CN105885689A - Inorganic sequin and preparation method thereof - Google Patents

Inorganic sequin and preparation method thereof Download PDF

Info

Publication number
CN105885689A
CN105885689A CN201610309371.7A CN201610309371A CN105885689A CN 105885689 A CN105885689 A CN 105885689A CN 201610309371 A CN201610309371 A CN 201610309371A CN 105885689 A CN105885689 A CN 105885689A
Authority
CN
China
Prior art keywords
inorganic
diamante
nano
premix material
under
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610309371.7A
Other languages
Chinese (zh)
Other versions
CN105885689B (en
Inventor
李植来
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201610309371.7A priority Critical patent/CN105885689B/en
Publication of CN105885689A publication Critical patent/CN105885689A/en
Application granted granted Critical
Publication of CN105885689B publication Critical patent/CN105885689B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • 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
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • 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
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • 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
    • 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

Abstract

The invention discloses an inorganic sequin and a preparation method thereof, aiming at providing an inorganic sequin which does not melt at 800 degrees centigrade and has high transparency as well as adjustable density. The technical scheme is that the inorganic sequin is prepared from the following components in parts by weight: 4-6 parts of organic oligomer, 11-17 parts of tetraethoxysilane, 16-24 parts of polycarbosilane, 8-12 parts of nanometer oxide filler, 0.8-1.2 parts of silicon dioxide, 16-24 parts of tetrahydrofuran, 21-31 parts of xylene, 0.12-0.18 part of sodium hexametaphosphate, 0.09-0.13 part of polysiloxane defoamer, 0.64-0.96 part of 1,2-benzisothiazole-3-ketone, 0.01 part of phthalo blue, 1.6-2.4 parts of n-butyl alcohol, 0.8-1.2 parts of glycol ether, and 0.02 part of tripropylene glycol n-butyl ether.

Description

A kind of inorganic diamante and preparation method thereof
Technical field
The invention discloses a kind of diamante, specifically, be a kind of inorganic flash of light paillette, the invention also discloses this inorganic sudden strain of a muscle The preparation method of mating plate.
Background technology
There is the material of flash effect because of very popular, general diamantes such as its good visual effect, decoration performances Be electroplated by mylar after coat color, cleaved growth 0.1-3mm, wide 0.1-3mm, thickness is the small pieces of 20-30nm； Diamante, owing to there being the effect of aluminizer metallic luster, is affected by light, and injects light and color.Ground is mylar, And mylar maximum temperature 240 DEG C, after exceeding this temperature, will be melted, ineffective.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide one and do not melt at 800 degrees Celsius, transparency is high, and density can be reconciled Inorganic diamante and preparation method thereof.
For solving above-mentioned technical problem, the previous technical scheme that the present invention provides is such that
A kind of inorganic diamante is mainly made up of following components in parts by weight: organic oligomer 4-6 part, tetraethoxysilane 11-17 Part, Polycarbosilane 16-24 part, nano-oxide filler 8-12 part, silicon dioxide 0.8-1.2 part, oxolane 16-24 part, Dimethylbenzene 21-31 part, sodium hexameta phosphate 0.12-0.18 part, polysiloxane defoaming agent 0.09-0.13 part, 1,2-benzisothia Azoles-3-ketone 0.64-0.96 part, phthalocyanine blue 0.01 part, n-butyl alcohol 1.6-2.4 part, ethylene glycol 0.8-1.2 part and 3 third Glycol butyl ether 0.02 part.
Further, the inorganic diamante of above-mentioned one, also include 5-7.6 parts by weight of cerium oxide, 0.02-0.04 weight portion Zirconium driers and 0.16-0.24 weight portion HMMM resin.
Further, the inorganic diamante of above-mentioned one, described nano-oxide filler is by 3.16-4.74 weight portion nano oxygen Change titanium, 2.2-3.3 weight portion nano zircite, 2.28-3.42 weight portion nano silicon, 0.33-0.50 weight portion nanometer Iron sesquioxide and 0.24-0.37 weight portion nano ferriferrous oxide composition.
Further, the inorganic diamante of above-mentioned one, it is characterised in that described organic oligomer is the silica-based envelope of triethoxy PFPE-the caprolactone of end.
Further, the inorganic diamante of above-mentioned one, described HMMM resin is CYMEL303；Institute The polysiloxane defoaming agent stated is enlightening height Foamex 840；Described Polycarbosilane be CFC key lab of the National University of Defense technology from The PCS that row is developed, Tan solid, fusing point is 210 DEG C, molecular weight 1500.
In order to prepare above-mentioned inorganic diamante, the latter solution that the present invention provides is such that
1) each component is weighed；
2) by organic oligomer, tetraethoxysilane, oxolane, Polycarbosilane, dimethylbenzene, nano-oxide filler, phthalein Ultramarine, n-butyl alcohol, ethylene glycol, tripropylene glycol butyl ether put into ball mill, and ball milling disperses, and obtains premix material；
3) by step 2) the premix material ultrasonic vibration prepared 4 hours, add step 1) sodium hexameta phosphate weighed, poly-silica Alkane defoamer and chelating agen stirring 20min, mix homogeneously, obtain stand-by slurry；
4) by step 3) slurry prepared, pour in the oil groove of dry type coating machine, get the thick mylar of thickness 20-25um ready, Under 240 DEG C of environment, coated machine works, and slurry is coated on the top layer of mylar, dries and be formed under 180 DEG C of environment Machine slurry coating layer, organic ink coating thickness is 20-25um, after coating, constant temperature 1h, warp under 200 DEG C of environment Cross stripping machine to peel off, coiled stand-by；
5) by coiled organic ink coating layer, heated in argon gas atmosphere stove, cracking, it is thin that de-liberation of hydrogen becomes inorganic transparent Film；
6) the inorganic transparent thin film after cracking, being sent into continuous vacuum coating machine, aluminizer thickness 30-60nm, through coating Two-sided color coated by machine, is cutting into difformity.
Further, the preparation method of above-mentioned inorganic diamante, step 2) described in method particularly as follows: first by step 1) The organic oligomer weighed, tetraethoxysilane and 8-12 part oxolane add ball mill, and ball milling disperses 5-7 hour, obtains pre- Batch mixing A；Then by step 1) Polycarbosilane, dimethylbenzene and the step 2 that weigh) remaining oxolane adds ball mill, ball Mill dispersion 1.5-2.5 hour, obtains premix material B；Again by step 1) described in nano-oxide filler, phthalocyanine blue, n-butyl alcohol, Ethylene glycol, tripropylene glycol butyl ether put into ball mill, and ball milling disperses 5-7 hour, obtains premix material C；By premix material A, premix Material B and premix material C mix homogeneously obtain premix material.
Further, the preparation method of above-mentioned inorganic diamante, step 3) in, adding sodium hexameta phosphate, polysiloxanes After defoamer and chelating agen are uniformly mixed, add the HMMM of formula ratio, ceria and zirconium and urge Dry agent also uses ultrasonic vibration 5 hours, obtains stand-by slurry.
Further, the preparation method of above-mentioned inorganic diamante, step 4) particularly as follows: by step 3) slurry prepared, fall Entering in the oil groove of dry type coating machine, get the thick mylar of thickness 20-25um ready, under 240 DEG C of environment, coated machine works, Slurry is coated on the top layer of mylar, dries under 180 DEG C of environment and form organic ink coating layer, organic ink coating layer Thickness is 20-25um, after coating, and constant temperature 2h under 120 DEG C of environment, then naturally cool to room temperature, be sent into freezer room, Cold preservation 2h under-20 DEG C of environment, after taking-up, is warming up to 200 DEG C under the speed of 5 DEG C/min, and constant temperature under 200 DEG C of environment 1h, finally naturally cools to room temperature, peels off through stripping machine, coiled stand-by.
Further, the preparation method of above-mentioned inorganic diamante, step 5) particularly as follows: by coiled organic ink coating Layer, in argon gas atmosphere stove, is first warming up to 300 DEG C from room temperature with the speed of 2 DEG C/min, cracks 0.5 hour, the most again Being warming up to 600-800 DEG C with the speed of 1-2 DEG C/min, crack 1h, de-liberation of hydrogen becomes inorganic transparent thin film.
Compared with prior art, the technical scheme that the present invention provides has a following technological merit:
1, Polycarbosilane gradually liberation of hydrogen more than 200 DEG C in the technical scheme that the present invention provides, is that Polycarbosilane is turned by organic material Turning to inorganic material, temperature rises network structure and rises；
2, Polycarbosilane, tetraethoxysilane and organic oligomer and nano-oxide hybridization compounding, is that thin layer solidifies rear surface Having " double thin ", i.e. hydrophobicity and oleophobic property, temperature brings up to 800 DEG C, and major ingredient liberation of hydrogen or deoxidation are complete, are converted into amorphous Silicon fiml.
3, nanometer rutile, zirconium oxide and the silicon dioxide that the present invention provides enhances anti-ultraviolet ability, prevents aging, subtracts Few film layer porosity 66%, increases wearability, makes film layer have non-slip；Ferric oxide, ferroso-ferric oxide and phthalocyanine blue produce Micro-interference of film, minimizing scattering；The interpolation of ethylene glycol helps the wettability of Nano filling；Tripropylene glycol butyl ether promotes nanometer Flavoring agent and major ingredient levelability improve；Sodium hexameta phosphate makes nano-oxide filler be easily dispersed, polysiloxane defoaming agent, 1,2-benzene And isothiazole-3-ketone improves the rate of drying of coating materials.
4, oxolane uses and separately grinds, and owing to the time is different, produces variable grain degree, makes course of reaction in rational speed Under carry out, contribute to Multicomponent reaction fully.
5, each component uses long-time ball milling respectively to coordinate long-time supersonic oscillations, makes each component especially nano-oxide effective Dispersion, both effective mix homogeneously, avoid again reuniting.Two ways combines so that the mixing of material is more uniform.
Sum it up, the technical scheme that provides of the present invention its do not melt at up to 800 degrees Celsius, transparency is high, is not limited by temperature System, density is at 1-1.4g/cm3In can reconcile, range is wide.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the claim of the present invention is described in further detail, but does not constitute the present invention Any restriction, the amendment of any limited number of time made in the claims in the present invention protection domain, still the present invention right want Within seeking protection domain.
Embodiment 1
The inorganic diamante of one that the present invention provides, is made up of the component of following weight: the PFPE of the silica-based end-blocking of triethoxy- Caprolactone 6kg, the PFPE of the silica-based end-blocking of described triethoxy-caprolactone Shi Liu state outstanding person, Li Jia, Sun Fang, Cheng Song, old Executing, the 7th whole nation functional fluorine silicon materials of 2009-and Coating Market exploitation and application " Wengfu blue sky cup " technical seminar are public PFPE-the caprolactone of the silica-based end-blocking of triethoxy opened；Tetraethoxysilane 11kg, Polycarbosilane 24kg, described is poly- Carbon silane is the PCS that CFC key lab of the National University of Defense technology develops voluntarily, Tan solid, and fusing point is 210 DEG C, molecular weight " aerospace material technique " Polycarbosilanes described in the 3rd phase in 2005 such as 1500, i.e. Chen Man China；3.16kg nano-titanium oxide (particle diameter 10nm), 3.3kg nano zircite (particle diameter 30nm), 2.28kg nano silicon (particle diameter 10nm), 0.50kg Nanometer iron sesquioxide (particle diameter 10nm)；0.24kg nano ferriferrous oxide (particle diameter 20nm), oxolane 16kg, diformazan Benzene 31kg, sodium hexameta phosphate 0.12kg, enlightening height Foamex 840 0.13kg, HMMM resin (CYMEL303) 0.16kg, 1,2-benzisothiazole-3-ketone 0.96kg, ceria 5kg, zirconium driers 0.04kg；0.01kg Phthalocyanine blue；1.6kg n-butyl alcohol；1.2kg ethylene glycol；0.02kg tripropylene glycol butyl ether.
Embodiment 2
The inorganic diamante of another kind that the present invention provides, is made up of the component of following weight: the perfluor of the silica-based end-blocking of triethoxy gathers Ether-caprolactone ester 4kg, the PFPE of the silica-based end-blocking of described triethoxy-caprolactone Shi Liu state outstanding person, Li Jia, Sun Fang, journey Pine, old executes, and the 7th whole nation functional fluorine silicon materials of 2009-and Coating Market exploitation and application " Wengfu blue sky cup " technology grind Beg for the PFPE-caprolactone of the disclosed silica-based end-blocking of triethoxy of meeting；Tetraethoxysilane 17kg, Polycarbosilane 16kg, 4.74kg nano-titanium oxide (particle diameter 10nm), 2.2kg nano zircite (particle diameter 30nm), 3.42kg nano silicon (grain Footpath 10nm), 0.33kg nanometer iron sesquioxide (particle diameter 10nm)；0.37kg nano ferriferrous oxide (particle diameter 20nm), four Hydrogen furan 24kg, dimethylbenzene 21kg, sodium hexameta phosphate 0.18kg, enlightening height Foamex 840 0.09-0.13kg, hexa methoxy Methyl melamine resin 0.24kg, 1,2-benzisothiazole-3-ketone 0.96kg, ceria 7.6kg, zirconium driers 0.02kg； 0.01kg phthalocyanine blue；2.4kg n-butyl alcohol；0.8kg ethylene glycol；0.02kg tripropylene glycol butyl ether.
Embodiment 3
The inorganic diamante of another kind that the present invention provides, is made up of the component of following weight: the perfluor of the silica-based end-blocking of triethoxy gathers Ether-caprolactone ester 5kg, the PFPE of the silica-based end-blocking of described triethoxy-caprolactone Shi Liu state outstanding person, Li Jia, Sun Fang, journey Pine, old executes, and the 7th whole nation functional fluorine silicon materials of 2009-and Coating Market exploitation and application " Wengfu blue sky cup " technology grind Beg for the PFPE-caprolactone of the disclosed silica-based end-blocking of triethoxy of meeting；Tetraethoxysilane 14kg, Polycarbosilane 20kg, 3.95kg nano-titanium oxide (particle diameter 10nm), 2.77kg nano zircite (particle diameter 30nm), 2.85kg nano silicon (grain Footpath 10nm), 0.42kg nanometer iron sesquioxide (particle diameter 10nm)；0.31kg nano ferriferrous oxide (particle diameter 20nm), dioxy SiClx 1kg, oxolane 20kg, dimethylbenzene 25kg, sodium hexameta phosphate 0.16kg, enlightening height Foamex 840 0.09kg, six Methoxy melmac 0.24kg, 1,2-benzisothiazole-3-ketone 0.64kg, ceria 7.6kg, zirconium is urged dry Agent 0.02kg；0.01kg phthalocyanine blue；2.4kg n-butyl alcohol；0.8kg ethylene glycol；0.02kg tripropylene glycol butyl ether.
In embodiment 1 to 3, the preparation method of any one a kind of inorganic diamante is as follows:
1) in embodiment 1 to 3, any one group of mass number weighs each component；
2) first by step 1) organic oligomer that weighs, tetraethoxysilane and 8-12 part oxolane add ball mill, Ball milling disperses 5-7 hour, obtains premix material A；Then by step 1) Polycarbosilane, dimethylbenzene and the step 2 that weigh) remaining Oxolane adds ball mill, and ball milling disperses 1.5-2.5 hour, obtains premix material B；Again by step 1) described in nano-oxide Filler, phthalocyanine blue, n-butyl alcohol, ethylene glycol, tripropylene glycol butyl ether put into ball mill, and ball milling disperses 6 hours, obtains premix Material C；Premix material A, premix material B and premix material C mix homogeneously are obtained premix material；
3) by step 2) the premix material ultrasonic vibration prepared 4 hours, add sodium hexameta phosphate, polysiloxane defoaming agent and chela After mixture is uniformly mixed, adds the HMMM of formula ratio, ceria and zirconium driers and use Ultrasonic wave concussion 5 hours, obtains stand-by slurry；
4) by step 3) slurry prepared, pour in the oil groove of dry type coating machine, get the thick mylar of thickness 20-25um ready, Under 240 DEG C of environment, coated machine works, and slurry is coated on the top layer of mylar, dries and be formed under 180 DEG C of environment Machine slurry coating layer, organic ink coating thickness is 20-25um, after coating, constant temperature 2h under 120 DEG C of environment, so After naturally cool to room temperature, be sent into freezer room, cold preservation 2h under-20 DEG C of environment, after taking-up, rise under the speed of 5 DEG C/min Temperature to 200 DEG C, and constant temperature 1h under 200 DEG C of environment, finally naturally cool to room temperature, peel off through stripping machine, coiled treat With；
5) by coiled organic ink coating layer, in argon gas atmosphere stove, first it is warming up to the speed of 2 DEG C/min from room temperature 300 DEG C, cracking 0.5 hour, be warming up to 600-800 DEG C with the speed of 1-2 DEG C/min the most again, crack 1h, de-liberation of hydrogen becomes Inorganic transparent thin film；
6) the inorganic transparent thin film after cracking, it is sent into continuous vacuum coating machine (1.8*10-2Pa；0.2nm/S), aluminize thickness Degree 30nm, coats two-sided color through coating machine, cuts into difformity further according to being actually needed, it is common that 0.1-3mm, The small pieces of wide 0.1-3mm.
Embodiment 4
The inorganic diamante of one that the present invention provides, is made up of the component of following weight number: the perfluor of the silica-based end-blocking of triethoxy gathers Ether-caprolactone ester 6kg, the PFPE of the silica-based end-blocking of described triethoxy-caprolactone Shi Liu state outstanding person, Li Jia, Sun Fang, journey Pine, old executes, and the 7th whole nation functional fluorine silicon materials of 2009-and Coating Market exploitation and application " Wengfu blue sky cup " technology grind Beg for the PFPE-caprolactone of the disclosed silica-based end-blocking of triethoxy of meeting；Tetraethoxysilane 11kg, Polycarbosilane 24kg, institute The Polycarbosilane stated is the PCS that CFC key lab of the National University of Defense technology develops voluntarily, Tan solid, and fusing point is 210 DEG C, point " aerospace material technique " Polycarbosilanes described in the 3rd phase in 2005 such as son measures 1500, i.e. Chen Man China；3.16kg nano oxygen Change titanium (particle diameter 10nm), 3.3kg nano zircite (particle diameter 30nm), 2.28kg nano silicon (particle diameter 10nm), 0. 50kg nanometer iron sesquioxide (particle diameter 10nm)；0.24kg nano ferriferrous oxide (particle diameter 20nm), silica 1 .2kg, Oxolane 16kg, dimethylbenzene 31kg, sodium hexameta phosphate 0.12kg, polysiloxane defoaming agent 0.13kg, 1,2-benzisothia Azoles-3-ketone 0.64kg, phthalocyanine blue 0.01kg, n-butyl alcohol 2.4kg, ethylene glycol 0.8kg and tripropylene glycol butyl ether 0.02kg.
Embodiment 5
The inorganic diamante of one that the present invention provides, is made up of the component of following weight number: the perfluor of the silica-based end-blocking of triethoxy gathers Ether-caprolactone ester 4kg, the PFPE of the silica-based end-blocking of described triethoxy-caprolactone Shi Liu state outstanding person, Li Jia, Sun Fang, journey Pine, old executes, and the 7th whole nation functional fluorine silicon materials of 2009-and Coating Market exploitation and application " Wengfu blue sky cup " technology grind Beg for the PFPE-caprolactone of the disclosed silica-based end-blocking of triethoxy of meeting；Tetraethoxysilane 17kg, Polycarbosilane 16kg, institute The Polycarbosilane stated is the PCS that CFC key lab of the National University of Defense technology develops voluntarily, Tan solid, and fusing point is 210 DEG C, point " aerospace material technique " Polycarbosilanes described in the 3rd phase in 2005 such as son measures 1500, i.e. Chen Man China；3.16kg nano oxygen Change titanium (particle diameter 10nm), 3.3kg nano zircite (particle diameter 30nm), 2.28kg nano silicon (particle diameter 10nm), 0. 50kg nanometer iron sesquioxide (particle diameter 10nm)；0.24kg nano ferriferrous oxide (particle diameter 20nm), silicon dioxide 0.8kg, Oxolane 24kg, dimethylbenzene 21kg, sodium hexameta phosphate 0.18kg, polysiloxane defoaming agent 0.09kg, 1,2-benzisothia Azoles-3-ketone 0.96kg, phthalocyanine blue 0.01kg, n-butyl alcohol 1.6kg, ethylene glycol 1.2kg and tripropylene glycol butyl ether 0.02kg.
1) in embodiment 4 to 5, any one group of mass number weighs each component；
2) by ethyl-silicone block PFPE-caprolactone ester, tetraethoxysilane, oxolane, Polycarbosilane, two Toluene, nano-oxide filler, phthalocyanine blue, n-butyl alcohol, ethylene glycol, tripropylene glycol butyl ether put into ball mill, and ball milling divides Dissipate, obtain premix material；
3) by step 2) the premix material ultrasonic vibration prepared 4 hours, add step 1) sodium hexameta phosphate weighed, poly-silica Alkane defoamer and chelating agen stirring 20min, mix homogeneously, obtain stand-by slurry；
4) by step 3) slurry prepared, pour in the oil groove of dry type coating machine, get the thick mylar of thickness 20-25um ready, Under 240 DEG C of environment, coated machine works, and slurry is coated on the top layer of mylar, dries and be formed under 180 DEG C of environment Machine slurry coating layer, organic ink coating thickness is 20-25um, after coating, constant temperature 1h, warp under 200 DEG C of environment Cross stripping machine to peel off, coiled stand-by；
5) by coiled organic ink coating layer, heated in argon gas atmosphere stove, cracking, it is thin that de-liberation of hydrogen becomes inorganic transparent Film；
6) the inorganic transparent thin film after cracking, it is sent into continuous vacuum coating machine (1.8*10-2Pa；0.2nm/S), aluminize thickness Degree 30nm, coats two-sided color through coating machine, cuts into difformity further according to being actually needed, it is common that 0.1-3mm, The small pieces of wide 0.1-3mm.
It should be noted that the parameter that is not shown in detail in of technical scheme provided in the present invention, all according to this area routine techniques hands Duan Jinhang.
In order to prove the technique effect of inorganic diamante that the present invention provides, the glittering present invention provided is conventional with on market to be dodged Paillette carries out fusing point test, and result see table.

Claims (10)

1. an inorganic diamante, it is characterised in that be mainly made up of following components in parts by weight: organic oligomer 4-6 part, Tetraethoxysilane 11-17 part, Polycarbosilane 16-24 part, nano-oxide filler 8-12 part, silicon dioxide 0.8-1.2 part, Oxolane 16-24 part, dimethylbenzene 21-31 part, sodium hexameta phosphate 0.12-0.18 part, polysiloxane defoaming agent 0.09-0.13 Part, 1,2-benzisothiazole-3-ketone 0.64-0.96 part, phthalocyanine blue 0.01 part, n-butyl alcohol 1.6-2.4 part, ethylene glycol 0.8-1.2 part and tripropylene glycol butyl ether 0.02 part.
The inorganic diamante of one the most according to claim 1, it is characterised in that also include 5-7.6 parts by weight of cerium oxide, 0.02-0.04 weight portion zirconium driers and 0.16-0.24 weight portion HMMM resin.
The inorganic diamante of one the most according to claim 1, it is characterised in that described nano-oxide filler by 3.16-4.74 weight portion nano-titanium oxide, 2.2-3.3 weight portion nano zircite, 2.28-3.42 weight portion nano silicon, 0.33-0.50 weight portion nanometer iron sesquioxide and 0.24-0.37 weight portion nano ferriferrous oxide composition.
The inorganic diamante of one the most according to claim 1, it is characterised in that described organic oligomer is triethoxy PFPE-the caprolactone of silica-based end-blocking.
The inorganic diamante of one the most according to claim 1, it is characterised in that described HMMM Resin is CYMEL303；Described polysiloxane defoaming agent is enlightening height Foamex 840；Described Polycarbosilane is that science and techniques of defence are big Learning the PCS that CFC key lab develops voluntarily, Tan solid, fusing point is 210 DEG C, molecular weight 1500.
6. the method for the inorganic diamante prepared described in claim 1, it is characterised in that comprise the steps: successively
1) weight portion as described in claim 1 weighs each component；
2) by organic oligomer, tetraethoxysilane, oxolane, Polycarbosilane, dimethylbenzene, nano-oxide filler, phthalein Ultramarine, n-butyl alcohol, ethylene glycol, tripropylene glycol butyl ether put into ball mill, and ball milling disperses, and obtains premix material；
3) by step 2) the premix material ultrasonic vibration prepared 4 hours, add step 1) sodium hexameta phosphate weighed, poly-silica Alkane defoamer and chelating agen stirring 20min, mix homogeneously, obtain stand-by slurry；
4) by step 3) slurry prepared, pour in the oil groove of dry type coating machine, get the thick mylar of thickness 20-25um ready, Under 240 DEG C of environment, coated machine works, and slurry is coated on the top layer of mylar, dries and be formed under 180 DEG C of environment Machine slurry coating layer, organic ink coating thickness is 20-25um, after coating, constant temperature 1h, warp under 200 DEG C of environment Cross stripping machine to peel off, coiled stand-by；
5) by coiled organic ink coating layer, heated in argon gas atmosphere stove, cracking, it is thin that de-liberation of hydrogen becomes inorganic transparent Film；
6) the inorganic transparent thin film after cracking, being sent into continuous vacuum coating machine, aluminizer thickness 30-60nm, through coating Two-sided color coated by machine, is cutting into difformity.
The preparation method of inorganic diamante the most according to claim 6, it is characterised in that step 2) described in method tool Body is: first by step 1) organic oligomer that weighs, tetraethoxysilane and 8-12 part oxolane add ball mill, ball Mill dispersion 5-7 hour, obtains premix material A；Then by step 1) Polycarbosilane, dimethylbenzene and the step 2 that weigh) remaining four Hydrogen furan adds ball mill, and ball milling disperses 1.5-2.5 hour, obtains premix material B；Again by step 1) described in nano-oxide fill out Material, phthalocyanine blue, n-butyl alcohol, ethylene glycol, tripropylene glycol butyl ether put into ball mill, and ball milling disperses 5-7 hour, obtains premix Material C；Premix material A, premix material B and premix material C mix homogeneously are obtained premix material.
The preparation method of inorganic diamante the most according to claim 6, it is characterised in that step 3) in, adding six After Polymeric sodium metaphosphate., polysiloxane defoaming agent and chelating agen are uniformly mixed, add the hexamethoxy methyl melamine of formula ratio Amine, ceria and zirconium driers also use ultrasonic vibration 5 hours, obtain stand-by slurry.
The preparation method of inorganic diamante the most according to claim 6, it is characterised in that step 4) particularly as follows: will step Rapid 3) slurry prepared, pours in the oil groove of dry type coating machine, gets the thick mylar of thickness 20-25um ready, at 240 DEG C of rings Under border, coated machine works, and slurry is coated on the top layer of mylar, dries and form organic ink painting under 180 DEG C of environment Layer of cloth, organic ink coating thickness is 20-25um, and after coating, under 120 DEG C of environment, constant temperature 2h, the coldest But to room temperature, it is sent into freezer room, cold preservation 2h under-20 DEG C of environment, after taking-up, under the speed of 5 DEG C/min, is warming up to 200 DEG C, And under 200 DEG C of environment constant temperature 1h, finally naturally cool to room temperature, through stripping machine peel off, coiled stand-by.
The preparation method of inorganic diamante the most according to claim 6, it is characterised in that step 5) particularly as follows: will Coiled organic ink coating layer, in argon gas atmosphere stove, is first warming up to 300 DEG C from room temperature with the speed of 2 DEG C/min, Cracking 0.5 hour, be warming up to 600-800 DEG C with the speed of 1-2 DEG C/min the most again, crack 1h, de-liberation of hydrogen becomes inorganic transparent Thin film.
CN201610309371.7A 2016-05-10 2016-05-10 A kind of inorganic diamante and preparation method thereof Active CN105885689B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610309371.7A CN105885689B (en) 2016-05-10 2016-05-10 A kind of inorganic diamante and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610309371.7A CN105885689B (en) 2016-05-10 2016-05-10 A kind of inorganic diamante and preparation method thereof

Publications (2)

Publication Number Publication Date
CN105885689A true CN105885689A (en) 2016-08-24
CN105885689B CN105885689B (en) 2018-01-09

Family

ID=56703576

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610309371.7A Active CN105885689B (en) 2016-05-10 2016-05-10 A kind of inorganic diamante and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105885689B (en)

Citations (5)

* Cited by examiner, † Cited by third party
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
JP2005159032A (en) * 2003-11-26 2005-06-16 Jsr Corp Insulating film, its forming method, composition for forming the same, laminate having the same, and its forming method
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
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
JP2005159032A (en) * 2003-11-26 2005-06-16 Jsr Corp Insulating film, its forming method, composition for forming the same, laminate having the same, and its forming method
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

Also Published As

Publication number Publication date
CN105885689B (en) 2018-01-09

Similar Documents

Publication Publication Date Title
CN105623506B (en) Ceramic base composite coating and preparation method thereof
CN103911024B (en) Glass pigment micro powder, dispersion liquid, ink-jet ink and forming method thereof
CN103224726B (en) Glaze ink with leather pattern effect for ceramic jet printing and preparation method thereof
CN100378035C (en) Boride-silicon carbide multiple phase ceramic and its preparation method
CN103551497B (en) A kind of production method of cast iron alcohol radical Flow Coating
CN106380979A (en) Silicone-acrylic weather-resistant reflective heat-insulation natural stone paint and preparation method thereof
CN109266080B (en) Water-based smokeless and odorless inorganic nano ceramic fireproof coating and preparation method thereof
CN107021787A (en) A kind of preparation method of anti-yaw damper coating
CN103224724B (en) Metal glaze printing ink for ceramic ink-jet printing and preparation method thereof
Qian-Gang et al. Oxidation protective glass coating for SiC coated carbon/carbon composites for application at 1773 K
CN103483963B (en) A kind of multi-functional batch of scratch-type single, double component heat insulating coatings and preparation method thereof
CN109868056B (en) Melting erosion-resistant ablation coating and preparation method thereof
CN106497313B (en) A kind of high temperature resistant microwave absorbing coating and its application
CN104673091A (en) RTV anti-pollution flashover coating suitable for automatic dip-coating of insulator and preparation method of RTV anti-pollution flashover coating
CN109796870A (en) Can the porcelainization silicon rubber composite material of resistance to ablation coating and its coating preparation method
CN104861866A (en) Heat-resistant paint and preparation method thereof
CN107815003A (en) A kind of high insulating refractory polyolefin/graphene semiconductive composite and preparation method thereof
CN115851070A (en) Anti-oxidation ablation-resistant coating and preparation method thereof
CN105885689A (en) Inorganic sequin and preparation method thereof
CN105482552A (en) White glass ink used for ink-jet printing and preparation method thereof
CN102924985B (en) Smoke-free and tasteless inorganic nano high-temperature resistant anti-corrosive wear-resistant paint and preparation method thereof
CN107245254A (en) The preparation method and its coating of the silicon nitride ceramics coating material of heat-insulating flame-retardant
CN104987834B (en) Scratch-resistant glass coating
CN104418577B (en) A kind of aerosil is modified the preparation method of external thermal insulation block of glass wool
CN107880544A (en) A kind of high-impact brush can ceramic flame-retarded resin and preparation method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant