CN106543612A - A kind of sound insulation PVB films and preparation method thereof - Google Patents
A kind of sound insulation PVB films and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/42—Layered products comprising a layer of synthetic resin comprising condensation resins of aldehydes, e.g. with phenols, ureas or melamines
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
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- C08K5/00—Use of organic ingredients
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- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/03—3 layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/24—All layers being polymeric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/10—Properties of the layers or laminate having particular acoustical properties
- B32B2307/102—Insulating
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- C08J2329/00—Characterised by the use of 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; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- 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
- C08K2003/2258—Oxides; Hydroxides of metals of tungsten
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
The present invention relates to a kind of sound insulation PVB films and preparation method thereof, are constituted by A, B, C three-layer thin-film is compound successively, intermediate layer B film thicknesses are 100 200 microns, and on the outside of A and C, two layers of thickness is 300 500 microns;The intermediate layer B thin-film materials are prepared by the modified PVB resin powder that melting means is 6 10g/10min, and on the outside of A and C, double-layer filmses material is prepared by the modified PVB resin powder that melting means is 4 5g/10min.The three layers of sound insulation PVB films for preparing can effectively intercept the noise in the range of human ear 1000 4000Hz of sensitivity, and 3 5dB of soundproof effect can be lifted compared with general thickness PVB.
Description
Technical field
The present invention relates to a kind of sound insulation PVB films, belong to folder acoustic mastic glass applications field.
Background technology
Sound is a kind of vibration wave, and the especially sensitive frequency of human ear is 1000~4000Hz.The terminal in glass applications field
Client reduces noise to automobile and building glass and increasingly payes attention to, while also emphasis considers safety factorss, because noise pollution, shadow
Ring the working environment and comfortableness of people.
Past people generally utilize solid or substantial amounts of product design unit usually increase thickness of glass, with improve glass every
Sound performance, however as pay attention to day by day of the people to environmental problem, the limitation of Glass Design, increasing thickness and hardness has necessarily
Restriction, " environmental protection " has also become the matter of utmost importance that automaker and builder face, and wherein automotive light weight technology is then gone up
It is upgraded to important Consideration in Automobile Design.Therefore decay can only be increased, by adding viscoelastic plastics, noise is changed into
Vibrational energy, and then it is changed into heat energy.Therefore, the energy such as the noise of electromotor, road traffic noise, undesirable sound of the wind how to be reduced
Enough incoming noises are the key subjects of.
PVB laminated glass has higher security performance, is widely used with automotive field in building.With making an uproar
The exploitation of deadener is tried to explore in sound pollution problem, PVB doubling glass industry in recent years, and United States Patent (USP) US5340654 is proposed
An a kind of layer includes the PVB with 30-80% vinyl acetate contents.Chinese patent CN200910159694.2 is disclosed
A kind of PVB multifilms of with sound insulation value at least two points of thin film composition, wherein first point of thin film contains polyvinyl acetate
Vinegar group ratio is the PVB of PVB and second point of thin film ratio containing vinyl acetate for 5-8% of 0.1-11%.Also there are other special
Profit reaches the report of soundproof effect in the monolayer PVB films using special formulation, but does not commercially have Related product to go out
It is existing.Below all it is, by using MULTILAYER COMPOSITE technology, and to change the structure or PVB plasticizer proportionings of different layers PVB resin
To realize sound insulation value.But PVB resin structure is improved, by increasing fourth aldehyde group content, hydroxy radical content is reduced, or increases increasing
Modeling agent proportioning has following risk come the mechanical loss factor for regulating and controlling different PVB layers:The mechanical properties decrease of film, ageing properties
Reduce, it is plasticizer extraction etc..Meanwhile, prior art is when plural layers are prepared as material property differs greatly, it is difficult to formed
The thin film of thickness uniformity, processing difficulties cause practicality not strong, do not have the marketization.
The content of the invention
Sound insulation PVB films are mainly three-decker at present, the hydroxyl of existing document and patent by change different layers PVB resin
Based component ratio or PVB plasticizer proportionings, this kind of design possess feasibility in theory, but the curtain coating of trilamellar membrane is processed
There are many difficulties in process, such as addition auxiliary agent dispersion problem of non-uniform, trilamellar membrane plasticizer is inconsistent causes follow-up plasticizer to exist
Different layers are migrated and precipitation problem, middle puigging poor fluidity cause intermediate layer thickness problem of non-uniform, so as to ultimately result in
Sound insulation PVB films are unable to industrialized production, and practicality is not strong.
In order to solve the above-mentioned problems in the prior art, the present invention provides a kind of sound insulation PVB films and its preparation side
Method.Sound insulation PVB films of the present invention are constituted by A, B, C three-layer thin-film is compound successively, and intermediate layer B film thicknesses are 100-
200 microns, on the outside of A and C, two layers of thickness is 300-500 microns.Wherein the raw material PVB resin powder of intermediate layer B thin film is Gao Rong
Refer to product, play sound-insulating and heat-insulating and phototropic effect, two outside layers A and C have good cohesive force to glass.
Further, modified PVB resin powder of the intermediate layer B thin-film materials by melting means for 6-10g/10min is prepared into
Arrive, with high fluidity, curtain coating is easily formed the uniform thin film of 100-200 microns.
Further, B film resins formula (mass ratio):72% modified PVB resin powder and 28% plasticizer 3G8.
Further, on the outside of A and C, modified PVB resin powder of the double-layer filmses material by melting means for 4-5g/10min is prepared into
Arrive, mobility is poor, the film of formation is easily controllable in 300-500 microns.
Further, A and C film resins formula (mass ratio):72% modified PVB resin powder and 28% plasticizer
3G8。
Further, the component and mass percent of described modified PVB resin powder is:
Polyvinyl alcohol:8-8.5wt%
N-butyl alcohol:4.5-5wt%
Antioxidant:0.01-0.03wt%
Ultraviolet absorber:0.01-0.02wt%
Nano-oxide:0-0.02%wt
Surface tension modifier:0-0.01wt%
Hydrochloric acid:2-3wt%
Balance of water.
Further, the antioxidant is selected from the mixture of phenols and phosphorous acid esters, wherein described phenols is selected from four
(3,5- di-t-butyl -4- hydroxyls) benzenpropanoic acid pentaerythritol ester (being commonly called as 1010), 2- di-2-ethylhexylphosphine oxides (4- methyl-6-tert butyl benzene
Phenol), the one kind in β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propanoic acid;Described phosphorous acid esters are selected from
Three (2,4- di-t-butyl) phenyl-phosphite (being commonly called as 168), double penta diphosphites of stearyl alcohol season, double (3,5- bis- tertiary fourths
Base phenyl) one kind in pentaerythritol diphosphites.
Further, described UV absorbers are Benzotriazole Ultraviolet Stabilizer, selected from 2- (2 ˊ-hydroxyl -5
ˊ-methyl)-benzotriazole, 2- (2 ˊ--3 ˊ of hydroxyl--5 ˊ of the tert-butyl group-methyl) the chloro- benzotriazole of -5-, 2- (5 ˊ of -3 ˊ of 2 ˊ-hydroxyl -
Di-t-butyl) the chloro- benzotriazole of -5-, 2'- (the 2'- hydroxyl -3'- tert-butyl group -5'- aminomethyl phenyls) -5- chlorobenzotriazoles (be commonly called as
UV-326 it is), a kind of in 2- (2 ˊ--5 ˊ of hydroxyl-t-octyl)-benzotriazole.
Further, the surface tension modifier is inorganic salts, selected from potassium acetate, potassium formate, magnesium acetate, acetic acid
One kind in calcium, sodium acetate.
Further, the nano-oxide is nano-ITO, nano ATO, nanometer GTO, the one kind in nanometer tungsten bronze;
More preferably nanometer tungsten bronze.
Further, when for preparing the intermediate layer B thin film of sound insulation PVB films, raw material PVA viscosity is controlled to 24-
28mPas (testing standard GB/T 12010.2-2010), average degree of polymerization 1500-1800 (testing standard GB/T 12010.5-
2010), alcoholysis degree 98-99% (testing standard GB/T 12010.5-2010), the commercially available trade mark in market have Changchun chemical industry (river
Soviet Union) the company limited trade mark BF-14, BF-17, BF-14W.
Further, when for preparing A the and C layer films of sound insulation PVB films, raw material PVA viscosity is 28-
30mPas (test mark GB/T12010.2-2010), average degree of polymerization 1700-2500 (testing standards GB/T12010.5-
2010), alcoholysis degree 98-99% (testing standard GB/T 12010.5-2010), the commercially available trade mark in market have Changchun chemical industry (river
Soviet Union) the company limited trade mark BP-20, BP-24, BP-26.
Further, the mass concentration of the hydrochloric acid is 31% (testing standard GB 320-2006).
Further, the pure resistivity of water >=18M Ω .CM (testing standard GB6682-92).
The present invention also protects the preparation method of above-mentioned modified PVB resin powder, i.e., by synthesizing from raw material PVB resin powder
Add antioxidant, ultraviolet absorber, surface tension modifier, nano-oxide in journey.
Further, concrete step is:
(1) condensation reaction
First, solution of the concentration less than 10% is made into 90-95 DEG C of water and appropriate polyvinyl alcohol, the solution is lowered the temperature
To after 40-45 DEG C, hutanal, and the antioxidant by proportioning, ultraviolet absorber, nano-oxide, surface tension adjustment are added
Agent.Stirring 1-3h;After reaction mixture is cooled to 20-25 DEG C, the appropriate hydrochloric acid of addition, insulation reaction at least 1-5 hours, then will
Reaction mixture is delivered to condensation reaction kettle, and 40 DEG C were gradually heating at 1 hour, then insulation reaction 1-2 hour, afterwards again
55 DEG C, then insulation reaction 1-2 hour were gradually heating to 1 hour, are then cooled to room temperature;
(2) neutralisation treatment
Reactant liquor after the cooling is delivered to washing kettle to wash 5-6 time, 40-50 DEG C is warming up to afterwards, is added appropriate
Soda bath adjusts pH value to 8-10, then is incubated 2-3 hours, fully neutralization deacidification;
(3) it is dehydrated and is dried
Reactant liquor after the neutralization deacidification is washed after 6-8 time again and is less than to moisture content Jing after centrifuge dewatering
30%, enter with air-flow and be obtained after cyclone dryer drying the modified PVB resin powder.
Compared with prior art, the beneficial effects of the present invention is:
(1) antioxidant, ultraviolet absorber be modified used in resin-oatmeal building-up process, nano-oxide and surface tension
Regulator is modified, and in the range of the concrete composition of above-mentioned auxiliary agent and proportioning, synergistic between each composition arrives
Fully play, technique effect is optimal.On the one hand, heat resistance is good, shows 2 hours values of chromatism of resistance to 180 DEG C of constant temperature and is less than 1, passes
The PVB resin powder temperature tolerance of system production is poor, easy xanthochromia, and resistance to 180 DEG C of constant temperature, the 2 hours values of chromatism of performance are between 1-2.5.The opposing party
Face, shows good heat-proof quality, and it is, more than 20%, especially to use to show as the modified PVB resin powder infrared barrier rate of nano-ITO
The modified PVB resin powder of nanometer tungsten bronze is more than 90% to infrared rejection rate, and conventional PVB resin powder is to infrared rejection rate
Less than 10%.Have again and there is to glass moderate adhesion strength exactly, it is 5-6 level levels to show as the percussion value to glass, and
Conventional PVB resin powder is 7-9 levels to the caking property percussion value of glass.
(2) preparation method of the invention cleverly addition antioxidant, ultraviolet suction in raw material PVB resin powder building-up process
Receive agent, surface tension modifier, function nano particle so that these auxiliary agents are may be uniformly dispersed in resin-oatmeal, are modified
PVB resin powder, the modified PVB resin powder of acquisition directly together with plasticizer can be extruded curtain coating and produce PVB films so that PVB
Eliminate PVB resin powder and antioxidant, ultraviolet absorber, surface tension modifier, nanoparticle to mix in film production technology
Material premix link, thoroughly solves nanoparticle and auxiliary agent and disperses problem of non-uniform in resin-oatmeal, improve PVB film extrusions
The production efficiency of curtain coating, eliminates spice premix link and can be prevented effectively from powder body pollution.
(3) the three layers of sound insulation PVB films prepared using the different modified resin powder of the present invention effectively can be intercepted
Noise in the range of human ear sensitivity 1000-4000Hz, can lift soundproof effect 3-5dB compared with general thickness PVB.
Description of the drawings
The SEM figures of sound insulation PVB films material object prepared by Fig. 1 embodiments 7
Sound insulation PVB films prepared by Fig. 2 embodiments 7 are contrasted with the soundproof effect of common PVB laminated glass
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and not structure
Into limitation of the present invention.
The concrete preparation method of modified resin powder is as follows
(1) condensation reaction:
First, solution of the concentration less than 10% is made into using 95 DEG C of water and appropriate polyvinyl alcohol in a kettle., will
The solution cool to 45 DEG C add appropriate auxiliary agents (antioxidant, ultraviolet absorber, nano-oxide, surface tension modifier) and
Hutanal is stirred 1h;Secondly, the reaction mixture is cooled to into 20 DEG C, adds appropriate hydrochloric, insulation is anti-
Answer at least 1 hour, then reaction mixture is delivered to into two kettles of condensation, 40 DEG C were gradually heating at 1 hour, then insulation reaction 1 is little
When, 55 DEG C were gradually heating to 1 hour again afterwards, then insulation reaction 1 hour, then cool to room temperature;
(2) neutralisation treatment:
Reactant liquor after the cooling is delivered to washing kettle to wash 6 times, 45 DEG C are warming up to afterwards, adds appropriate Caustic soda molten
Liquid adjusts pH value to 9, then is incubated 3 hours, fully neutralization deacidification;
(3) it is dehydrated and is dried:
Reactant liquor after the neutralization deacidification is washed after 6 times again Jing after centrifuge dewatering to moisture content less than 30% with
Air-flow is obtained the modified polyvinyl butyral resin finished product after entering cyclone dryer drying.
Embodiment 1-6 is prepared according to above-mentioned concrete preparation method, and concrete raw material and proportioning are referring to table 1.Comparative example
In without any auxiliary agent, be also prepared according to above-mentioned concrete preparation method.
The formula of the PVB resin powder of 1 embodiment of table and comparative example
For the explanation of table 1:
(1) embodiment 1-3 is the PVA raw materials for adopting, and PVA viscosity is controlled to 24-28mPas (testing standards GB/T
12010.2-2010), average degree of polymerization 1500-1800 (testing standard GB/T12010.5-2010), alcoholysis degree 98-99% (are surveyed
The quasi- GB/T 12010.5-2010 of test-object), market purchase is BF-14 for the trade mark of Changchun chemical industry (Jiangsu) company limited production, instead
It is high to melt finger that sound insulation resin PVB should be synthesized, and melts finger at 6-10g/10min (140 DEG C, 21.6kg counterweights), and feature is processing levelling
Property it is good, curtain coating be easily formed the uniform thin film of 100-200 microns.For preparing intermediate layer film.
(2) embodiment 4-6 is the PVA raw materials for adopting, and PVA viscosity is 28-30mPas (test mark GB/T12010.2-
2010), average degree of polymerization 1700-2500 (testing standard GB/T 12010.5-2010), alcoholysis degree 98-99% (testing standards
GB/T 12010.5-2010), market purchase is BP-20 for the trade mark of Changchun chemical industry (Jiangsu) company limited production, and reaction obtains
PVB features are to melt that finger is relatively low, and viscosity is high, and mechanical mechanics property is good, it is ensured that the safety of doubling glass.For preparing bottom thin
Film.
Following performance test is carried out to the above-mentioned modified PVB resin powder for preparing.
(1) melt finger method of testing:
1st, instrument:XNR-400GM type melt flow rate (MFR) analyzers, Changzhou De Tu precision instruments company limited.
2nd, method:By plasticizer:PVB powder material=1:3 ratio weighs corresponding 3G8 plasticizers and PVB powder material, past
In the PVB resin powder of 3.75g, accurate Deca 1.25g plasticizer, is uniformly mixing to obtain testing sample with Glass rod.Wait XNR-
400GM type melt flow rate (MFR) analyzer barrels are warming up to 140 DEG C of setting value, stable 10min, extract piston rod, plus treat test sample
Product.Piston rod compacting is reinserted, 21.6kg counterweights are added after 4~6 minutes temperature stabilizations, when material bar drops to lower Marking ring
Start test when mutually neat with barrel, mono- sample of testing time 5min is weighed from the weight for melting the batten for referring to that tester membrana oralis flows out
For m1, m2, m3, m4, m5.
3 calculate:Melt finger=(m1+m2+m3+m4+m5) * 2/5 (unit:g/10min)
(2) chromatism test method:
1st, take the ultra-clear glasses (thickness of 2 pieces of wiped cleans:2mm length:10cm width 10cm).
2nd, the PVB resin powder of 3-5g is taken, is uniformly layered in the middle of 2 blocks of glass, be then placed within 180 DEG C of drying baker constant temperature 10
Minute obtains test sample.Sample is cooled to room temperature and measures L*1, a*1, b*1 using Agilent CARRY5000 color difference meter.
3rd, sample is put into into constant temperature 2 hours in 180 DEG C of drying baker, sample be cooled to room temperature using color difference meter measure L*2,
A*2, b*2.
4th, value of chromatism is calculated:Aberration to be referred to and represent that two kinds of colors give people the difference on color perception with the method for numerical value.
CIE1976 (or L*a*b*) system, become now countries in the world formally adopt, as international colour examining standard.Change
Property 180 DEG C of PVB resin powder in drying baker constant temperature 2 hours sample is all pressed L*, a*, b* and demarcates color in front and back, then 180 DEG C it is permanent
2 hours total color difference △ E*ab and every individual event aberration in front and back between the two of temperature can be calculated with following equation:
Luminosity equation:△ L*=L*1-L*2 formulas (1)
Colour difference:△ a*=a*1-a*2;△ b*=b*1-b*2 formulas (2)
Total color difference:ΔE* ab=[(Δ L*)2+(Δa*)2+(Δb*)2]1/2Formula (3)
(3) infrared barrier rate method of testing:Test according to 2680 sample preparation of GB GB/T.
(4) percussion value method of testing:Test according to the sample preparation of industry standard JC/T2166-2013.
Concrete test result is as follows:
The characteristic of table 2PVB resin-oatmeals
Can be seen that from above-mentioned test result:The resin-oatmeal of the present invention is through antioxidant, ultraviolet absorber, follow-up PVB glue
In the piece course of processing can be without this analog assistant, it is to avoid breading operation, reduce powder body pollution, the resistance to ring of the PVB resin that is modified powder
Border excellent performance, shows as modified PVB resin powder 180 DEG C of temperature constant temperature 2 hours chroma difference less than 1, and comparative example is not used
Modified 180 DEG C of the conventional PVB resin powder constant temperature 2 hours chroma difference of antioxidant and ultraviolet absorber is more than 1;Infrared heat-proof quality
Excellent, embodiment 1 and 3 is modified using nano-ITO, and infrared barrier rate is more than 20%;Embodiment 2 is modified using nanometer tungsten bronze,
Infrared barrier rate is more than 90%, and embodiment 4 and comparative example do not use nano-oxide to be modified, and infrared barrier rate is less than 10% water
It is flat;Caking property of the PVB films to glass is effectively controlled, by JC/T2166-2013 standards, embodiment of the present invention 1-6 is used
The modified PVB resin powder of surface tension modifier taps value stabilization in 5-6 level levels to the adhesion strength index of glass, and contrasts
It is 7-9 levels to the adhesion strength index percussion value of glass that example 1-2 does not use the conventional PVB resin powder powder of surface tension modifier.
Embodiment 7
The modified PVB resin powder 72kg of Example 1, the common 28kg of plasticizer 3G8, are existed by 52 type double screw extruders
Plastify at a temperature of 160 DEG C, plasticizing resin imports the middle B modules of three layers of mould;The modified PVB resin powder of Example 5
The common 28kg of 72kg, plasticizer 3G8, is plastified at a temperature of 160 DEG C by 95 type double screw extruders, and three layers of mould are imported after plasticizing
The outer layer A and C of tool.The PVB films with sound insulation value are obtained by three layers of mould film extrusion.
Product is carried out into sem analysis, and its soundproof effect is tested, it is as a result as follows:
From accompanying drawing 1 as can be seen that the intermediate layer B thickness of the PVB films is 131 microns, outer layer A is 375 microns, and C is
437 microns.
From accompanying drawing 2 as can be seen that sound insulation film lifts soundproof effect 3-5 decibels relative to conventional film, wherein, test mark
Accurate is GB/T8485-2008, and glass structure is 2mm glass+0.76PVB film+2mm glass.
Although by referring to the preferred embodiments of the present invention, invention has been described, this area it is common
It will be appreciated by the skilled person that various changes can be made in the form and details to which, without departing from appended right
The spirit and scope of the present invention limited by claim.
Claims (7)
1. a kind of sound insulation PVB films, it is characterised in that constituted by A, B, C three-layer thin-film is compound successively, intermediate layer B film thicknesses
For 100-200 microns, on the outside of A and C, two layers of thickness is 300-500 microns;The intermediate layer B thin-film materials are 6-10g/ by melting means
The modified PVB resin powder of 10min is prepared, and on the outside of A and C, double-layer filmses material is by the modified PVB that melting means is 4-5g/10min
Resin-oatmeal is prepared.
2. sound insulation PVB films according to claim 1, it is characterised in that three-layer thin-film resin formula be 72% it is modified
PVB resin powder and 28% plasticizer 3G8.
3. sound insulation PVB films according to claim 1, it is characterised in that the component and matter of described modified PVB resin powder
Measuring percent is:
Polyvinyl alcohol:8-8.5wt%
N-butyl alcohol:4.5-5wt%
Antioxidant:0.01-0.03wt%
Ultraviolet absorber:0.01-0.02wt%
Nano-oxide:0-0.02%wt
Surface tension modifier:0-0.01wt%
Hydrochloric acid:2-3wt%
Balance of water.
4. sound insulation PVB films according to claim 3, it is characterised in that the antioxidant is selected from phenols and phosphite ester
The mixture of class, wherein described phenols is selected from four (3,5- di-t-butyl -4- hydroxyls) benzenpropanoic acid pentaerythritol ester, 2- methylene
One kind in double (4- methyl-6-tert-butylphenols), β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propanoic acid;
Described phosphorous acid esters are selected from three (2,4- di-t-butyls) phenyl-phosphite, double penta diphosphites of stearyl alcohol season, double
One kind in (3,5- di-tert-butyl-phenyl) pentaerythritol diphosphites;Described UV absorbers are that benzotriazole is purple
Ultraviolet absorbers, selected from 2- (2 ˊ--5 ˊ of hydroxyl-methyl)-benzotriazole, 2- (2 ˊ--3 ˊ of hydroxyl--5 ˊ of the tert-butyl group-methyl) -5-
Chloro- benzotriazole, 2- (- 35 ˊ of ˊ of 2 ˊ-hydroxyl-di-t-butyl) the chloro- benzotriazole of -5-, the 2'- (2'- hydroxyl -3'- tert-butyl group -5'-
Aminomethyl phenyl) it is -5- chlorobenzotriazoles, a kind of in 2- (2 ˊ--5 ˊ of hydroxyl-t-octyl)-benzotriazole;The surface tension adjustment
Agent is inorganic salts, the one kind in potassium acetate, potassium formate, magnesium acetate, calcium acetate, sodium acetate;The nano-oxide is
One kind in nano-ITO, nano ATO, nanometer GTO, nanometer tungsten bronze;More preferably nanometer tungsten bronze;The quality of the hydrochloric acid
Concentration is 31%;The pure resistivity of water >=18M Ω .CM.
5. sound insulation PVB films according to claim 3, it is characterised in that when for preparing the intermediate layer of sound insulation PVB films
During B thin film, raw material PVA viscosity is controlled to 24-28mPas, average degree of polymerization 1500-1800, alcoholysis degree 98-99%;When with
When A the and C layer films of sound insulation PVB films are prepared, raw material PVA viscosity is 28-30mPas, average degree of polymerization 1700-
2500, alcoholysis degree 98-99%.
6. sound insulation PVB films according to claim 3, it is characterised in that the preparation method of the modified PVB resin powder
For by adding antioxidant, ultraviolet absorber, surface tension modifier, nano oxygen from raw material PVB resin powder building-up process
Compound.
7. sound insulation PVB films according to claim 6, it is characterised in that the preparation method of the modified PVB resin powder
For:
(1) condensation reaction
First, solution of the concentration less than 10% is made into 90-95 DEG C of water and appropriate polyvinyl alcohol, the solution is cooled to
After 40-45 DEG C, hutanal, and the antioxidant by proportioning, ultraviolet absorber, nano-oxide, surface tension modifier are added.
Stirring 1-3h;After reaction mixture is cooled to 20-25 DEG C, the appropriate hydrochloric acid of addition, insulation reaction at least 1-5 hours, then will be anti-
Answer mixed liquor to be delivered to condensation reaction kettle, 40 DEG C were gradually heating at 1 hour, then insulation reaction 1-2 hour, afterwards again with 1
Hour is gradually heating to 55 DEG C, then insulation reaction 1-2 hour, then cools to room temperature;
(2) neutralisation treatment
Reactant liquor after the cooling is delivered to washing kettle to wash 5-6 time, 40-50 DEG C is warming up to afterwards, appropriate Caustic soda is added
Solution adjusts pH value to 8-10, then is incubated 2-3 hours, fully neutralization deacidification;
(3) it is dehydrated and is dried
Reactant liquor after the neutralization deacidification is washed again 30% is less than to moisture content Jing after centrifuge dewatering after 6-8 time, with
Air-flow is obtained the modified PVB resin powder after entering cyclone dryer drying.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107323056A (en) * | 2017-06-02 | 2017-11-07 | 忠信(清远)光伏材料科技有限公司 | A kind of PVB films and preparation method with sound insulation value |
CN108032579A (en) * | 2017-11-30 | 2018-05-15 | 浙江德斯泰新材料股份有限公司 | A kind of internally plasticized sound insulation PVB films and preparation method |
CN108724868A (en) * | 2017-04-14 | 2018-11-02 | 浙江德斯泰新材料股份有限公司 | A kind of heat-insulating sound-insulating PVB films and preparation method thereof |
CN109486075A (en) * | 2018-10-24 | 2019-03-19 | 吉林诺德高科新材料有限公司 | A kind of polyvinyl butyral film modified resin and the preparation method and application thereof |
CN113072899A (en) * | 2021-03-30 | 2021-07-06 | 深圳市捷源环保科技有限公司 | PVB film with excellent sound absorption characteristic and manufacturing method thereof |
Citations (1)
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CN101637991A (en) * | 2008-08-01 | 2010-02-03 | 可乐丽欧洲有限责任公司 | Multilayer films of plasticizer-containing polyvinyl acetal with sound-absorbing properties |
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2016
- 2016-11-07 CN CN201610975475.1A patent/CN106543612B/en active Active
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101637991A (en) * | 2008-08-01 | 2010-02-03 | 可乐丽欧洲有限责任公司 | Multilayer films of plasticizer-containing polyvinyl acetal with sound-absorbing properties |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108724868A (en) * | 2017-04-14 | 2018-11-02 | 浙江德斯泰新材料股份有限公司 | A kind of heat-insulating sound-insulating PVB films and preparation method thereof |
CN107323056A (en) * | 2017-06-02 | 2017-11-07 | 忠信(清远)光伏材料科技有限公司 | A kind of PVB films and preparation method with sound insulation value |
CN108032579A (en) * | 2017-11-30 | 2018-05-15 | 浙江德斯泰新材料股份有限公司 | A kind of internally plasticized sound insulation PVB films and preparation method |
CN109486075A (en) * | 2018-10-24 | 2019-03-19 | 吉林诺德高科新材料有限公司 | A kind of polyvinyl butyral film modified resin and the preparation method and application thereof |
CN113072899A (en) * | 2021-03-30 | 2021-07-06 | 深圳市捷源环保科技有限公司 | PVB film with excellent sound absorption characteristic and manufacturing method thereof |
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