parts:
Afluon (Asta) 1-2, trithiocyanuric acid 0.7-1, HMPA 0.4-1, casein 1-2, polytetrafluoroethylwax wax 2-3,
Aluminium dihydrogen phosphate 0.3-1, ammonium hydrogen carbonate 4-5, hydrated sulfuric acid vanadyl 1-1.5, Disodium tungstate (Na2WO4) dihydrate 6-7, silane coupler
KH57020-30, the ammonia spirit 60-70 of MTES 5-7,2-3%, aminopropyl triethoxysilane 0.3-0.4,
Nonyl phenol 0.1-0.2, calcium palmitate 1-2, propylgallate 0.1-0.2.
The preparation method of a kind of described casein modified film coating, comprises the following steps:
(1) above-mentioned ammonium hydrogen carbonate is joined in the deionized water of its weight 20-34 times, stir, add two tungstic acid hydrate
Sodium, magnetic force disperses 2-3 minute, obtains dispersion liquid；
(2) above-mentioned aluminium dihydrogen phosphate is joined in the deionized water of its weight 7-10 times, stir, add casein,
Insulated and stirred 3-4 minute at 50-60 DEG C, obtains casein solution；
(3) take above-mentioned hydrated sulfuric acid vanadyl, join in the deionized water of its weight 10-14 times, drip above-mentioned under stirring condition
Dispersion liquid, magnetic agitation 40-50 minute after dropping, filters, precipitate with deionized water and dehydrated alcohol is washed 2-3 successively
Secondary, it is vacuum dried 100-120 minute at 40-50 DEG C, sends in heating furnace, in a nitrogen atmosphere with the liter of 10-12 DEG C/min
Temperature speed liter high-temperature is to 800-860 DEG C, and Heat preservation 2.7-3 hour, discharging cools down, must mix tungsten hypovanadic oxide powder；
(4) contributing in above-mentioned casein solution by above-mentioned tungsten hypovanadic oxide powder of mixing, rise high-temperature and be 80-90 DEG C, insulation is stirred
Mix and do to water, obtain and modified mix tungsten hypovanadic oxide powder；
(5) 70-80% of above-mentioned silane coupler KH570 weight is mixed with calcium palmitate, at 60-70 DEG C, preheat 3-5 divide
Clock, joins in the butyl acetate of compound weight 40-50 times, stirs, and adds above-mentioned modification and mixes tungsten hypovanadic oxide powder,
Ultrasonic 18-20 minute, ball milling 6-8 hour, by ball milling liquid sucking filtration, washs filter cake 2-3 time with normal octane, vacuum at 40-45 DEG C
It is dried 100-120 minute, cooling, joins in the butyl acetate of its weight 6-8 times, stir, obtain nano dispersion fluid；
(6) take the ammonia spirit of above-mentioned 2-3%, mix with the dehydrated alcohol of its weight 1-1.2 times, stir；
(7) by remaining silane coupler KH570, MTES, nonyl phenol mixing, magnetic agitation 3-5 minute,
Drip the mixed liquor of above-mentioned ammonia, ethanol, insulated and stirred 4-4.5 hour at 86-90 DEG C, obtain siloxane prepolymer；
(8) above-mentioned nano dispersion fluid is joined in siloxane prepolymer, ultrasonic 17-20 minute, add and remain each raw material, stirring
Uniformly, to obtain final product.
The invention have the advantage that using method:
By coating bar film on diaphragm of the present invention, cold curing is dried 7-8 days,.
The present invention, with hydrated sulfuric acid vanadyl and ammonium hydrogen carbonate as raw material, prepares presoma, calcining by solution reaction, it is thus achieved that
Vanadium dioxide and mix the hypovanadic oxide powder of W, by vanadium dioxide (W) powder body ball milling modification, centrifugal preparation nano-dispersed
Liquid, joins in polysiloxane prepolymers, with aminopropyl triethoxysilane as firming agent, be prepared under room temperature polysiloxanes/
Vanadium dioxide (W) nanocomposite coating, the phase transition temperature of this nanocomposite coating is close to room temperature, and hardness is high, and the transparency is good, the reddest
External modulation ability is preferable, is highly suitable for the preparation of in-service film surface intelligence heat insulating coat；
The hypovanadic oxide powder of prepared by the present invention mix tungsten has the near-infrared that reversible metal-semiconductor phase-change characteristic causes and intercepts
Performance, and the doping of tungsten can reduce the phase transition temperature of vanadium dioxide, improves the heat phase transition performance processed of film, then passes through
Butyl acetate disperses efficiently so that its film formed has the good transparency, and the present invention uses silane coupler
KH570 modification, is grafted to mix on tungsten hypovanadic oxide powder granule by silane coupler KH570 molecule, effectively raises
The hydrophobicity of modified particle, simultaneously because the hypovanadic oxide powder mixing tungsten has good mechanical property and this particle and poly-silicon
The crosslinked action of oxygen alkane, also further increases the surface strength of film.The present invention uses casein modified, effectively raises
Nanoparticle dispersibility in coating, improves the stability of finished product coating.
Detailed description of the invention
A kind of casein modified film coating, it is made up of the raw material of following weight parts:
Afluon (Asta) 1, trithiocyanuric acid 0.7, HMPA 0.4, casein 1, polytetrafluoroethylwax wax 2, aluminium dihydrogen phosphate
0.3, ammonium hydrogen carbonate 4, hydrated sulfuric acid vanadyl 1, Disodium tungstate (Na2WO4) dihydrate 6, silane coupler KH57020, MTES
5,2% ammonia spirit 60, aminopropyl triethoxysilane 0.3, nonyl phenol 0.1, calcium palmitate 1, propylgallate 0.1.
The preparation method of a kind of described casein modified film coating, comprises the following steps:
(1) above-mentioned ammonium hydrogen carbonate is joined in the deionized water of its weight 20 times, stirs, add Disodium tungstate (Na2WO4) dihydrate,
Magnetic force disperses 2 minutes, obtains dispersion liquid；
(2) above-mentioned aluminium dihydrogen phosphate is joined in the deionized water of its weight 7 times, stir, add casein, at 50 DEG C
Lower insulated and stirred 3 minutes, obtains casein solution；
(3) take above-mentioned hydrated sulfuric acid vanadyl, join in the deionized water of its weight 10 times, under stirring condition, drip above-mentioned dispersion
Liquid, magnetic agitation 40 minutes after dropping, filter, precipitate with deionized water and dehydrated alcohol are washed 2 times successively, at 40 DEG C
Lower vacuum drying 100 minutes, sends in heating furnace, rises high-temperature to 800 with the programming rate of 10 DEG C/min in a nitrogen atmosphere
DEG C, Heat preservation 2.7 hours, discharging cools down, must mix tungsten hypovanadic oxide powder；
(4) contributing in above-mentioned casein solution by above-mentioned tungsten hypovanadic oxide powder of mixing, rising high-temperature is 80 DEG C, and insulated and stirred is extremely
Water is done, and obtains and modified mixes tungsten hypovanadic oxide powder；
(5) mix the 70% of above-mentioned silane coupler KH570 weight with calcium palmitate, preheat 3 minutes at 60 DEG C, join
In the butyl acetate that compound weight is 40 times, stir, add above-mentioned modification and mix tungsten hypovanadic oxide powder, ultrasonic 18 minutes,
Ball milling 6 hours, by ball milling liquid sucking filtration, washs filter cake 2 times with normal octane, is vacuum dried 100 minutes at 40 DEG C, and cooling adds
In the butyl acetate of its weight 6 times, stir, obtain nano dispersion fluid；
(6) take the ammonia spirit of above-mentioned 2%, mix with the dehydrated alcohol of its weight 1 times, stir；
(7) by remaining silane coupler KH570, MTES, nonyl phenol mixing, magnetic agitation 3 minutes, drip
Adding the mixed liquor of above-mentioned ammonia, ethanol, at 86 DEG C, insulated and stirred 4 hours, obtain siloxane prepolymer；
(8) joining in siloxane prepolymer by above-mentioned nano dispersion fluid, ultrasonic 17 minutes, add and remain each raw material, stirring is all
Even, to obtain final product.
The transparency: the transmitance at 550 nm still reaches more than 60%；
Mechanical property: hardness >=900MPa；
Heat phase transition performance processed: 2500nm infrared modulated amplitude: 23.2%.
Claims (2)
1. a casein modified film coating, it is characterised in that it is made up of the raw material of following weight parts:
Afluon (Asta) 1-2, trithiocyanuric acid 0.7-1, HMPA 0.4-1, casein 1-2, polytetrafluoroethylwax wax 2-3,
Aluminium dihydrogen phosphate 0.3-1, ammonium hydrogen carbonate 4-5, hydrated sulfuric acid vanadyl 1-1.5, Disodium tungstate (Na2WO4) dihydrate 6-7, silane coupler
KH57020-30, the ammonia spirit 60-70 of MTES 5-7,2-3%, aminopropyl triethoxysilane 0.3-0.4,
Nonyl phenol 0.1-0.2, calcium palmitate 1-2, propylgallate 0.1-0.2.
2. the preparation method of a casein modified film coating as claimed in claim 1, it is characterised in that include following step
Rapid:
(1) above-mentioned ammonium hydrogen carbonate is joined in the deionized water of its weight 20-34 times, stir, add two tungstic acid hydrate
Sodium, magnetic force disperses 2-3 minute, obtains dispersion liquid；
(2) above-mentioned aluminium dihydrogen phosphate is joined in the deionized water of its weight 7-10 times, stir, add casein,
Insulated and stirred 3-4 minute at 50-60 DEG C, obtains casein solution；
(3) take above-mentioned hydrated sulfuric acid vanadyl, join in the deionized water of its weight 10-14 times, drip above-mentioned under stirring condition
Dispersion liquid, magnetic agitation 40-50 minute after dropping, filters, precipitate with deionized water and dehydrated alcohol is washed 2-3 successively
Secondary, it is vacuum dried 100-120 minute at 40-50 DEG C, sends in heating furnace, in a nitrogen atmosphere with the liter of 10-12 DEG C/min
Temperature speed liter high-temperature is to 800-860 DEG C, and Heat preservation 2.7-3 hour, discharging cools down, must mix tungsten hypovanadic oxide powder；
(4) contributing in above-mentioned casein solution by above-mentioned tungsten hypovanadic oxide powder of mixing, rise high-temperature and be 80-90 DEG C, insulation is stirred
Mix and do to water, obtain and modified mix tungsten hypovanadic oxide powder；
(5) 70-80% of above-mentioned silane coupler KH570 weight is mixed with calcium palmitate, at 60-70 DEG C, preheat 3-5 divide
Clock, joins in the butyl acetate of compound weight 40-50 times, stirs, and adds above-mentioned modification and mixes tungsten hypovanadic oxide powder,
Ultrasonic 18-20 minute, ball milling 6-8 hour, by ball milling liquid sucking filtration, washs filter cake 2-3 time with normal octane, vacuum at 40-45 DEG C
It is dried 100-120 minute, cooling, joins in the butyl acetate of its weight 6-8 times, stir, obtain nano dispersion fluid；
(6) take the ammonia spirit of above-mentioned 2-3%, mix with the dehydrated alcohol of its weight 1-1.2 times, stir；
(7) by remaining silane coupler KH570, MTES, nonyl phenol mixing, magnetic agitation 3-5 minute,
Drip the mixed liquor of above-mentioned ammonia, ethanol, insulated and stirred 4-4.5 hour at 86-90 DEG C, obtain siloxane prepolymer；
(8) above-mentioned nano dispersion fluid is joined in siloxane prepolymer, ultrasonic 17-20 minute, add and remain each raw material, stirring
Uniformly, to obtain final product.
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| CN201610516192.0A CN106118459A (en) | 2016-07-04 | 2016-07-04 | A kind of casein modified film coating and preparation method thereof |
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| CN105131735A (en) * | 2015-08-27 | 2015-12-09 | 安徽明威照明器材有限公司 | Brightening yellowing-resistant LED heat dissipation coating and preparation method therefor |
| CN105368305A (en) * | 2015-10-28 | 2016-03-02 | 天长市润达金属防锈助剂有限公司 | Flexible aluminum alloy anticorrosion lifting-and-pulling sol and preparation method thereof |
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2016
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Patent Citations (7)
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|---|---|---|---|---|
| CN103409008A (en) * | 2013-07-03 | 2013-11-27 | 安徽真信涂料有限公司 | High-adhesive force interior wall coating material and preparation method thereof |
| CN104046160A (en) * | 2014-05-22 | 2014-09-17 | 滁州市宁扬胶业有限公司 | Environment-friendly interior wall latex paint with low heat conductivity |
| CN104119758A (en) * | 2014-06-26 | 2014-10-29 | 安徽快来防水防腐有限公司 | Dense anti-leakage waterproof coating |
| CN104610488A (en) * | 2015-01-28 | 2015-05-13 | 浙江威廉姆节能科技有限公司 | High-permeability anti-radiation coating and preparation method thereof |
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