CN108314970A - The resist blocking and that PVB films and its preparation method of long-term non-isolating film protection when more than 10 DEG C - Google Patents
The resist blocking and that PVB films and its preparation method of long-term non-isolating film protection when more than 10 DEG C Download PDFInfo
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- C09J129/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
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- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
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Abstract
The invention discloses the resist blocking and that PVB films that long-term non-isolating film is protected when a kind of environment temperature is more than 10 DEG C and its preparation methods.It filters out some and can be modified PVB hydroxyls and be other groups or can increase the antiblocking agent of steric hindrance between PVB hydroxyls; and before the molding of PVB films, in molding and after molding; it is set to be mainly distributed on the surface layers PVB by new manufacturing method; weaken intermolecular hydrogen bonding between PVB films surface layers on a microscopic level and inhibits PVB film stick to each others; make it that there is resistance to blocking when environment temperature is more than 10 DEG C and isolation film protection can be exempted, this PVB films entirety ingredient is in parts by weight：0.0001 10 parts, other kinds analog assistants of antiblocking agent are 0.0001 10 parts total, 0.0001 2 parts of water, 3 50 parts of plasticizer, 28 96.9997 parts of resin-oatmeal.
Description
Technical field
The present invention relates to it is a kind of be more than 10 DEG C when long-term non-isolating film protection resist blocking and that PVB films and its preparation method, belong to
Polymeric material field.
Background technology
PVB is writing a Chinese character in simplified form for polyvinyl butyral, is a kind of macromolecule resin material, and Chinese is polyvinyl alcohol
Butyral.
PVB films usually using PVB resin powder and plasticizer as primary raw material, are formed using extruder thermoplastic extrusion.
PVB films are the fields widely used one such as automobile doubling glass, building doubling glass, photovoltaic double-glass doubling component
Kind solid-state adhesive film.PVB films on current market are divided into single layer PVB films, three layers of PVB films, multilayer PVB according to structure
The compound PVB films of film, PET film, PU membrane composite PVB films etc.；It is divided into sound insulation PVB films, heat-insulated PVB glue according to function
Piece, sound-insulating and heat-insulating PVB films, the PVB films with sunshade colored ribbon, coming back shows HUD PVB films, fire prevention PVB films, discoloration
Glass PVB films, conduction PVB films, lead proton PVB films, electronical display PVB films, prevent at dimming glass PVB films
Play PVB films etc.；It is divided into automotive grade PVB films, architectural grade PVB films, photovoltaic grade PVB films etc. according to user；According to shape point
For the identical rectangle PVB films of wedge-shaped PVB films, upper and lower film thickness etc. of upper and lower film thickness gradual change；PVB film stock thickness is usually
0.38~1.52mm, film breadth are usually 400~5000mm.
So far, above-mentioned all PVB films are produced under more than 10 DEG C environment, are stored, transporting and in use, being either in more
Layer heap folds form or multilayer roll form, and one layer of isolation film must all be clamped between every layer of PVB film（Also known as release paper）
As lining, otherwise meeting stick to each other is difficult to separate between PVB films face and face, can make film distortion when being separated with strength and lead
Cause its product doubling glass light distortion.So isolation film has become the standard configuration article of protection PVB films, by domestic and international phase shutout
Family is widely used.However, isolation film also brings many troubles, such as in the winding workshop section of production PVB films, PVB glue
Piece and isolation film will online trimming, the clast that when isolation film cutting edge generates often is adsorbed to the surfaces PVB and pollutes；Make
With the unreel workshop section of PVB films, makes the electrostatic that PVB film faces accumulate that can adsorb dust in environment because removing isolation film, make
It is reduced at the pollution of PVB films and doubling glass optical quality.In addition, after PVB films are finished, isolation film, which just becomes, to be difficult to handle
Waste.Because isolation film is typically disposable product and is easily broken, it is difficult to as the protective film of new PVB films, these
Old isolation film must return be film-made with secondary extrusions of the casting machine of profession after factory after could be utilized again.But since isolation film is very fluffy
Pine, volume be big, light weight, long-distance transport return factory melt down it is uneconomical.Finally, be finished after PVB films all can be isolation for many producers
Film is directly abandoned as rubbish, not only causes material waste, but also seriously pollute environment.Isolation film be mostly polyethylene (PE) or
Haloflex (CPE) material, at least need decades even the centuries could natural degradation, discarded isolation film, which has become, works as
Preceding " white pollution " object one of very harmful to natural environment.
PVB is the macromolecule resin material very sensitive to temperature.It can also be kept to make PVB films not have to isolation film protection
Lower from adhesive, certain producers produce in the environment of being forced in less than 10 DEG C, store, transporting and using PVB, but guarantor for a long time
It holds 10 DEG C or less low temperature environments and is undoubtedly the huge financial burden of enterprise.Under normal temperature environment, people attempt to spend using mechanical compaction
Line etc. improves PVB film faces roughness reduces tack, such as patent text to reduce the direct contact area between film
EP0710545A1, EP0185863B1 are offered, but is stretched due to the gravity pressure of PVB films when stacking or is coiled and using preceding heating
Deng necessary process, PVB surface roughnesses have significantly reduced trend, cause these PVB films still can stick to each other.People were also once
Attempt reduce plasticizer loading come reduce between film from adhesive, but this can seriously reduce film shock resistance and penetration
Etc. mechanical properties.People also once attempted that certain antiplastering aids are added in film formula, such as patent document CN02825306,
CN200480011069, CN200680008950, although also slightly having effect, these antiplastering aids all by uniform dissolution or are dispersed in
In entire PVB films, the antiplastering aid on PVB films surface layer is caused to be not achieved it can be made to exempt isolation film protection because concentration is too small
Resist blocking and that effect, however when enough antiplastering aids are added in formula, again can be to doubling glass product mist degree, light transmittance, cohesive force
Etc. adversely affecting.
Therefore, so far in temperature more than production in 10 DEG C of environment, storage, transport and when using PVB films, no matter PVB
Film is in multiple-level stack form or multilayer roll form, people be all still forced the isolation films such as PE and CPE is used to be protected with
Prevent its stick to each other.
Invention content
Problems to be solved by the invention
PVB films are easy, from adhesion, inconvenience to be caused to user.To prevent PVB film stick to each others, it is more than 10 in temperature
Production in DEG C environment, storage, transport and when using PVB films, people are still forced to carry out using isolation films such as PE and CPE so far
Protection.However during PVB productions and use, the surfaces PVB can be caused clast and dust often occur because using isolation film
Equal pollutants, and reduce doubling glass optical quality.In addition, after PVB is finished, isolation film is difficult to be utilized again, is often treated as
Rubbish abandons, and becomes one of " white pollution " object of present environmental risks.To reduce dependence of the PVB films to isolation film, so far
People have many trials, but actual effect is all bad.Such as the operation under the low temperature environment less than 10 DEG C, although can alleviate
Adhesive between PVB films is simultaneously exempted using isolation film, but the tremendous economic of enterprise is caused to bear；In production PVB films
Formula in certain antiplastering aids are added, but because antiplastering aid it is evenly dispersed in PVB films, surface concentration is too small and cannot reach
Significant anti-self-adhesion effect, can lead to the mist degree and the transparency of doubling glass product again when enough antiplastering aids being added in formula
Etc. unqualified.So to prevent PVB from adhesion, enterprise is still forced to use isolation film protection PVB films so far.
The solution to the problem
The applicant has found after studying intensively for a long time, the hydrogen atom in microcosmic point between the great amount of hydroxy group of PVB films surface layer
It attracts each other with oxygen atom and forms intermolecular hydrogen bonding, which becomes the cohesive force between film, is to cause PVB films mutual
The basic reason of adhesion.
The present invention technical principle be：New antiblocking agent is filtered out, by the hydroxyl modification at PVB films surface layer position at other
Group, or increase the steric hindrance between the hydroxyl of PVB films surface layer, thus between weakening PVB films surface layer on a microscopic level
Intermolecular hydrogen bonding, and then inhibit PVB film stick to each others, and PVB film manufacturing methods are improved, so that antiblocking agent is mainly distributed
On the surface layers PVB, and then produces environment temperature and be more than the PVB films protected without isolation film at 10 DEG C.In addition, in manufacture doubling
During the high temperature and pressure of glass, the antiblocking agent on the surface layers PVB can be diluted to spreading inside film, to make resist blocking and that
Content ratio of the agent in entire PVB films is relatively low, can thus keep adhesiveness and system appropriate between PVB films and glass
The transparency of product doubling glass.
The antiblocking agent that is filtered out of the present invention can be the mica powder of micron-scale and nano-scale, silica,
The inorganic material powders such as calcium carbonate, titanium dioxide, zinc oxide.Applicants have discovered that these inorganic material powders are mainly doped to PVB
Behind film surface layer, not only there is good compatibility with PVB films, but also the sky between the hydroxyl of PVB films surface layer can also be increased
Between steric hindrance, have excellent resist blocking and that effect.
The antiblocking agent that the present invention is filtered out can be PVB resin powder.Applicants have discovered that PVB resin powder can be quickly
It is dissolved into the PVB films surface layer that temperature is more than 60 DEG C, film surface layer plasticizer concentration can be diluted on microcosmic, moreover it is possible to increase PVB
Steric hindrance between the hydroxyl of film surface layer, thus there is excellent resist blocking and that effect.PVB resin powder is as the anti-of PVB films
Adhesion agent spreads flour to dough surface to reduce the adhesion between dough when kneading dough similar to people.In addition, PVB resin powder is answered
PVB resin powder including various models, various hydroxyl values also includes various modified PVB resin powder.
The antiblocking agent that is filtered out of the present invention can be acidic materials, including and be not limited to formic acid, acetic acid, propionic acid,
Butyric acid, hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid etc..Applicants have discovered that acidic materials can by with PVB films surface layer hydroxyl
It learns reaction and generates ester, and then reduce PVB films surface layer hydroxyl quantity and weaken the adhesive between PVB films.
The antiblocking agent that the present invention is filtered out can be some organic compounds of esters, amine, salt, specifically
For single hexanedioic acid stearyl pentaerythritol ester, two hexanedioic acid stearyl pentaerythritol esters, three hexanedioic acid stearyl pentaerythritol esters,
Alkyl phosphate, hexanedioic acid stearyl pentaerythritol ester, pentaerythritol tetrastearate, pentaerythritol ester, oil base palmitic acid acyl
Straight chain alcohol peptamine, the aliphatic acid of amine, oleyl palmitamide, oleoyl palmitamide, oleic acid diethyl amide, aliphatic acid
Amide, hydroxystearic, polyethylene glycol oleamide, stearmide, stearyl erucyl amide, erucyl amide, erucic acid are hard
Acyl amine, behenamide, erucyl Stearyl Amine, hydroxy stearic acid amide, oleamide, Stearic acid diethanolamine salt,
It is stearic amide, wax, alkylbenzene sulfonate, alkylsulfonate, alkyl sulfate, alkyl carboxylate, poly-alkoxyl carboxylate, hard
Resin acid silicon, calcium stearate, magnesium stearate, neopelex, dodecyl sodium sulfate.Salt in above-mentioned antiblocking agent
There is no restrictions for cation, such as can be exemplified by the cations such as lithium, sodium, potassium, magnesium, calcium, ammonium root；Compound in above-mentioned antiblocking agent
Alkyl there is no limiting, such as methyl, ethyl, propyl can be exemplified by etc..Applicants have discovered that these organising of filtering out
After conjunction object is mainly distributed to PVB films surface layer, not only there is good compatibility with PVB films, but also PVB glue can also be increased
Steric hindrance between the hydroxyl of piece surface layer has excellent resist blocking and that effect.
In addition, after the antiblocking agent filtered out in the present invention is mainly dispersed in PVB films surface layer, even if environment temperature is big
In 10 DEG C, it is more than to remain to only just be separated from each other by its own gravity after 24 hours that PVB films are in direct contact the time face-to-face, the effect
Also " reducing stick to each other ", " can be easily separated or be open ", " the increase smooth sense in surface " etc., institute are commonly described as between PVB films
It should be equal to people with this antiblocking agent and be accustomed to address：Antitack agent, opening agent, opens film, slipping agent, lubricant at anticaking agent
Deng.
The present invention innovation be：Filter out can by PVB hydroxyl modifications at other groups and can increase PVB hydroxyls it
Between steric hindrance antiblocking agent and so that it is mainly distributed on PVB films surface layer position, on a microscopic level weaken PVB film tables
Intermolecular hydrogen bonding and inhibit PVB film stick to each others between layer, long-term non-isolating film protection at 10 DEG C is more than to produce
Resist blocking and that PVB films.In addition, when PVB films are processed to doubling glass together with glass, using 40-200 DEG C of precompressed and
High-pressure molding technique makes the antiblocking agent on the surface layers PVB be diluted to spreading inside film, to make antiblocking agent entire
Concentration in PVB films is not exceeded, can thus keep adhesiveness and product doubling glass appropriate between PVB films and glass
The transparency.
The concrete scheme that the present invention solves the problems, such as is not only to filter out antiblocking agent, makes PVB films integral into being divided into：
Antiblocking agent 0.0001-10 parts by weight；
Other kinds of analog assistants add up to 0.0001-10 parts by weight；
Water 0.0001-2 parts by weight；
Plasticizer 3-50 parts by weight；
Resin-oatmeal 28-96.9997 parts by weight；
And change manufacturing method, so that antiblocking agent is mainly distributed on PVB films surface layer, contained by the position of PVB films surface layer
Antiblocking agent concentration is N times of antiblocking agent concentration contained by the PVB film stock thickness centre, and the lower limit of N is
1.000000001, preferably 1.25, the further preferably upper limit of 2, N are 1 × 1020, preferably 10000, further preferably
50。
The key of the resist blocking and that PVB film manufacturing methods of long-term non-isolating film protection is when more than 10 DEG C：PVB films at
Before type, in molding or after molding, limited amount antiblocking agent is added in PVB films and it is made to be mainly distributed on PVB films
Surface layer position.Specifically and because the method that antiblocking agent is added before PVB films are molded is to be incorporated into resin-oatmeal, be incorporated into increasing
In modeling agent, it is incorporated into other kinds of analog assistants, is incorporated into the mixture of more than one raw materials, is added to extruder feed port
In, the combination that at least one of is added to PVB meltings sizing material surface；Antiblocking agent method for being added in the molding of PVB films is
The liquid containing antiblocking agent is sprayed near PVB film molding die die lips, leaving mold in PVB films carries out hot-stretch expansion
When exhibition spray the liquid containing antiblocking agent, using when mould heat pressure PVB films film surface layer coat antiblocking agent powder in
At least one combination；The method that antiblocking agent is added after the molding of PVB films is that PVB films are immersed in containing antiblocking agent
Solution in, using carry antiblocking agent liquid coarse roller PVB films are embossed and are drawn, print antiblocking agent
PVB is adhered to PVB film faces, by the liquid spray containing antiblocking agent to PVB film faces, by the powder of antiblocking agent
The combination of at least one of film face.Liquid jet coating method in above-mentioned manufacturing method needs first evenly dispersed in a liquid
Or then dissolving antiblocking agent, atomization are ejected into the surfaces PVB by pressure-air.Solution in above-mentioned manufacturing method impregnates
Method needs first uniform dissolution antiblocking agent in a solvent.Solvent for use all has volatility in spraying method and immersion process, packet
Water, ethyl alcohol etc. are included but be not limited to, can all be heated in time after liquid deposition is on the surfaces PVB, so that solvent is vapored away, stay in table
The resist blocking and that in face can penetrate into the surface layers PVB while hot, and the concentration of antiblocking agent is usually 0.1wt%-20wt% in liquid, the concentration energy
Making both sides surface layer, there are the PVB films of antiblocking agent still to have resistance to blocking good enough when temperature is more than 10 DEG C, to exempt from
Except being protected using isolation film.In addition, antiblocking agent is incorporated into raw material in above-mentioned manufacturing method, is added to melting sizing material table
Face, the method printed or adhere to film face, antiblocking agent are preferably its powder, can directly pass through Weighing control antiblocking agent
Addition, and then it is adjusted on film surface layer and the content in whole PVB films ingredient.
In the present invention, lower limit of the antiblocking agent content in whole PVB films ingredient is 0.0001 parts by weight, preferably
0.001 parts by weight, further preferably 0.01 parts by weight, the upper limit of the antiblocking agent content in whole PVB films ingredient are 10
Parts by weight, preferably 5 parts by weight, further preferably 1 parts by weight.When antiblocking agent content is less than 0.0001 parts by weight, even if
All antiblocking agents are all distributed in film surface layer, and the requirement that PVB films are not necessarily to isolation film protection is still not achieved in resistance to blocking；It is anti-
When adhesion agent content is more than 10 parts by weight, the PVB films transparency and adhesivity can be deteriorated.
It is polyvinyl butyral resin powder as the resin-oatmeal of one of resist blocking and that PVB film ingredients of the present invention（PVB）、
At least one of the modified polyvinyl butyral resin-oatmeal ingredient.PVB resin powder be molecular weight between thousands of to tens
Ten thousand high-molecular compound is mainly made of many units of three kinds of hydroxyl, butyraldehyde base and vinyl acetate base groups.Modified PVB
Other groups typically are grafted in PVB former bases group, or other functional materials are adulterated in former PVB resin powder, so modified PVB
Main body be still PVB resin powder.According to hydroxyl size, PVB and modified PVB powder can be divided into high hydroxyl PVB resin powder, middle hydroxyl again
Base PVB resin powder, high hydroxyl PVB resin powder etc..In the present invention, lower limit of the resin powder content in whole PVB films ingredient is
The upper limit of 28 parts by weight, preferably 50 parts by weight, further preferably 70 parts by weight, resin powder content is 96.9997 parts by weight,
Preferably 90 parts by weight, further preferably 85 parts by weight.When resin powder content is less than 28 parts by weight, PVB films are difficult to be molded；
When resin powder content is more than 96.9997 parts by weight, PVB films will lose flexibility.
As the plasticizer of one of resist blocking and that PVB film ingredients of the present invention, it is not particularly limited, such as can include：
Plasticizer include and be not limited to dihexyl adipate, dioctyl adipate, diisononyl adipate, adipic acid heptyl nonyl ester,
Bis- (2- butoxy) ethyl esters of adipic acid, Kui adipate, cyclohexyl hexyl adipate, two tricaprylate of triethylene glycol, triethylene glycol
Two-(2 Ethylbutanoic acid esters), triethylene glycol two-(2 ethyl hexanoic acid ester), triethylene glycol diheptylate, tetraethylene glycol diheptanoate, two -2-
Thylhexoic acid tetraethylene glycol ester, two -2 Ethylbutanoic acid triglycol esters, two -2 Ethylbutanoic acid tetraethylene glycol esters, two enanthic acid tetrems
The double 2- butoxyethyls of diol ester, two enanthic acid triglycol esters, adipic acid, tributoxyethyl phosphate, isodecyl phenyl ester,
At least one of the tricresyl phosphate isopropyl ester ingredient.In the present invention, lower limit of the plasticizer loading in entire PVB films is 3
The upper limit of parts by weight, preferably 10 parts by weight, further preferably 15 parts by weight, plasticizer loading is 50 parts by weight, preferably
40 parts by weight, further preferably 35 parts by weight.When plasticizer loading is less than 3 parts by weight, PVB film plasticizing effects difference rigidity is too
By force；When plasticizer loading is more than 50 parts by weight, the excessively soft inconvenient processing of PVB films, and also there are the risks of plasticizer extravasation.
As other kinds of analog assistants of one of resist blocking and that PVB film ingredients of the present invention, it is not particularly limited, such as can example
It enumerates：Antioxidant, infrared absorbent, percussion value conditioning agent, insulation agent, brightening agent, chelating agent, divides ultra-violet absorber
Powder, anti-whiting agent, flame retardant, quickly penetrating agent, frothing inhibitor, surfactant, chain extender, conductive agent, is led at resistance to humectant
At least one of proton agent, antistatic agent, the pigment ingredient.Wherein, antioxidant include and be not limited to 1010,
1076,168,2,6- di-tert-butyl-4-methy phenols etc., ultra-violet absorber include and be not limited to UV326, UV327,
UV328, UV329, Tinuvin144 etc., infrared absorbent include and are not limited to naphthalene phthalocyanine compound, anthraquinone dye etc., strike
It hits value conditioning agent to include and be not limited to sodium acetate, potassium acetate, sodium chloride, magnesium chloride etc., insulation agent includes and is not limited to mix
Antimony oxidation tin, wolframic acid caesium, tin indium oxide etc., brightening agent include and are not limited to fluorescent powder etc., and chelating agent includes and is not limited to
B diammonium edta, 2,2'- bipyridyls etc., dispersant include and are not limited to polyvinyl alcohol, sodium tripolyphosphate etc., the packet of resistance to humectant
Calcium carbonate, calcium chloride etc. are included and are not limited to, anti-whiting agent includes and is not limited to benzoyl peroxide, polyvinyl amide
Deng, flame retardant includes and is not limited to magnesium hydroxide, aluminium hydroxide etc., quickly penetrating agent include and be not limited to polyethylene glycol,
Polypropylene glycol etc., frothing inhibitor include and are not limited to polyoxyethylene polyoxypropylene pentaerythrite ether, polyoxyethylene polyoxy third
Alcohol amidogen ether etc., surfactant include and are not limited to fatty glyceride etc., and chain extender includes and is not limited to boric acid, boron
Sand, phthalic anhydride etc., conductive agent include and are not limited to carbon nanotube, graphene etc., lead proton agent and include and do not limit
In lithium perchlorate, potassium hyperchlorate etc., antistatic agent includes and is not limited to mix bismuth zinc oxide, mixes bismuth tin oxide etc., pigment includes
And be not limited to phthalocyanine blue, phthalocyanine green, carbon black etc..In the present invention, other kinds of analog assistant total contents are in entire PVB films ingredient
Lower limit be 0.0001 parts by weight, preferably 0.001 parts by weight, further preferably 0.01 parts by weight, other kinds of analog assistants are total
The upper limit of content is 10 parts by weight, preferably 5 parts by weight, further preferably 1 parts by weight.Other kinds of analog assistant total contents are whole
When being less than 0.0001 parts by weight in a PVB films, the performances such as the weatherability of PVB films cannot be improved, when more than 10 parts by weight, meeting
Deteriorate the transparency and adhesivity of PVB films.
It is light water, preferably deionized water, water is entire as the water of one of resist blocking and that PVB film ingredients of the present invention
Lower limit in PVB film ingredients is 0.0001 parts by weight, preferably 0.001 parts by weight, further preferably 0.01 parts by weight, water
The upper limit in entire PVB films ingredient is 2 parts by weight, preferably 1 parts by weight, further preferably 0.5 parts by weight.Water is whole
When content is less than 0.0001 parts by weight in a PVB films, the flexibility of PVB films can be reduced, when more than 2 parts by weight, can be deteriorated
The adhesivity of PVB films, and bubble can be generated in doubling glass product.
As the shape of resist blocking and that PVB films of the present invention, including and it is not limited to as complete wedge-shaped, part wedge shape, rectangle
At least one of combination.PVB films containing wedge structure can be used for the automobile doubling glass shown that comes back.
As the structure of resist blocking and that PVB films of the present invention, the PVB films number of plies is at least one layer, and every layer of PVB film is thick
It is 0.001 millimeter to spend lower limit, preferably 0.01 millimeter, further preferably 0.1 millimeter, and every layer of PVB film stock thickness upper limit is 10
Millimeter, preferably 5 millimeters, further preferably 2 millimeters.The PVB films of multilayered structure can be used for sound insulation doubling glass, be answered with PU films
It closes and manufactures shellproof doubling glass and the other function doubling glass of PET film composite manufacturing etc..
As the thermoplastic casting apparatus for manufacturing resist blocking and that PVB films in the present invention, it is not particularly limited, including and do not limit
In single screw extrusion machine, parallel double-screw extruder, conical double screw extruder, parallel dual-screw extruding machine and incongruous double screw
Extruder etc..
As resist blocking and that PVB film production lines are manufactured in the present invention, it is not particularly limited, other than extruder, further includes
And be not limited to weightless title, weighing balance, batch mixer, feeder, blender, bead cutter, lap changing apparatus, winder, baling press etc..
As in the present invention manufacture resist blocking and that PVB film production lines process, can be divided into PVB films molding before, molding when,
Three master operations after molding, specifically include and be not limited to spice, feeding, thermoplastic, extrusion, draw, enter water, cross roller, drying,
Tempering, adjustment, winding, packing etc..
The effect of invention
The applicant filters out can be by the hydroxyl modification at PVB films surface layer position at other groups or increase PVB films surface layer hydroxyl
The antiblocking agent of steric hindrance between base, to be formed between weakening PVB films surface layer hydroxyl on a microscopic level intermolecular
Hydrogen bond simultaneously inhibits PVB film stick to each others, and limited amount antiblocking agent is mainly distributed on PVB surface sections by the applicant
Position, to make PVB that there is excellent resist blocking and that effect in more than 10 DEG C ranges and isolation film protection can be exempted.In production doubling
The glass stage is pressurizeed by heating, and the antiblocking agent at the surface layers PVB position is made to be able to diffusion dilution to film internal penetration, to
Keep content ratio of the antiblocking agent in entire PVB films not exceeded, adhesiveness appropriate between PVB films and glass can be kept
And the transparency of product doubling glass.In addition, reduce PVB films using the isolation films such as PE and CPE, and can reduce have to environment it is broken
Bad " white pollution object ".
Resistance to blocking test method
The resist blocking and that PVB films of long-term non-isolating film protection, more not relevant when due to being not greater than 10 DEG C on current market
Professional standard, and it is existing《Plastic film adhesive test method》（GB/T16276-1996）Thickness in monolayer is only applicable to again to exist
Plastic film between 0.025~0.01mm.The applicant has developed a set of self checking method in practice thus：Claim two unilateral
Product is all 300mm × 300mm and the identical PVB film qualities of thickness are M, then overlaps PVB films face-to-face and stacks, up and down
The polytetrafluoroethylene of a piece of identical size is respectively clamped, is then horizontally arranged on the table.In upper layer polytetrafluoroethylene
On pallet that place a bottom surface again also be 300mm × 300mm, it is the fine sand of 10M and evenly laid out that quality is added in pallet,
Simulation the born pressure of two panels PVB films is equal to the pressure that bottom film is born when about 20 identical PVB film waters are flat to be stacked, room
It is 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C that interior temperature, which is distinguished constant,.Pallet is removed after 24 hours, if a piece of PVB is only
It can be separated from each other with another PVB by its own gravity, then show that its resistance to blocking qualification can be not necessarily to for a long time when more than 10 DEG C
Isolation film is protected, and is used ● is indicated；Then show that its resistance to blocking is unqualified still when but if only leaning on its own gravity that cannot be separated from each other
It needs isolation film to protect, is indicated with zero.In addition, in practice it has proved that the PVB films of above-mentioned resistance to blocking qualification store up for a long time when more than 10 DEG C
Even if stack after depositing 300 still can delamination and normal use without leading to film distortion, so its preventing adhesiving effect is sufficient
So that it is protected without isolation film for a long time, and it is all qualified that the performance tests such as the optics after doubling glass, mechanics, weather-proof are made.
Description of the drawings
Fig. 1 antiblocking agents are mainly distributed on the single layer PVB films of the long-term non-isolating film protection on surface layer；
Fig. 2 antiblocking agents are mainly distributed on three layers of PVB films of the long-term non-isolating film protection on surface layer；
Fig. 3 antiblocking agents are mainly distributed on the films of PVB containing colored ribbon of the long-term non-isolating film protection on surface layer；
Fig. 4 antiblocking agents are mainly distributed on the wedge-shaped PVB films of the long-term non-isolating film protection on surface layer；
Wherein 11 be antiblocking agent, and 12 be PVB films, and 21 be three layers of PVB film middle layers, and 31 be colored ribbon.
Specific implementation mode
Embodiment 1
Antiblocking agent is added before PVB films are molded, antiblocking agent is added in PVB melting sizing materials surface, manufacture is more than 10
DEG C when single layer PVB films without isolation film protection, detailed process is as follows：
(1) 95 extruders and miscellaneous equipment form a PVB production line；
(2) PVB resin powder claims A pairs of 95 machines feed, feeding speed to be 72 parts by weight/minute through weightlessness, and inlet is the extruder
Powder feed inlet；
By the antiblocking agent butyric acid of 0.01 parts by weight, the 3GO plasticizer of 26 parts by weight, 0.2 parts by weight 1010 antioxidant,
328 ultra-violet absorbers of 0.2 parts by weight, the sodium acetate percussion value conditioning agent of 0.09 parts by weight, 0.5 parts by weight water uniformly mix
B is claimed also to be fed to 95 machine through weightlessness after conjunction, inlet is the first pouring orifice of the extruder, and feeding speed is 27 weight
Part/minute；
(4) claim C to be also fed to 95 machine through weightlessness antiblocking agent butyric acid, inlet is the second pouring orifice of the extruder, is supplied
Material speed is 1 parts by weight/minute, and the antiblocking agent butyric acid injected at this time in the screw rod end of extruder is arranged in the second pouring orifice
It is mainly distributed on PVB melting sizing materials surface, is seldom stirred again into inside PVB melting sizing materials, melting sizing material passes through filter screen,
Recycle melt pump pressure to enter in distributor, be then re-introduced into a rack-style casting mold intracavitary and it is evenly laid out after it is logical
Crossing die lip mouth curtain coating and squeezing becomes single layer PVB films；
(5) PVB films cool down through water-carrying groove and shape, and the baking oven for being about 70 DEG C across five meters long and temperature removes surface moisture, utilizes
As soon as PVB films are wound into tubular around a hollow plastic barrel and are packaged sealing by winder, it is manufactured that single layer structure PVB glue
Piece；
(6) by this technique, antiblocking agent butyric acid is mainly distributed on the both sides surface layer of single layer structure PVB films, and butyric acid can be with
PVB film surface part hydroxyl reactions generate butyl ester, and then weaken the intermolecular hydrogen bonding between PVB film face hydroxyls, therefore
Make the PVB films that there is higher anti-protected from adhesive and without isolation film when more than 10 DEG C；
(7) resist blocking and that effect that the PVB is protected at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C without isolation film is detected such as
Shown in table 1.
Table 1 is：
Embodiment 2
Antiblocking agent is added before PVB films are molded, antiblocking agent is incorporated into the mixture of more than one raw materials, manufacture is big
The three-decker PVB films for the resist blocking and that non-isolating film is protected when 10 DEG C, detailed process are as follows：
By the antiblocking agent erucyl amide of 0.01 parts by weight, the PVB resin powder of 54 parts by weight, 45 parts by weight 3GO plasticizer,
The percussion value conditioning agent acetic acid of the antioxidant 1010 of 0.2 parts by weight, the ultra-violet absorber 328 of 0.2 parts by weight, 0.09 parts by weight
The water of potassium and 0.5 parts by weight, after mixing feeding to 52 type double screw extruder for squeezing out in three-decker PVB
Interbed；
(2) by the antiblocking agent erucyl amide of 0.51 parts by weight, the antiblocking agent stearic acid silicon of 0.5 parts by weight, 72 parts by weight
The ultra-violet absorber of PVB resin powder, the plasticizer 3GO of 26 parts by weight, the antioxidant 1010 of 0.2 parts by weight, 0.2 parts by weight
328, the water of the percussion value conditioning agent potassium acetate and 0.5 parts by weight of 0.09 parts by weight, feeding is double to 95 types after mixing
Screw extruder is used to squeeze out the both sides surface layer of three-decker PVB；
(3) 52 extruders, 95 extruders and miscellaneous equipment form a PVB production line；
(4) two extruders screw rod area temperature is set as 40 DEG C -180 DEG C from low to high, and mixed material is added by two extruders respectively
Become two-way after heat and melt sizing material, is respectively carried through filter screen through twin-screw, recycles melt pump pressure that two-way is made to melt glue
Material enters containing there are three in the compound distributor of independent flow passage, and 95 machines melting sizing material is bisected into two strands and centre accommodates one
Stock 52 machines melt sizing material, three bursts melting co-implanted to one rack-style casting mold intracavitary of sizing material and it is evenly laid out after pass through mould
Lip curtain coating squeezes the PVB films as three-decker；
(5) PVB films are shaped after leaving mold through water-carrying groove cooling, the baking oven removing table for being about 70 DEG C across five meters long and temperature
Face moisture is manufactured that one as soon as PVB films are wound into tubular around a hollow plastic barrel using winder and are packaged sealing
PVB films are rolled up, due to the PVB film middle layer flexible relatives and Recover The Acoustic Wave Impedance Coefficient is big, which can be taken as acoustic mastic
Piece is applied to the doubling glass field such as automobile and building；
(6) film two sides surface layer is mainly distributed on by this technique, antiblocking agent erucyl amide and stearic acid silicon, in manufacture doubling
It just can significantly migrate and be diluted to middle layer under the high temperature and high pressure environment of glass, erucyl amide and stearic acid silicon can be to PVB
The steric hindrance that film face hydroxyl causes weakens its intermolecular hydrogen bonding, therefore it is higher anti-from adhesive so that the PVB films is had
And it is protected without isolation film when more than 10 DEG C；
(7) resist blocking and that effect that the PVB is protected at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C without isolation film is detected such as
Shown in table 1.
Embodiment 3
Antiblocking agent is added in PVB film forming processes, is sprayed when PVB films leave mold progress hot-stretch extension anti-stick
Even agent, manufacture are more than the single layer PVB films for the resist blocking and that protected without isolation film at 10 DEG C, and detailed process is as follows：
(1) by the antiblocking agent oleyl palmitamide of 0.01 parts by weight, the 3GO of the PVB resin powder of 72 parts by weight, 26 parts by weight
Plasticizer, 1010 antioxidant of 0.2 parts by weight, 328 ultra-violet absorbers of 0.2 parts by weight, 0.09 parts by weight potassium acetate strike
The water of value conditioning agent and 0.5 parts by weight is hit, feeding is used to produce the PVB glue to a 95 type double screw extruders after mixing
Piece, rate of feeding are 99 parts by weight/minute；
(2) 95 extruders and miscellaneous equipment form a PVB production line；
(3) 95 extruder screw area temperature are set as 40 DEG C -180 DEG C from low to high, and mixed material becomes all the way after being heated by screw rod
Sizing material is melted, filter screen is carried through by twin-screw, recycles melt pump pressure that melting sizing material is made to enter in distributor, then
Be re-introduced into a rack-style casting mold intracavitary and it is evenly laid out after by die lip mouth curtain coating squeeze become single layer PVB films,
When PVB films leave mold progress hot-stretch extension, antiblocking agent oil base palmitic acid acyl is uniformly sprayed on two surface of PVB films
Amine powder, spraying speed be 1 parts by weight/minute, at this time PVB films just in forming process, surface temperature still 120 DEG C-
Between 160 DEG C, the oleyl palmitamide powder sprayed to the surfaces PVB can be melted rapidly and be penetrated into the surface layers PVB；
(4) PVB films cool down through water-carrying groove and shape, and the baking oven for being about 70 DEG C across five meters long and temperature removes surface moisture, utilizes
As soon as PVB films are wound into tubular around a hollow plastic barrel and are packaged sealing by winder, it is manufactured that single layer structure PVB glue
Piece；
(5) by this technique, antiblocking agent oleyl palmitamide is mainly distributed in the surface layer of PVB films two sides, is pressed from both sides in manufacture
It just can significantly be diluted to film thickness Center shift under the high temperature and high pressure environment of glue glass, oleyl palmitamide can be to PVB
The steric hindrance that film face hydroxyl causes weakens its intermolecular hydrogen bonding, therefore it is higher anti-from adhesive so that the PVB films is had
And it is protected without isolation film when more than 10 DEG C；
(6) resist blocking and that effect that the PVB is protected at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C without isolation film is detected such as
Shown in table 1.
Embodiment 4
Antiblocking agent is added in PVB film forming processes, using mold by rectangle PVB film hot pressing be wedge type when in film
Surface layer coats antiblocking agent, and manufacture is more than the wedge-shaped PVB films for the resist blocking and that protected without isolation film at 10 DEG C, and detailed process is such as
Under：
(1) it is 1000mm using the 52 machines production width of volume 1, the rectangle PVB films that thickness is 0.91mm；
(2) utilize two conical metals to build wedge-shaped hot pressing die to pressure roller etc., the two cone-shaped metal rollers make it with electrical heating
Constant surface temperature is 100 DEG C, and it is 0.3mrad to adjust to the angle of wedge in pressure roller gap.Slowly the film is passed through using carry-over pinch rolls
Wedge-shaped hot pressing die, and antiblocking agent polyvinyl butyral resin dried bean noodles powder, carry-over pinch rolls are uniformly coated in time on film two sides
Rotating speed is 2 ms/min, and rectangle PVB films become wedge shape to pressure roller hot pressing by two conical metals and make PVB resin dry powder
It is rapidly soaked into PVB film faces, cooling and shaping, PVB films upper end thickness is 1.06mm, bottom thickness 0.76mm at this time,
And thickness uniformly successively decreases from top to bottom, is wound in wedge-shaped PVB films around a hollow plastic barrel using winder coniform
And it is packaged sealing, it is just manufactured that wedge-shaped PVB films and film two sides surface layer is permeated with antiblocking agent polyvinyl butyral
Resin-oatmeal；
(3) by this technique, antiblocking agent PVB resin powder is hot-pressed in the surface layer of wedge-shaped PVB films two sides, in manufacture doubling glass
It just can significantly be diluted, i.e., be moulded by the plasticizer inside film to film thickness Center shift under the high temperature and high pressure environment of glass
Change, PVB resin powder can cause steric hindrance to weaken its intermolecular hydrogen bonding PVB film face hydroxyls, therefore the PVB films is made to have
There is higher anti-protected from adhesive and without isolation film when more than 10 DEG C；
(4) resist blocking and that effect that the PVB is protected at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C without isolation film is detected such as
Shown in table 1.
Embodiment 5
Antiblocking agent is added after the molding of PVB films, by the liquid spray containing antiblocking agent to PVB film faces, manufacture is big
The PVB films with blue sunshade band when 10 DEG C without the resist blocking and that of isolation film protection, detailed process are as follows：
(1) by the antiblocking agent dodecyl sodium sulfate of 0.01 parts by weight, the 3GO of the PVB resin powder of 72 parts by weight, 26 parts by weight
Plasticizer, 1010 antioxidant of 0.2 parts by weight, 328 ultra-violet absorbers of 0.2 parts by weight, 0.09 parts by weight potassium acetate strike
The water of value conditioning agent and 0.5 parts by weight is hit, feeding is used to produce the PVB glue to a 95 type double screw extruders after mixing
Piece；
(2) the PVB white tiles corner broken material of 99.9 parts by weight and the phthalocyanine blue pigment of 0.1 parts by weight are individually fed after mixing
Expect to be used to produce the blue sunshade band at the top of the PVB films to 35 type extruders；
(3) 95 extruders, 35 extruders and miscellaneous equipment form a PVB production line；
(4) two extruders screw rod area temperature is set as 40 DEG C -180 DEG C from low to high, and mixed material is added by two extruders respectively
Become two-way after heat and melt sizing material, is respectively carried through filter screen through twin-screw, recycles melt pump pressure that two-way is made to melt glue
Material enters in compound distributor, is that runner is arranged in blue sizing material in the stainless steel insert side end of compound distributor, makes PVB films top
The white material that the blue sunshade band in portion is clamped in 95 machines extrusion is intermediate, and co-implanted to one rack-style casting mold intracavitary is simultaneously equal
Being squeezed by die lip mouth curtain coating after even tiling becomes the PVB films with blue sunshade band, and PVB films leave mold using water
After slot cooling sizing, the baking oven for being about 70 DEG C across five meters long and temperature removes surface moisture, then with spray gun by anti-adhesive agent
The aqueous solution of the dodecyl sodium sulfate of 0.5mol/L sprays in PVB film both side surfaces, is then passed through that five meters long and temperature is set
Being set to 80 DEG C of baking oven keeps dodecyl sodium sulfate uniform curing on PVB films both sides surface layer, and PVB films are surrounded one using winder
A hollow plastic barrel is wound into tubular and is packaged sealing, is just manufactured that the resist blocking and that PVB films with blue sunshade band；
(5) by this technique, antiblocking agent dodecyl sodium sulfate is mainly distributed in the surface layer of PVB films two sides, is pressed from both sides in manufacture
It just can significantly be diluted to film thickness Center shift under the high temperature and high pressure environment of glue glass, dodecyl sodium sulfate can be to PVB
The steric hindrance that film face hydroxyl causes weakens its intermolecular hydrogen bonding, therefore it is higher anti-from adhesive so that the PVB films is had
And it is protected without isolation film when more than 10 DEG C；
(6) resist blocking and that effect that the PVB is protected at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C without isolation film is detected such as
Shown in table 1.
Contrast sample
Contrast sample from the PVB films optionally produced on the market by other manufacturers as the present invention removes isolation film, inspection
Survey PVB films resist blocking and that effect such as 1 institute of table that non-isolating film is protected at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C
Show.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of resist blocking and that PVB films being more than long-term non-isolating film protection at 10 DEG C, which is characterized in that the PVB films exist
After temperature is more than the multiple-level stack form being in direct contact with face more than 24 hours retaining surfaces in 10 DEG C of environment and multilayer roll form,
Wherein a piece of PVB only leans on its own gravity that can be separated from each other with another PVB, and the PVB films entirety ingredient is in parts by weight
For：0.0001-10 parts, other kinds analog assistants of antiblocking agent are 0.0001-10 parts total, 0.0001-2 parts of water, 3-50 parts of plasticizer,
28-96.9997 parts of resin-oatmeal.
2. resist blocking and that PVB films according to claim 1, which is characterized in that the antiblocking agent is mica powder, titanium dioxide
Silicon, calcium carbonate, titanium dioxide, zinc oxide, polyvinyl butyral resin powder, modified polyvinyl butyral resin-oatmeal, formic acid,
Acetic acid, propionic acid, butyric acid, hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, single hexanedioic acid stearyl pentaerythritol ester, two hexanedioic acid stearyl seasons
Doutrate, three hexanedioic acid stearyl pentaerythritol esters, alkyl phosphate, hexanedioic acid stearyl pentaerythritol ester, four stearic acid
Pentaerythritol ester, pentaerythritol ester, oleyl palmitamide, oleyl palmitamide, oleoyl palmitamide, oleic acid two
Glycollic amide, the straight chain alcohol peptamine of aliphatic acid, fatty acid amide, hydroxystearic, polyethylene glycol oleamide, stearoyl
Amine, stearyl erucyl amide, erucyl amide, erucyl steramide, behenamide, erucyl Stearyl Amine, hydroxyl are hard
Resin acid amide, oleamide, Stearic acid diethanolamine salt, stearic amide, wax, alkylbenzene sulfonate, alkylsulfonate, alkyl
Sulfate, alkyl carboxylate, poly-alkoxyl carboxylate, stearic acid silicon, calcium stearate, magnesium stearate, neopelex,
The combination of at least one of dodecyl sodium sulfate ingredient.
3. resist blocking and that PVB films according to claim 1, which is characterized in that the resin-oatmeal is polyvinyl butyral
The combination of at least one of resin-oatmeal, modified polyvinyl butyral resin-oatmeal ingredient, the plasticizer be dihexyl adipate,
Bis- (2- butoxy) ethyl esters of dioctyl adipate, diisononyl adipate, adipic acid heptyl nonyl ester, adipic acid, two fourth of Kui diacid
Ester, cyclohexyl hexyl adipate, two tricaprylate of triethylene glycol, triethylene glycol two-(2 Ethylbutanoic acid ester), triethylene glycol two-(2- ethyls
Capronate), triethylene glycol diheptylate, tetraethylene glycol diheptanoate, two -2 ethyl hexanoic acid tetraethylene glycol esters, two -2 Ethylbutanoic acids three
The double 2- of glycol ester, two -2 Ethylbutanoic acid tetraethylene glycol esters, two enanthic acid tetraethylene glycol esters, two enanthic acid triglycol esters, adipic acid
The combination of at least one of butoxyethyl, tributoxyethyl phosphate, isodecyl phenyl ester, tricresyl phosphate isopropyl ester ingredient.
4. resist blocking and that PVB films according to claim 1, which is characterized in that the other kinds of analog assistants be antioxidant,
Ultra-violet absorber, insulation agent, infrared absorbent, brightening agent, chelating agent, dispersant, resistance to humectant, is prevented percussion value conditioning agent
Whiten agent, flame retardant, quickly penetrating agent, frothing inhibitor, surfactant, chain extender, conductive agent, proton conductive agent, anti-quiet
The combination of at least one of electric agent, pigment ingredient.
5. resist blocking and that PVB films according to claim 1, which is characterized in that the PVB films shape is full wedge shape, portion
Divide the combination of at least one of wedge shape, rectangle.
6. resist blocking and that PVB films according to claim 1, which is characterized in that the PVB films number of plies is at least one layer,
Every layer of PVB film stock thickness lower limit is 0.001 millimeter, preferably 0.01 millimeter, further preferably 0.1 millimeter, every layer of PVB film
Upper thickness limit is 10 millimeters, preferably 5 millimeters, further preferably 2 millimeters.
7. resist blocking and that PVB films according to claim 1, which is characterized in that antiblocking agent is mainly distributed on PVB film tables
Layer, antiblocking agent concentration is antiblocking agent concentration contained by the PVB film stock thickness centre contained by the position of PVB films surface layer
N times, the lower limit of N is 1.000000001, preferably 1.25, and further preferably the upper limit of 2, N is 1 × 1020, preferably
10000, further preferably 50.
8. the preparation method of the resist blocking and that PVB films of long-term non-isolating film protection when more than 10 DEG C, which is characterized in that antiblocking agent can be
It is added before the molding of PVB films, Adding Way is to be incorporated into resin-oatmeal, be incorporated into plasticizer, being incorporated into other kinds of analog assistants
In, be incorporated into the mixture of more than one raw materials, be added in extruder feed port, being added in PVB meltings sizing material surface
At least one combination.
9. the preparation method of the resist blocking and that PVB films of long-term non-isolating film protection when more than 10 DEG C, which is characterized in that antiblocking agent can be
It being added in the molding of PVB films, Adding Way is that the liquid containing antiblocking agent is sprayed near PVB film molding die die lips,
It is left when mold carries out hot-stretch extension in PVB films and sprays the liquid containing antiblocking agent, when using mould heat pressure PVB films
The combination of at least one of antiblocking agent powder is coated on film surface layer.
10. the preparation method of the resist blocking and that PVB films of long-term non-isolating film protection when more than 10 DEG C, which is characterized in that antiblocking agent can
It is added after the molding of PVB films, Adding Way is that PVB films are immersed in the solution containing antiblocking agent, is anti-using carrying
The coarse roller of adhesion agent liquid is embossed and draws to PVB films, antiblocking agent is printed onto to PVB film faces, will be contained
There is the liquid spray of antiblocking agent to adhere at least one of PVB film faces to PVB film faces, by the powder of antiblocking agent
Combination.
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| CN112080094A (en) * | 2020-08-19 | 2020-12-15 | 广州凌玮科技股份有限公司 | Anti-adhesion PVB film |
| CN113001702A (en) * | 2021-03-05 | 2021-06-22 | 浙江省林业科学研究院 | Preparation method of plant stem mould pressing tray |
| CN113238422A (en) * | 2020-01-22 | 2021-08-10 | 北京开阳亮微科技有限公司 | Ion transmission composite membrane, electrochromic glass comprising same and preparation method thereof |
| CN113238423A (en) * | 2020-01-22 | 2021-08-10 | 北京开阳亮微科技有限公司 | Ion transmission nano composite film, electrochromic glass comprising composite film and preparation method of electrochromic glass |
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| CN113238423A (en) * | 2020-01-22 | 2021-08-10 | 北京开阳亮微科技有限公司 | Ion transmission nano composite film, electrochromic glass comprising composite film and preparation method of electrochromic glass |
| CN113238422B (en) * | 2020-01-22 | 2022-12-02 | 青岛凯欧斯光电科技有限公司 | Ion transmission composite membrane, electrochromic glass comprising same and preparation method thereof |
| CN113238423B (en) * | 2020-01-22 | 2022-12-02 | 青岛凯欧斯光电科技有限公司 | Ion transmission nano composite film, electrochromic glass comprising composite film and preparation method of electrochromic glass |
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