CN105885689B - A kind of inorganic diamante and preparation method thereof - Google Patents

A kind of inorganic diamante and preparation method thereof Download PDF

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CN105885689B
CN105885689B CN201610309371.7A CN201610309371A CN105885689B CN 105885689 B CN105885689 B CN 105885689B CN 201610309371 A CN201610309371 A CN 201610309371A CN 105885689 B CN105885689 B CN 105885689B
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李植来
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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
    • C09D183/16—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 in which all the silicon atoms are connected by linkages other than oxygen atoms
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    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
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    • 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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    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
    • C08J2483/16—Characterised by the use of 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; Derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
    • 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
    • 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
    • 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
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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    • 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

Abstract

The invention discloses a kind of inorganic diamante and preparation method thereof, it is desirable to provide one kind does not melt at 800 degrees Celsius, and transparency is high, the adjustable inorganic diamante of density；Its technical scheme is made up of following components in parts by weight：46 parts of organic oligomer, 11 17 parts of tetraethoxysilane, 16 24 parts of Polycarbosilane, 8 12 parts of nano-oxide filler, 0.8 1.2 parts of silica, 16 24 parts of tetrahydrofuran, 21 31 parts of dimethylbenzene, 0.12 0.18 parts of calgon, 0.09 0.13 parts of polysiloxane defoaming agent, 1,0.64 0.96 parts of 2 benzisothiazole, 3 ketone, 0.02 part of 0.01 part of phthalocyanine blue, 1.6 2.4 parts of n-butanol, 0.8 1.2 parts of ethylene glycol ethyl ether and tripropylene glycol butyl ether.

Description

A kind of inorganic diamante and preparation method thereof
Technical field
The invention discloses a kind of diamante, is a kind of inorganic flash of light paillette, the invention also discloses the nothing specifically The preparation method of machine diamante.
Background technology
Material with flash effect is because of very popular, the in general such as its good visual effect, decoration performance Diamante is that color is coated after being electroplated by polyester film, cleaved growth 0.1-3mm, wide 0.1-3mm, and thickness is 20-30nm's Small pieces；Diamante is influenceed, and inject light and color due to there is aluminizer metallic luster by light.Ground is poly- Ester film, and 240 DEG C of polyester film maximum temperature, after this temperature, will be melted, ineffective.
The content of the invention
In view of the above-mentioned problems, not melted at 800 degrees Celsius it is an object of the invention to provide one kind, transparency is high, and density can Inorganic diamante reconciled and preparation method thereof.
In order to solve the above technical problems, previous technical scheme provided by the invention is such：
A kind of inorganic diamante is mainly made up of following components in parts by weight：Organic oligomer 4-6 parts, tetraethoxysilane 11-17 parts, Polycarbosilane 16-24 parts, nano-oxide filler 8-12 parts, silica 0.8-1.2 parts, tetrahydrofuran 16-24 Part, dimethylbenzene 21-31 parts, calgon 0.12-0.18 parts, polysiloxane defoaming agent 0.09-0.13 parts, 1,2- benzisothia Azoles -3- ketone 0.64-0.96 parts, 0.01 part of phthalocyanine blue, n-butanol 1.6-2.4 parts, ethylene glycol ethyl ether 0.8-1.2 parts and tripropylene glycol 0.02 part of butyl ether.
Further, above-mentioned a kind of inorganic diamante, in addition to 5-7.6 parts by weight of cerium oxide, 0.02-0.04 weight Part zirconium driers and 0.16-0.24 parts by weight HMMM resins.
Further, a kind of above-mentioned inorganic diamante, described nano-oxide filler are received by 3.16-4.74 parts by weight Rice titanium oxide, 2.2-3.3 parts by weight nano zircites, 2.28-3.42 parts by weight nano silicons, 0.33-0.50 parts by weight Nanometer di-iron trioxide and 0.24-0.37 parts by weight nano ferriferrous oxide composition.
Further, above-mentioned a kind of inorganic diamante, it is characterised in that described organic oligomer is triethoxysilicane PFPE-caprolactone of base end-blocking.
Further, a kind of above-mentioned inorganic diamante, described HMMM resin are CYMEL303；Described polysiloxane defoaming agent is the high Foamex 840 of enlightening；Described Polycarbosilane is National University of Defense technology CFC The PCS that key lab voluntarily develops, Tan solid, fusing point are 210 DEG C, molecular weight 1500.
In order to prepare above-mentioned inorganic diamante, latter solution provided by the invention is such：
1) each component is weighed；
2) by organic oligomer, tetraethoxysilane, tetrahydrofuran, Polycarbosilane, dimethylbenzene, nano-oxide filler, Phthalocyanine blue, n-butanol, ethylene glycol ethyl ether, tripropylene glycol butyl ether are put into ball mill, and ball milling disperses, and obtains premix；
3) the premix ultrasonic vibration for preparing step 2) 4 hours, calgon, poly- silica that step 1) weighs are added Alkane defoamer and chelating agent stirring 20min, are well mixed, obtain stand-by slurry；
4) slurry for preparing step 3), is poured into the oil groove of dry type coating machine, gets the thick polyesters of thickness 20-25um ready Film, under 240 DEG C of environment, coated machine work, slurry is coated on to the top layer of polyester film, shape is dried under 180 DEG C of environment Into organic ink coating layer, organic ink coating thickness is 20-25um, after coating, the constant temperature 1h under 200 DEG C of environment, Peeled off by stripping machine, it is coiled stand-by；
5) by coiled organic ink coating layer, heated in argon gas atmosphere stove, cracking, taking off liberation of hydrogen turns into inorganic Bright film；
6) the inorganic transparent film after having cracked, continuous vacuum coating machine is sent into, aluminize film thickness 30-60nm, passes through Coating machine coats two-sided color, is cutting into different shape.
Further, the preparation method of above-mentioned inorganic diamante, the method described in step 2) are specially：First by step 1) organic oligomer weighed, tetraethoxysilane and 8-12 parts tetrahydrofuran add ball mill, and ball milling disperses 5-7 hours, obtained Premix A；Then the remaining tetrahydrofuran of Polycarbosilane, dimethylbenzene and step 2) step 1) weighed adds ball mill, ball Mill scattered 1.5-2.5 hours, obtain premix B；Again by the nano-oxide filler described in step 1), phthalocyanine blue, n-butanol, second two Alcohol ether, tripropylene glycol butyl ether are put into ball mill, and ball milling disperses 5-7 hours, obtains premix C；By premix A, premix B and in advance Batch mixing C is well mixed to obtain premix.
Further, the preparation method of above-mentioned inorganic diamante, in step 3), calgon, poly- silica are being added After alkane defoamer and chelating agent are uniformly mixed, add the HMMM of formula ratio, ceria and Zirconium driers simultaneously use ultrasonic vibration 5 hours, obtain stand-by slurry.
Further, the preparation method of above-mentioned inorganic diamante, step 4) are specially：Slurry prepared by step 3), Pour into the oil groove of dry type coating machine, get the thick polyester films of thickness 20-25um, under 240 DEG C of environment, coated machine work ready Make, slurry is coated on to the top layer of polyester film, dried under 180 DEG C of environment and form organic ink coating layer, organic ink applies Ply gage is 20-25um, after coating, the constant temperature 2h under 120 DEG C of environment, then naturally cools to room temperature, is sent into freezer Room, 2h is refrigerated under -20 DEG C of environment, after taking-up, 200 DEG C are warming up under 5 DEG C/min speed, and it is permanent under 200 DEG C of environment Warm 1h, finally naturally cools to room temperature, is peeled off by stripping machine, coiled stand-by.
Further, the preparation method of above-mentioned inorganic diamante, step 5) are specially：Coiled organic ink is applied Layer of cloth, in argon gas atmosphere stove, be warming up to 300 DEG C from room temperature with 2 DEG C/min speed first, crack 0.5 hour, then again with 1-2 DEG C/min speed is warming up to 600-800 DEG C, cracks 1h, and de- liberation of hydrogen turns into inorganic transparent film.
Compared with prior art, technical scheme provided by the invention has following technological merit：
1st, Polycarbosilane gradual liberation of hydrogen more than 200 DEG C in technical scheme provided by the invention is Polycarbosilane by organic Material is converted into inorganic material, and temperature rises network structure and risen；
2nd, Polycarbosilane, tetraethoxysilane and organic oligomer and nano-oxide hybridization compounding, it is film layer solidification Surface has " double to dredge " afterwards, i.e., hydrophobicity and oleophobic property, temperature bring up to 800 DEG C, and major ingredient liberation of hydrogen or deoxidation are complete, are converted into non- Crystal silicon film.
3rd, nanometer rutile provided by the invention, zirconium oxide and silica enhance anti-ultraviolet ability, prevent old Change, reduce film layer porosity 66%, increase wearability, make film layer that there is non-slip；Ferric oxide, ferroso-ferric oxide and phthalocyanine blue Produce micro- interference of film, reduce scattering；The addition of ethylene glycol ethyl ether helps the wetability of Nano filling；Tripropylene glycol butyl ether promotes Nanometer condiment and major ingredient levelability improve；Calgon is easily dispersed nano-oxide filler, polysiloxane defoaming agent, 1, 2- benzisothiazole-3-ketones improve the rate of drying of coating materials.
4th, tetrahydrofuran, because the time is different, is produced variable grain degree, makes course of reaction rational using separately grinding Carried out under speed, contribute to Multicomponent reaction abundant.
5th, each component coordinates long-time supersonic oscillations using long-time ball milling respectively, makes each component especially nano oxidized Thing is effectively scattered, both effectively well mixed, avoids reuniting again.Two ways combines so that the mixing of material is more uniform.
Sum it up, technical scheme provided by the invention its do not melted at up to 800 degrees Celsius, transparency is high, not by temperature Degree limitation, density is in 1-1.4g/cm3Interior to reconcile, use range is wide.
Embodiment
With reference to embodiment, the claim of the present invention is described in further detail, but not formed pair Any restrictions of the present invention, the modification of any limited number of time made in the claims in the present invention protection domain, still in the present invention Claims within.
Embodiment 1
A kind of inorganic diamante provided by the invention, is made up of the component of following weight：Triethoxy silicon substrate blocks complete Perfluoroalkyl polyether-caprolactone 6kg, PFPE-caprolactone of described triethoxy silicon substrate end-blocking is Liu Guojie, Li Jia, Sun Fang, journey Pine, old to apply, " Wengfu blue sky cup " Discussion on Technology is developed and applied to 2009- the 7th national feature fluorine silicon materials and Coating Market PFPE-caprolactone of triethoxy silicon substrate end-blocking disclosed in meeting；Tetraethoxysilane 11kg, Polycarbosilane 24kg, it is described Polycarbosilane be the PCS that voluntarily develops of CFC key labs of the National University of Defense technology, Tan solid, fusing point is 210 DEG C, point Son amount 1500, i.e. Chen Man China etc.《Aerospace material technique》Polycarbosilane described in 3rd phase in 2005；3.16kg nano-titanium oxide (particle diameter 10nm), 3.3kg nano zircites (particle diameter 30nm), 2.28kg nano silicons (particle diameter 10nm), 0.50kg nanometers Di-iron trioxide (particle diameter 10nm)；0.24kg nano ferriferrous oxides (particle diameter 20nm), tetrahydrofuran 16kg, dimethylbenzene 31kg, Calgon 0.12kg, the high 0.13kg of Foamex 840 of enlightening, HMMM resin (CYMEL303) 0.16kg, 1,2- benzisothiazole-3-ketone 0.96kg, ceria 5kg, zirconium driers 0.04kg；0.01kg phthalocyanine blues； 1.6kg n-butanol；1.2kg ethylene glycol ethyl ether；0.02kg tripropylene glycol butyl ether.
Embodiment 2
The inorganic diamante of another kind provided by the invention, is made up of the component of following weight：Triethoxy silicon substrate end-blocking PFPE-caprolactone ester 4kg, PFPE-caprolactone of described triethoxy silicon substrate end-blocking is Liu Guojie, Li Jia, grandson Virtue, Cheng Song is old to apply, and " Wengfu blue sky cup " skill is developed and applied to 2009- the 7th national feature fluorine silicon materials and Coating Market PFPE-caprolactone that triethoxy silicon substrate disclosed in art seminar blocks；Tetraethoxysilane 17kg, Polycarbosilane 16kg, 4.74kg nano-titanium oxide (particle diameter 10nm), 2.2kg nano zircites (particle diameter 30nm), 3.42kg nano silicons (particle diameter 10nm), 0.33kg nanometer di-iron trioxides (particle diameter 10nm)；0.37kg nano ferriferrous oxides (particle diameter 20nm), tetrahydrochysene Furans 24kg, dimethylbenzene 21kg, calgon 0.18kg, the high 0.09-0.13kg of Foamex 840 of enlightening, hexamethoxy methyl Melmac 0.24kg, 1,2- benzisothiazole-3-ketone 0.96kg, ceria 7.6kg, zirconium driers 0.02kg； 0.01kg phthalocyanine blues；2.4kg n-butanol；0.8kg ethylene glycol ethyl ethers；0.02kg tripropylene glycol butyl ether.
Embodiment 3
The inorganic diamante of another kind provided by the invention, is made up of the component of following weight：Triethoxy silicon substrate end-blocking PFPE-caprolactone ester 5kg, PFPE-caprolactone of described triethoxy silicon substrate end-blocking is Liu Guojie, Li Jia, grandson Virtue, Cheng Song is old to apply, and " Wengfu blue sky cup " skill is developed and applied to 2009- the 7th national feature fluorine silicon materials and Coating Market PFPE-caprolactone that triethoxy silicon substrate disclosed in art seminar blocks；Tetraethoxysilane 14kg, Polycarbosilane 20kg, 3.95kg nano-titanium oxide (particle diameter 10nm), 2.77kg nano zircites (particle diameter 30nm), 2.85kg nano silicons (particle diameter 10nm), 0.42kg nanometer di-iron trioxides (particle diameter 10nm)；0.31kg nano ferriferrous oxides (particle diameter 20nm), dioxy SiClx 1kg, tetrahydrofuran 20kg, dimethylbenzene 25kg, calgon 0.16kg, the high 0.09kg of Foamex 840 of enlightening, hexakis-methoxy Methyl melamine resin 0.24kg, 1,2- benzisothiazole-3-ketone 0.64kg, ceria 7.6kg, zirconium driers 0.02kg；0.01kg phthalocyanine blues；2.4kg n-butanol；0.8kg ethylene glycol ethyl ethers；0.02kg tripropylene glycol butyl ether.
A kind of preparation method of inorganic diamante of any one in embodiment 1 to 3 is as follows：
1) any one group of mass number weighs each component in embodiment 1 to 3；
2) organic oligomer for first weighing step 1), tetraethoxysilane and 8-12 parts tetrahydrofuran add ball milling Machine, ball milling disperse 5-7 hours, obtain premix A；Then Polycarbosilane, dimethylbenzene and the step 2) step 1) weighed is remaining Tetrahydrofuran adds ball mill, and ball milling disperses 1.5-2.5 hours, obtains premix B；The nano-oxide described in step 1) is filled out again Material, phthalocyanine blue, n-butanol, ethylene glycol ethyl ether, tripropylene glycol butyl ether are put into ball mill, and ball milling is scattered 6 hours, obtains premix C；Will Premix A, premix B and premix C are well mixed to obtain premix；
3) the premix ultrasonic vibration 4 hours for preparing step 2), add calgon, polysiloxane defoaming agent and After chelating agent is uniformly mixed, the HMMM, ceria and zirconium driers of formula ratio are added simultaneously Using ultrasonic oscillation 5 hours, stand-by slurry is obtained；
4) slurry for preparing step 3), is poured into the oil groove of dry type coating machine, gets the thick polyesters of thickness 20-25um ready Film, under 240 DEG C of environment, coated machine work, slurry is coated on to the top layer of polyester film, shape is dried under 180 DEG C of environment Into organic ink coating layer, organic ink coating thickness is 20-25um, after coating, the constant temperature 2h under 120 DEG C of environment, Then room temperature is naturally cooled to, freezer room is sent into, 2h is refrigerated under -20 DEG C of environment, after taking-up, is risen under 5 DEG C/min speed Temperature is to 200 DEG C, and the constant temperature 1h under 200 DEG C of environment, finally naturally cools to room temperature, is peeled off by stripping machine, coiled stand-by；
5) by coiled organic ink coating layer, in argon gas atmosphere stove, first from room temperature with 2 DEG C/min speed liter Temperature cracks 0.5 hour to 300 DEG C, is then warming up to 600-800 DEG C again with 1-2 DEG C/min speed, crack 1h, take off liberation of hydrogen into For inorganic transparent film；
6) the inorganic transparent film after having cracked, it is sent into continuous vacuum coating machine (1.8*10-2Pa；0.2nm/S), aluminize Film thickness 30nm, two-sided color is coated by coating machine, cuts into different shape further according to being actually needed, typically 0.1- 3mm, wide 0.1-3mm small pieces.
Embodiment 4
A kind of inorganic diamante provided by the invention, is made up of the component of following weight number：Triethoxy silicon substrate end-blocking PFPE-caprolactone ester 6kg, PFPE-caprolactone of described triethoxy silicon substrate end-blocking is Liu Guojie, Li Jia, grandson Virtue, Cheng Song is old to apply, and " Wengfu blue sky cup " skill is developed and applied to 2009- the 7th national feature fluorine silicon materials and Coating Market PFPE-caprolactone that triethoxy silicon substrate disclosed in art seminar blocks；Tetraethoxysilane 11kg, Polycarbosilane 24kg, the PCS that described Polycarbosilane is voluntarily developed for CFC key labs of the National University of Defense technology, Tan solid, fusing point are 210 DEG C, molecular weight 1500, i.e. Chen Man China etc.《Aerospace material technique》Polycarbosilane described in 3rd phase in 2005；3.16kg nanometer Titanium oxide (particle diameter 10nm), 3.3kg nano zircites (particle diameter 30nm), 2.28kg nano silicons (particle diameter 10nm), 0.50kg nanometer di-iron trioxides (particle diameter 10nm)；0.24kg nano ferriferrous oxides (particle diameter 20nm), silica 1 .2kg, Tetrahydrofuran 16kg, dimethylbenzene 31kg, calgon 0.12kg, polysiloxane defoaming agent 0.13kg, 1,2- benzisothiazole- 3- ketone 0.64kg, phthalocyanine blue 0.01kg, n-butanol 2.4kg, ethylene glycol ethyl ether 0.8kg and tripropylene glycol butyl ether 0.02kg.
Embodiment 5
A kind of inorganic diamante provided by the invention, is made up of the component of following weight number：Triethoxy silicon substrate end-blocking PFPE-caprolactone ester 4kg, PFPE-caprolactone of described triethoxy silicon substrate end-blocking is Liu Guojie, Li Jia, grandson Virtue, Cheng Song is old to apply, and " Wengfu blue sky cup " skill is developed and applied to 2009- the 7th national feature fluorine silicon materials and Coating Market PFPE-caprolactone that triethoxy silicon substrate disclosed in art seminar blocks；Tetraethoxysilane 17kg, Polycarbosilane 16kg, the PCS that described Polycarbosilane is voluntarily developed for CFC key labs of the National University of Defense technology, Tan solid, fusing point are 210 DEG C, molecular weight 1500, i.e. Chen Man China etc.《Aerospace material technique》Polycarbosilane described in 3rd phase in 2005；3.16kg nanometer Titanium oxide (particle diameter 10nm), 3.3kg nano zircites (particle diameter 30nm), 2.28kg nano silicons (particle diameter 10nm), 0.50kg nanometer di-iron trioxides (particle diameter 10nm)；0.24kg nano ferriferrous oxides (particle diameter 20nm), silica 0.8kg, Tetrahydrofuran 24kg, dimethylbenzene 21kg, calgon 0.18kg, polysiloxane defoaming agent 0.09kg, 1,2- benzisothiazole- 3- ketone 0.96kg, phthalocyanine blue 0.01kg, n-butanol 1.6kg, ethylene glycol ethyl ether 1.2kg and tripropylene glycol butyl ether 0.02kg.
1) any one group of mass number weighs each component in embodiment 4 to 5；
2) by ethyl-silicone block PFPE-caprolactone ester, tetraethoxysilane, tetrahydrofuran, Polycarbosilane, Dimethylbenzene, nano-oxide filler, phthalocyanine blue, n-butanol, ethylene glycol ethyl ether, tripropylene glycol butyl ether are put into ball mill, ball milling point Dissipate, obtain premix；
3) the premix ultrasonic vibration for preparing step 2) 4 hours, calgon, poly- silica that step 1) weighs are added Alkane defoamer and chelating agent stirring 20min, are well mixed, obtain stand-by slurry；
4) slurry for preparing step 3), is poured into the oil groove of dry type coating machine, gets the thick polyesters of thickness 20-25um ready Film, under 240 DEG C of environment, coated machine work, slurry is coated on to the top layer of polyester film, shape is dried under 180 DEG C of environment Into organic ink coating layer, organic ink coating thickness is 20-25um, after coating, the constant temperature 1h under 200 DEG C of environment, Peeled off by stripping machine, it is coiled stand-by；
5) by coiled organic ink coating layer, heated in argon gas atmosphere stove, cracking, taking off liberation of hydrogen turns into inorganic Bright film；
6) the inorganic transparent film after having cracked, it is sent into continuous vacuum coating machine (1.8*10-2Pa；0.2nm/S), aluminize Film thickness 30nm, two-sided color is coated by coating machine, cuts into different shape further according to being actually needed, typically 0.1- 3mm, wide 0.1-3mm small pieces.
It should be noted that the parameter not being shown in detail in technical scheme provided by the invention, conventional according to this area Technological means is carried out.
In order to prove the technique effect of inorganic diamante provided by the invention, by glittering provided by the invention and in the market Conventional glittering progress fusing point test, as a result see the table below.

Claims (4)

1. a kind of inorganic diamante, it is characterised in that mainly comprise the steps：
1) slurry is prepared；
2) slurry prepared is poured into the oil groove of dry type coating machine, the thick polyester films of thickness 20-25um is got ready, 240 Under DEG C environment, coated machine work, slurry is coated on to the top layer of polyester film, under 180 DEG C of environment drying form organic slurry Expect coating layer, organic ink coating thickness is 20-25um, after coating, the constant temperature 1h under 200 DEG C of environment, by peeling off Machine is peeled off, coiled stand-by；
3) by coiled organic ink coating layer, heated in argon gas atmosphere stove, cracking, it is thin as inorganic transparent to take off liberation of hydrogen Film；
4) the inorganic transparent film after having cracked, continuous vacuum coating machine is sent into, aluminize film thickness 30-60nm, by coating Machine coats two-sided color, is cutting into different shape；
Wherein：Slurry described in step 1) is mainly made up of following components in parts by weight：Organic oligomer 4-6 parts, tetraethoxy Silane 11-17 parts, Polycarbosilane 16-24 parts, nano-oxide filler 8-12 parts, silica 0.8-1.2 parts, tetrahydrofuran 16-24 parts, dimethylbenzene 21-31 parts, calgon 0.12-0.18 parts, polysiloxane defoaming agent 0.09-0.13 parts, 1,2- benzene And isothiazole -3- ketone 0.64-0.96 parts, 0.01 part of phthalocyanine blue, n-butanol 1.6-2.4 parts, ethylene glycol ethyl ether 0.8-1.2 parts and three 0.02 part of propandiol butyl ether；Described organic oligomer is PFPE-caprolactone of triethoxy silicon substrate end-blocking.
A kind of 2. inorganic diamante according to claim 1, it is characterised in that also including 5-7.6 parts by weight of cerium oxide, 0.02-0.04 parts by weight zirconium driers and 0.16-0.24 parts by weight HMMM resins.
A kind of 3. inorganic diamante according to claim 1, it is characterised in that described nano-oxide filler by 3.16-4.74 parts by weight nano-titanium oxides, 2.2-3.3 parts by weight nano zircites, 2.28-3.42 parts by weight nanometer titanium dioxides Silicon, 0.33-0.50 parts by weight nanometer di-iron trioxides and 0.24-0.37 parts by weight nano ferriferrous oxide composition.
A kind of 4. inorganic diamante according to claim 1, it is characterised in that described HMMM Resin is CYMEL303；Described polysiloxane defoaming agent is the high Foamex 840 of enlightening；Described Polycarbosilane is science and techniques of defence The PCS that CFC key labs of university voluntarily develop, Tan solid, fusing point are 210 DEG C, molecular weight 1500.
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CN1059543A (en) * 1991-09-25 1992-03-18 中国科学院上海有机化学研究所 The production method of glittering material
CN1490152A (en) * 2003-08-18 2004-04-21 李植来 Preparing method for polyester sequin
CN105542211A (en) * 2015-12-02 2016-05-04 安徽省通达包装材料有限公司 High temperature-resistant and anti-aging two-side coated polyester aluminized film and production method thereof

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Publication number Priority date Publication date Assignee Title
JP4143845B2 (en) * 2003-11-26 2008-09-03 Ｊｓｒ株式会社 Insulating film and method for forming the same, and laminate having insulating film and method for forming the same

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Publication number Priority date Publication date Assignee Title
US4004930A (en) * 1975-07-02 1977-01-25 Minnesota Mining And Manufacturing Company Fluid composition for forming retroreflective structures
CN1059543A (en) * 1991-09-25 1992-03-18 中国科学院上海有机化学研究所 The production method of glittering material
CN1490152A (en) * 2003-08-18 2004-04-21 李植来 Preparing method for polyester sequin
CN105542211A (en) * 2015-12-02 2016-05-04 安徽省通达包装材料有限公司 High temperature-resistant and anti-aging two-side coated polyester aluminized film and production method thereof

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