CN108864971A - A kind of preparation method of automobile-used rupture pressure disc - Google Patents
A kind of preparation method of automobile-used rupture pressure disc Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
- C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09J179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive
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- C09J2479/00—Presence of polyamine or polyimide
Abstract
The invention belongs to rupture pressure disc preparation technical fields, and in particular to a kind of preparation method of automobile-used rupture pressure disc.Tea Saponin can make water-oil separating in explosion-proof film surface, and there is good cleaning effect to film surface, anti-reflection film liquid of the invention can form titanium dioxide/vanadium dioxide composite film, vanadium dioxide crystal layer can obstruct the infrared light of high-energy, film layer is improved to the transmitance of visible light, there is temperature regulating power simultaneously, heat insulation is good, internal stress between aluminium ion and zinc ion increases, inhibit the growth of zinc oxide grain, to make the impurity scattering center formed in film reduce, visible light transmittance increases, under the conditions of high-intensity illumination, absorb the grain dispersion ordered arrangement that the carrier of luminous energy can assemble indium oxide and tin oxide, it is improved the consistency of crystal grain, so as to reduce the light intensity for injecting car of external light source, it has a extensive future.
Description
Technical field
The invention belongs to rupture pressure disc preparation technical fields, and in particular to a kind of preparation method of automobile-used rupture pressure disc.
Background technique
With the quickening of Urbanization in China, more and more automobiles are entered in our daily lifes, become daily life
Indispensable a part living.
Currently, automobile front-window and side vehicle window be all made of glass, vehicle glass the keeping out the wind of automobile, rain cover and
It all plays an important role in daylighting, is the important leverage that driver safety drives.But the sunlight outside glass will affect
The vision of driver, and can make to increase rapidly in the temperature short time in automobile, it is more serious, when accident occurs,
Broken glass, which is dispersed, can injure interior driver and passenger and periphery personnel.Therefore, it is necessary to stick one layer of rupture pressure disc on vehicle glass,
Good heat-proof quality is played, while can be improved the security performance of vehicle glass.
Rupture pressure disc is mounted in digital electronic goods display screen, automobile industry control display screen, shield glass, industrial work
Control one layer of rupture pressure disc with function on display screen.Summer hot weather, can be heat-insulated after pad pasting, and can save cold air energy
Source.Wintry weather cold wet can be reduced energy loss after pad pasting, keep vehicle interior temperature, moreover it is possible to play the work of barrier ultraviolet light
With；It can reduce dazzle after pad pasting, guarantee driving safety, comfortable；The base security of film can prevent splashing glass, guarantee safety.This
Outside, moreover it is possible to play the role of protecting privacy, prevent from peeping.
PET has the characteristics that excellent resistance to chemical reagents, heat resistance, electric property, mechanical property and insulating properties are good, therefore
To extensive use.Wherein PET film is because of its excellent tensile strength, good electrical insulation capability, cold resistance, heat resistance and receipts
Contracting stability etc., so that it can be used in various products application.Such as：Solar film, antistatic film, LED illumination film, liquid
Crystalline substance display film and film for packaging etc..But since the surface hardness of PET material is low, alkali resistance is poor, wears no resistance and resistance to molten
The disadvantages of agent is poor, so that the application of PET film is very limited.
Current rupture pressure disc be usually be made of release layer, hardened layer etc., between using optical glue bond.It was using
It is found in journey, the rupture pressure disc of existing manufacture craft production, the quality of adhesive force between layers, peeling force and integral membrane is not
Enough ideals, light transmittance is not high, and usually just needs replacing after a period of use.It additionally, there may be poor transparency, weatherability
Difference, antiultraviolet is inadequate, heat insulation is poor, it is low that internal light, surface hardness cannot be adjusted according to the power of external light source, intolerant to
The defects of mill.
Therefore, it is necessary to develop, a kind of raw material sources are wide, universality is high, meet the rupture pressure disc of different explosive-proof gradves with important
Meaning.
Summary of the invention
Present invention mainly solves the technical issues of, for current existing automobile-used rupture pressure disc, transparency is not high, and heat insulation is poor, no
A kind of preparation method of automobile-used rupture pressure disc can be provided according to the defect of the strong and weak adjustment internal light of external light source.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of preparation method of automobile-used rupture pressure disc, it is characterised in that specifically preparation step is：
（1）5~6g vanadic anhydride is mixed with 14~15g oxalic acid solution, obtains liquid to be restored, by liquid to be restored and anhydrous second
Alcohol mixing, is put into four-hole boiling flask, is stirred to react under condition of water bath heating with the revolving speed of 200~220r/min, obtains dioxy
Change vanadium forerunner coating liquid；
（2）40~50mL dehydrated alcohol is added into ultrasonic disperse instrument and 20~30mL butyl titanate, ultrasonic disperse are dispersed
Dispersion liquid is placed in the three-necked flask with blender and dropping funel, 20 is added into three-necked flask with dropping funel by liquid
~25mL reconciles liquid, while starting blender, starts to be stirred to react to obtain titanium dioxide with the revolving speed of 200~300r/min molten
Glue；
（3）Hydrogen peroxide is mixed with vanadium dioxide forerunner's coating liquid, oxidation coating liquid is obtained, according to parts by weight, by 8~10 parts
Zinc oxide, 15~20 parts of Tea Saponins, 40~45 parts of oxidation coating liquids, 10~12 parts of TiO 2 sols are added to 80~90 parts of second
In acetoacetic ester, mixed liquor is obtained, then mixed liquor is placed in high speed disperser, high speed dispersion, obtain anti-reflection film liquid；
（4）According to parts by weight, by 10~12 parts of stannous sulfates, 20~25 parts of ethylenediamine tetra-acetic acids and 6~10 parts of potassium hydroxide
It is added in the beaker equipped with 80~90 parts of deionized waters, stirs 30~35min, obtain complexing stannous sulfate solution, to complexing sulphur
4~5 parts of polyvinylpyrrolidonepowder powders are added in sour stannous solution, heat temperature raising stirs to get reducing solution；
（5）4~5g potassium chlorate, 8~10g potassium hydroxide, the mixing of 6~8g indium hydroxide are taken, 200~230mL deionized water is added
In, 20~25min is mixed, obtains oxidation solution, oxygen is added into the above-mentioned reducing solution of 800~900mL with dropping funel
Change solution, is stirred to react, obtains reaction solution；
（6）Above-mentioned reaction solution is placed in ultrasonic reaction machine, ultrasonic reaction obtains reaction product, and reaction product is placed in high speed
Centrifugal treating in centrifuge removes supernatant liquor, and precipitating is put into vacuum drying oven by isolated lower sediment, dry, obtains
Superfine tin indium oxide powder；
（7）According to parts by weight, by 20~25 parts of superfine tin indium oxide powder, 10~15 parts of zinc oxide, 30~33 part of nine hydration nitre
Sour aluminium mixes in 60~75 parts of polyamic acid colloidal sols, is dispersed with stirring 20~25min, obtains electrically conducting transparent glue, PET film just
Face is coated with a thickness electrically conducting transparent glue with coater, forms conductive light modulation film layer, then that anti-reflection film liquid is coated on PET film is anti-
Face forms antireflective coating, and finally drying sticks release paper and obtains automobile-used rupture pressure disc.
Step（1）The mass fraction of the oxalic acid solution is 20%, and liquid to be restored and dehydrated alcohol mixed volume ratio are 1 ︰
5, being stirred to react the time is 14~15h, and control bath temperature is 80~90 DEG C.
Step（2）The ultrasonic disperse power is 150~200W, and the ultrasonic disperse time is 4~6min, dropping funel drop
Rate of acceleration is 2~3mL/min, reconciles liquid to be the nitric acid solution for being 20% by mass fraction and n,N-Dimethylformamide by volume
Than forming for 5 ︰, 1 mixed preparing, being stirred to react the time is 50~55min.
Step（3）Described is 1 ︰ 2, high speed dispersion revolving speed by hydrogen peroxide and vanadium dioxide forerunner coating liquid mixed volume ratio
For 4000~4500r/min, the high speed dispersion time is 18~20min.
Step（4）Temperature is 40~50 DEG C after the heat temperature raising, and polyvinylpyrrolidonepowder powder is complete at the end of stirring
Fully dissolved.
Step（5）The dropping funel drop rate is 10~15mL/min, and being stirred to react the time is 40~45min.
Step（6）The supersonic frequency of the ultrasonic reaction machine is 25~30kHz, and the ultrasonic reaction time is 3~4h, high speed
Centrifuge speed is 5000~6000r/min, and the centrifugal treating time is 10~15min, and vacuum drying oven set temperature is 70~80
DEG C, drying time is 5~6h.
Step（7）The mass fraction of the polyamic acid colloidal sol is 20%, and PET film is transparent with a thickness of 0.1~0.2mm
Conductive gelatin is with a thickness of 20~30 μm, and antireflective coating is with a thickness of 10~15mm.
The beneficial effects of the invention are as follows：
（1）Vanadium dioxide forerunner's coating liquid is prepared with thermal reduction in vanadic anhydride by the present invention, using tetraethyl titanate and
Ethyl alcohol is that raw material ultrasonic disperse obtains dispersion liquid, then is reconciled to obtain TiO 2 sol with conciliation liquid, finally by hydrogen peroxide and two
The mixing of vanadium oxide forerunner's coating liquid obtains oxidation coating liquid, by multi-walled carbon nanotube, Tea Saponin, oxidation coating liquid, titanium dioxide
Colloidal sol is added in ethyl acetate, is dispersed in high speed disperser high speed, is obtained automatically cleaning anti-reflection film coating liquid, Tea Saponin is in dioxygen
Under the oxidation processes effect of water, surface can carry many hydrophilic radicals, will form cluster after reaching a certain concentration, cluster can be by two
Vanadium oxide crystal layer cladding, protection vanadium dioxide crystal layer is not oxidized, and Tea Saponin molecule is by hydrophilic sugared body and hydrophobic
Coordinating group is constituted, and can make water-oil separating in explosion-proof film surface, and have good cleaning effect, the present invention to film surface
Anti-reflection film liquid can form titanium dioxide/vanadium dioxide composite film, vanadium dioxide crystal layer can obstruct the infrared light of high-energy,
Film layer can be improved to the transmitance of visible light in titanium dioxide, tool when film layer being made to be applied to glass while to enhance light transmission features
There is temperature regulating power, heat insulation is good；
（2）Contain zinc oxide in the present invention in electrically conducting transparent glue, and is mixed with ANN aluminium nitrate nonahydrate, during the drying and film forming process,
The band gap and exciton bind energy of zinc oxide are larger, conduction light modulation film layer in transparency increase, due to aluminum ions concentration compared with
Height, the internal stress between aluminium ion and zinc ion increase, it is suppressed that the growth of zinc oxide grain, to make to be formed in film miscellaneous
Matter scattering center reduces, impurity scattering declines, and the visible light transmittance of film increases, current-carrying attached bag in conduction light modulation film layer
Two sources are included, first is that the Lacking oxygen in light modulation film layer, the electronics occupied originally by oxygen have very weak binding energy, inhale at room temperature
It receives luminous energy and is detached from constraint as free carrier, second is that zinc ion generates electronic carrier in Al-doping replacement lattice, carry
Stream increases with the raising of Al-doping concentration, and resistivity declines therewith, under the conditions of high-intensity illumination, absorbs luminous energy
The grain dispersion ordered arrangement that carrier can assemble indium oxide and tin oxide, is improved the consistency of crystal grain, thus
It can reduce the interior light intensity of the injection of external light source, have a extensive future.
Specific embodiment
5~6g vanadic anhydride is mixed with the oxalic acid solution that 14~15g mass fraction is 20%, obtains liquid to be restored, it will
Liquid to be restored is that 1 ︰ 5 is mixed with dehydrated alcohol by volume, is put into four-hole boiling flask, under condition of water bath heating with 200~
The revolving speed of 220r/min is stirred to react 14~15h, and control bath temperature is 80~90 DEG C, obtains vanadium dioxide forerunner's coating liquid；
40~50mL dehydrated alcohol and 20~30mL butyl titanate are added into ultrasonic disperse instrument, control ultrasonic power is 150~200W,
4~6min of ultrasonic disperse, obtains dispersion liquid, dispersion liquid is placed in the three-necked flask with blender and dropping funel, with drop
Liquid funnel is added 20~25mL into three-necked flask with the drop rate of 2~3mL/min and reconciles liquid, wherein reconciling liquid as quality point
Number is 20% nitric acid solution and n,N-Dimethylformamide is that 5 ︰, 1 mixed preparing forms, while starting blender by volume, with
The revolving speed of 200~300r/min, which starts to be stirred to react 50~55min, obtains TiO 2 sol；Before hydrogen peroxide and vanadium dioxide
Drive coating liquid is 1 ︰ 2 mixing by volume, oxidation coating liquid is obtained, according to parts by weight, by 8~10 parts of zinc oxide, 15~20
Part Tea Saponin, 40~45 parts of oxidation coating liquids, 10~12 parts of TiO 2 sols are added in 80~90 parts of ethyl acetate, are obtained
Mixed liquor, then mixed liquor is placed in high speed disperser, with revolving speed 18~20min of high speed dispersion of 4000~4500r/min, obtain
To anti-reflection film liquid；According to parts by weight, by 10~12 parts of stannous sulfates, 20~25 parts of ethylenediamine tetra-acetic acids and 6~10 parts of hydrogen-oxygens
Change potassium to be added in the beaker equipped with 80~90 parts of deionized waters, stir 30~35min, complexing stannous sulfate solution is obtained, to network
It closes and 4~5 parts of polyvinylpyrrolidonepowder powders is added in stannous sulfate solution, be heated to 40~50 DEG C, stirring to polyethylene
Pyrrolidinone powders are completely dissolved, and obtain reducing solution；Take 4~5g potassium chlorate, 8~10g potassium hydroxide, 6~8g indium hydroxide
Mixing is added in 200~230mL deionized water, and 20~25min is mixed, and obtains oxidation solution, with dropping funel with 10~
Oxidation solution is added into the above-mentioned reducing solution of 800~900mL, is stirred to react 40~45min for the drop rate of 15mL/min,
Obtain reaction solution；Above-mentioned reaction solution is placed in ultrasonic reaction machine, the supersonic frequency of control ultrasonic reaction machine is 25~30kHz,
3~4h of ultrasonic reaction, obtains reaction product, and reaction product is placed in the revolving speed in supercentrifuge with 5000~6000r/min
10~15min of centrifugal treating removes supernatant liquor, and isolated lower sediment, it is 70~80 DEG C that precipitating, which is put into set temperature,
Vacuum drying oven in, dry 5~6h obtains superfine tin indium oxide powder；According to parts by weight, by 20~25 parts of superfine tin indium oxides
Powder, 10~15 parts of zinc oxide, 30~33 parts of ANN aluminium nitrate nonahydrates mix the polyamic acid colloidal sol that 60~75 parts of mass fractions are 20%
In, it is dispersed with stirring 20~25min, obtains electrically conducting transparent glue, in the PET film front coater with a thickness of 0.1~0.2mm
Being coated with a layer thickness is 20~30 μm of electrically conducting transparent glue, forms conductive light modulation film layer, then that anti-reflection film liquid is coated on PET is thin
Film reverse side forms the antireflective coating of 10~15mm, and finally drying sticks release paper and obtains automobile-used rupture pressure disc.
Example 1
The oxalic acid solution that 5g vanadic anhydride and 14g mass fraction are 20% mix, liquid to be restored is obtained, by liquid to be restored and
Dehydrated alcohol is 1 ︰ 5 mixing by volume, is put into four-hole boiling flask, is stirred under condition of water bath heating with the revolving speed of 200r/min
14h is reacted, control bath temperature is 80 DEG C, obtains vanadium dioxide forerunner's coating liquid；It is anhydrous that 40mL is added into ultrasonic disperse instrument
Ethyl alcohol and 20mL butyl titanate, control ultrasonic power are 150W, ultrasonic disperse 4min, obtain dispersion liquid, dispersion liquid is placed in band
In the three-necked flask for having blender and dropping funel, it is added with the drop rate of 2mL/min into three-necked flask with dropping funel
20mL reconciles liquid, wherein it be 20% nitric acid solution and n,N-Dimethylformamide is 5 ︰ 1 mixed that reconcile liquid be mass fraction by volume
Conjunction is formulated, while starting blender, is started to be stirred to react 50min with the revolving speed of 200r/min and is obtained TiO 2 sol；
With vanadium dioxide forerunner coating liquid by volume it is that 1 ︰ 2 is mixed by hydrogen peroxide, oxidation coating liquid is obtained, according to parts by weight, by 8
Part zinc oxide, 15 parts of Tea Saponins, 40 parts of oxidation coating liquids, 10 parts of TiO 2 sols are added in 80 parts of ethyl acetate, are obtained
Mixed liquor, then mixed liquor is placed in high speed disperser, with the revolving speed high speed dispersion 18min of 4000r/min, obtain anti-reflection film
Liquid；According to parts by weight, by 10 parts of stannous sulfates, 20 parts of ethylenediamine tetra-acetic acids and 6 parts of potassium hydroxide be added equipped with 80 parts go from
In the beaker of sub- water, 30min is stirred, obtains complexing stannous sulfate solution, 4 parts of polyethylene are added into complexing stannous sulfate solution
Pyrrolidinone powders are heated to 40 DEG C, and stirring is completely dissolved to polyvinylpyrrolidonepowder powder, obtains reducing solution；It takes
4g potassium chlorate, 8g potassium hydroxide, the mixing of 6g indium hydroxide, are added in 200mL deionized water, 20min are mixed, is aoxidized
Oxidation solution is added into the above-mentioned reducing solution of 800mL with dropping funel with the drop rate of 10mL/min for solution, and stirring is anti-
40min is answered, reaction solution is obtained；Above-mentioned reaction solution is placed in ultrasonic reaction machine, the supersonic frequency of control ultrasonic reaction machine is
25kHz, ultrasonic reaction 3h, obtains reaction product, and reaction product is placed in supercentrifuge and is centrifuged with the revolving speed of 5000r/min
10min is handled, supernatant liquor is removed, precipitating is put into the vacuum drying oven that set temperature is 70 DEG C by isolated lower sediment,
Dry 5h, obtains superfine tin indium oxide powder；According to parts by weight, by 20 parts of superfine tin indium oxide powder, 10 parts of zinc oxide, 30 part nine
Nitric hydrate aluminium mixes in the polyamic acid colloidal sol that 60 parts of mass fractions are 20%, is dispersed with stirring 20min, obtains electrically conducting transparent glue
Liquid is coated with the electrically conducting transparent glue that a layer thickness is 20 μm with coater in the PET film front with a thickness of 0.1mm, and formation is led
Electricity light modulation film layer, then anti-reflection film liquid is coated on PET film reverse side, the antireflective coating of 10mm is formed, finally drying is sticked release
Paper obtains automobile-used rupture pressure disc.
Example 2
The oxalic acid solution that 5g vanadic anhydride and 14g mass fraction are 20% mix, liquid to be restored is obtained, by liquid to be restored and
Dehydrated alcohol is 1 ︰ 5 mixing by volume, is put into four-hole boiling flask, is stirred under condition of water bath heating with the revolving speed of 210r/min
14h is reacted, control bath temperature is 85 DEG C, obtains vanadium dioxide forerunner's coating liquid；It is anhydrous that 45mL is added into ultrasonic disperse instrument
Ethyl alcohol and 25mL butyl titanate, control ultrasonic power are 175W, ultrasonic disperse 5min, obtain dispersion liquid, dispersion liquid is placed in band
In the three-necked flask for having blender and dropping funel, it is added with the drop rate of 2mL/min into three-necked flask with dropping funel
23mL reconciles liquid, wherein it be 20% nitric acid solution and n,N-Dimethylformamide is 5 ︰ 1 mixed that reconcile liquid be mass fraction by volume
Conjunction is formulated, while starting blender, is started to be stirred to react 53min with the revolving speed of 250r/min and is obtained TiO 2 sol；
With vanadium dioxide forerunner coating liquid by volume it is that 1 ︰ 2 is mixed by hydrogen peroxide, oxidation coating liquid is obtained, according to parts by weight, by 9
Part zinc oxide, 17 parts of Tea Saponins, 43 parts of oxidation coating liquids, 11 parts of TiO 2 sols are added in 85 parts of ethyl acetate, are obtained
Mixed liquor, then mixed liquor is placed in high speed disperser, with the revolving speed high speed dispersion 19min of 4250r/min, obtain anti-reflection film
Liquid；According to parts by weight, by 11 parts of stannous sulfates, 23 parts of ethylenediamine tetra-acetic acids and 8 parts of potassium hydroxide be added equipped with 85 parts go from
In the beaker of sub- water, 33min is stirred, obtains complexing stannous sulfate solution, 4 parts of polyethylene are added into complexing stannous sulfate solution
Pyrrolidinone powders are heated to 45 DEG C, and stirring is completely dissolved to polyvinylpyrrolidonepowder powder, obtains reducing solution；It takes
4g potassium chlorate, 9g potassium hydroxide, the mixing of 7g indium hydroxide, are added in 215mL deionized water, 23min are mixed, is aoxidized
Oxidation solution is added into the above-mentioned reducing solution of 850mL with dropping funel with the drop rate of 13mL/min for solution, and stirring is anti-
43min is answered, reaction solution is obtained；Above-mentioned reaction solution is placed in ultrasonic reaction machine, the supersonic frequency of control ultrasonic reaction machine is
28kHz, ultrasonic reaction 3h, obtains reaction product, and reaction product is placed in supercentrifuge and is centrifuged with the revolving speed of 5500r/min
13min is handled, supernatant liquor is removed, precipitating is put into the vacuum drying oven that set temperature is 75 DEG C by isolated lower sediment,
Dry 5h, obtains superfine tin indium oxide powder；According to parts by weight, by 23 parts of superfine tin indium oxide powder, 13 parts of zinc oxide, 31 part nine
Nitric hydrate aluminium mixes in the polyamic acid colloidal sol that 68 parts of mass fractions are 20%, is dispersed with stirring 23min, obtains electrically conducting transparent glue
Liquid is coated with the electrically conducting transparent glue that a layer thickness is 25 μm with coater in the PET film front with a thickness of 0.1mm, and formation is led
Electricity light modulation film layer, then anti-reflection film liquid is coated on PET film reverse side, the antireflective coating of 13mm is formed, finally drying is sticked release
Paper obtains automobile-used rupture pressure disc.
Example 3
The oxalic acid solution that 6g vanadic anhydride and 15g mass fraction are 20% mix, liquid to be restored is obtained, by liquid to be restored and
Dehydrated alcohol is 1 ︰ 5 mixing by volume, is put into four-hole boiling flask, is stirred under condition of water bath heating with the revolving speed of 220r/min
15h is reacted, control bath temperature is 90 DEG C, obtains vanadium dioxide forerunner's coating liquid；It is anhydrous that 50mL is added into ultrasonic disperse instrument
Ethyl alcohol and 30mL butyl titanate, control ultrasonic power are 200W, ultrasonic disperse 6min, obtain dispersion liquid, dispersion liquid is placed in band
In the three-necked flask for having blender and dropping funel, it is added with the drop rate of 3mL/min into three-necked flask with dropping funel
25mL reconciles liquid, wherein it be 20% nitric acid solution and n,N-Dimethylformamide is 5 ︰ 1 mixed that reconcile liquid be mass fraction by volume
Conjunction is formulated, while starting blender, is started to be stirred to react 55min with the revolving speed of 300r/min and is obtained TiO 2 sol；
With vanadium dioxide forerunner coating liquid by volume it is that 1 ︰ 2 is mixed by hydrogen peroxide, obtains oxidation coating liquid, it according to parts by weight, will
10 parts of zinc oxide, 20 parts of Tea Saponins, 45 parts of oxidation coating liquids, 12 parts of TiO 2 sols are added in 90 parts of ethyl acetate, are obtained
It is placed in high speed disperser to mixed liquor, then by mixed liquor, with the revolving speed high speed dispersion 20min of 4500r/min, obtains anti-reflection film
Liquid；According to parts by weight, by 12 parts of stannous sulfates, 25 parts of ethylenediamine tetra-acetic acids and 10 parts of potassium hydroxide be added equipped with 90 parts go from
In the beaker of sub- water, 35min is stirred, obtains complexing stannous sulfate solution, 5 parts of polyethylene are added into complexing stannous sulfate solution
Pyrrolidinone powders are heated to 50 DEG C, and stirring is completely dissolved to polyvinylpyrrolidonepowder powder, obtains reducing solution；It takes
5g potassium chlorate, 10g potassium hydroxide, the mixing of 8g indium hydroxide, are added in 230mL deionized water, 25min are mixed, obtains oxygen
Change solution, with dropping funel with the drop rate of 15mL/min, oxidation solution be added into the above-mentioned reducing solution of 800~900mL,
It is stirred to react 45min, obtains reaction solution；Above-mentioned reaction solution is placed in ultrasonic reaction machine, the supersonic frequency of ultrasonic reaction machine is controlled
Rate is 30kHz, and ultrasonic reaction 4h obtains reaction product, and reaction product is placed in the revolving speed in supercentrifuge with 6000r/min
Centrifugal treating 15min, removes supernatant liquor, and precipitating is put into the vacuum that set temperature is 80 DEG C and dried by isolated lower sediment
In case, dry 6h obtains superfine tin indium oxide powder；According to parts by weight, by 25 parts of superfine tin indium oxide powder, 15 parts of zinc oxide,
33 parts of ANN aluminium nitrate nonahydrates mix in the polyamic acid colloidal sol that 75 parts of mass fractions are 20%, are dispersed with stirring 25min, obtain transparent
Conductive gelatin is coated with the electrically conducting transparent glue that a layer thickness is 30 μm with coater in the PET film front with a thickness of 0.2mm,
Conductive light modulation film layer is formed, then anti-reflection film liquid is coated on PET film reverse side, forms the antireflective coating of 15mm, finally drying patch
Upper release paper obtains automobile-used rupture pressure disc.
The automobile-used rupture pressure disc that comparative example is produced with Guangzhou company is as a comparison case to produced by the present invention automobile-used anti-
Automobile-used rupture pressure disc in quick-fried film and comparative example is detected, and testing result is as shown in table 1：
Tensile property measurement
It is tested according to standard ASTMD1204.
Light penetration measurement
According to JISK7105《The test method of plastic optics performance》Standard tested.
Wearability measurement
Dry sanding paper wipes the explosion-proof film surface before fitting protective layer, macroscopic scuffing occurs in explosion-proof film surface
Until, record wiping number.
Heat insulation test
By the automobile-used rupture pressure disc clip in automobile-used rupture pressure disc produced by the present invention and comparative example at the diaphragm of 40cm × 40cm, this
Diaphragm is laminated into laminated glass, every sheet glass with a thickness of 2.3mm, be placed in the opening of 30cm × 30cm × 40cm hot box
On（The structure of the hot box is that outermost layer is boarding, and centre is foam layer, and inner layer is aluminum membranous layer, the top layer of chest
It is unlimited, other are sealings）, the temperature in thermometer measure case is placed in chest.In the case where temperature is 35 DEG C of temperature
It is placed on the platform of direct sunlight, the sunlight irradiation through 50min records the glass of heat-insulating anti-explosion membrane and not containing the bilayer of middle layer
The temperature difference of glass.
1 performance measurement result of table
According to data in table 1 it is found that automobile-used rupture pressure disc produced by the present invention, peeling force, adhesive force and light transmittance are superior to
The rupture pressure disc of the prior art, and have the function of heat-insulated, antiultraviolet, defogging defrosting, manufacture craft is simple, and cost is relatively low, tool
There is wide prospect of the application.
Claims (8)
1. a kind of preparation method of automobile-used rupture pressure disc, it is characterised in that specifically preparation step is：
（1）5~6g vanadic anhydride is mixed with 14~15g oxalic acid solution, obtains liquid to be restored, by liquid to be restored and anhydrous second
Alcohol mixing, is put into four-hole boiling flask, is stirred to react under condition of water bath heating with the revolving speed of 200~220r/min, obtains dioxy
Change vanadium forerunner coating liquid；
（2）40~50mL dehydrated alcohol is added into ultrasonic disperse instrument and 20~30mL butyl titanate, ultrasonic disperse are dispersed
Dispersion liquid is placed in the three-necked flask with blender and dropping funel, 20 is added into three-necked flask with dropping funel by liquid
~25mL reconciles liquid, while starting blender, starts to be stirred to react to obtain titanium dioxide with the revolving speed of 200~300r/min molten
Glue；
（3）Hydrogen peroxide is mixed with vanadium dioxide forerunner's coating liquid, oxidation coating liquid is obtained, according to parts by weight, by 8~10 parts
Zinc oxide, 15~20 parts of Tea Saponins, 40~45 parts of oxidation coating liquids, 10~12 parts of TiO 2 sols are added to 80~90 parts of second
In acetoacetic ester, mixed liquor is obtained, then mixed liquor is placed in high speed disperser, high speed dispersion, obtain anti-reflection film liquid；
（4）According to parts by weight, by 10~12 parts of stannous sulfates, 20~25 parts of ethylenediamine tetra-acetic acids and 6~10 parts of potassium hydroxide
It is added in the beaker equipped with 80~90 parts of deionized waters, stirs 30~35min, obtain complexing stannous sulfate solution, to complexing sulphur
4~5 parts of polyvinylpyrrolidonepowder powders are added in sour stannous solution, heat temperature raising stirs to get reducing solution；
（5）4~5g potassium chlorate, 8~10g potassium hydroxide, the mixing of 6~8g indium hydroxide are taken, 200~230mL deionized water is added
In, 20~25min is mixed, obtains oxidation solution, oxygen is added into the above-mentioned reducing solution of 800~900mL with dropping funel
Change solution, is stirred to react, obtains reaction solution；
（6）Above-mentioned reaction solution is placed in ultrasonic reaction machine, ultrasonic reaction obtains reaction product, and reaction product is placed in high speed
Centrifugal treating in centrifuge removes supernatant liquor, and precipitating is put into vacuum drying oven by isolated lower sediment, dry, obtains
Superfine tin indium oxide powder；
（7）According to parts by weight, by 20~25 parts of superfine tin indium oxide powder, 10~15 parts of zinc oxide, 30~33 part of nine hydration nitre
Sour aluminium mixes in 60~75 parts of polyamic acid colloidal sols, is dispersed with stirring 20~25min, obtains electrically conducting transparent glue, PET film just
Face is coated with a thickness electrically conducting transparent glue with coater, forms conductive light modulation film layer, then that anti-reflection film liquid is coated on PET film is anti-
Face forms antireflective coating, and finally drying sticks release paper and obtains automobile-used rupture pressure disc.
2. a kind of preparation method of automobile-used rupture pressure disc according to claim 1, it is characterised in that：Step（1）The grass
The mass fraction of acid solution is 20%, and liquid to be restored and dehydrated alcohol mixed volume ratio are 1 ︰ 5, be stirred to react the time be 14~
15h, control bath temperature are 80~90 DEG C.
3. a kind of preparation method of automobile-used rupture pressure disc according to claim 1, it is characterised in that：Step（2）Described is super
It is 150~200W that sound, which disperses power, and the ultrasonic disperse time is 4~6min, and dropping funel drop rate is 2~3mL/min, is reconciled
Liquid be 20% by mass fraction nitric acid solution and n,N-Dimethylformamide be by volume that 5 ︰, 1 mixed preparing forms, stirring
Reaction time is 50~55min.
4. a kind of preparation method of automobile-used rupture pressure disc according to claim 1, it is characterised in that：Step（3）The general
Hydrogen peroxide and vanadium dioxide forerunner coating liquid mixed volume ratio are 1 ︰ 2, and high speed dispersion revolving speed is 4000~4500r/min, high speed
Jitter time is 18~20min.
5. a kind of preparation method of automobile-used rupture pressure disc according to claim 1, it is characterised in that：Step（4）Described adds
Temperature is 40~50 DEG C after heat heating, and polyvinylpyrrolidonepowder powder is completely dissolved at the end of stirring.
6. a kind of preparation method of automobile-used rupture pressure disc according to claim 1, it is characterised in that：Step（5）The drop
Liquid funnel drop rate is 10~15mL/min, and being stirred to react the time is 40~45min.
7. a kind of preparation method of automobile-used rupture pressure disc according to claim 1, it is characterised in that：Step（6）Described is super
The supersonic frequency of phonoresponse machine be 25~30kHz, the ultrasonic reaction time be 3~4h, supercentrifuge rotating speed be 5000~
6000r/min, centrifugal treating time are 10~15min, and vacuum drying oven set temperature is 70~80 DEG C, and drying time is 5~6h.
8. a kind of preparation method of automobile-used rupture pressure disc according to claim 1, it is characterised in that：Step（7）Described is poly-
The mass fraction of amide acid-sol be 20%, PET film with a thickness of 0.1~0.2mm, electrically conducting transparent glue with a thickness of 20~30 μm,
Antireflective coating is with a thickness of 10~15mm.
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| CN110591491A (en) * | 2019-10-10 | 2019-12-20 | 林华辉 | Preparation method of light-transmitting heat-insulating coating |
| CN113215536A (en) * | 2021-04-20 | 2021-08-06 | 北方夜视技术股份有限公司 | Small-grain anatase optical film, preparation method and application thereof |
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