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 PDF

Info

Publication number
CN106543612A
CN106543612A CN201610975475.1A CN201610975475A CN106543612A CN 106543612 A CN106543612 A CN 106543612A CN 201610975475 A CN201610975475 A CN 201610975475A CN 106543612 A CN106543612 A CN 106543612A
Authority
CN
China
Prior art keywords
pvb
sound insulation
resin powder
modified
nano
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610975475.1A
Other languages
Chinese (zh)
Other versions
CN106543612B (en
Inventor
谢怀玉
陈庚
许忠明
叶卫民
朱立疆
蔡海堤
王强
项舒武
金晓光
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Deste New Materials Ltd By Share Ltd
Original Assignee
Zhejiang Deste New Materials Ltd By Share Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Deste New Materials Ltd By Share Ltd filed Critical Zhejiang Deste New Materials Ltd By Share Ltd
Priority to CN201610975475.1A priority Critical patent/CN106543612B/en
Publication of CN106543612A publication Critical patent/CN106543612A/en
Application granted granted Critical
Publication of CN106543612B publication Critical patent/CN106543612B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06Layered 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
    • B32B17/10Layered 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
    • B32B17/10005Layered 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
    • B32B17/1055Layered 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/06Layered 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
    • B32B27/08Layered 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/18Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/42Layered products comprising a layer of synthetic resin comprising condensation resins of aldehydes, e.g. with phenols, ureas or melamines
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098Metal salts of carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/10Esters; Ether-esters
    • C08K5/101Esters; Ether-esters of monocarboxylic acids
    • C08K5/103Esters; Ether-esters of monocarboxylic acids with polyalcohols
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00Layers arrangement
    • B32B2250/033 layers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00Layers arrangement
    • B32B2250/24All layers being polymeric
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/10Properties of the layers or laminate having particular acoustical properties
    • B32B2307/102Insulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00Characterised 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
    • C08J2329/14Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2258Oxides; Hydroxides of metals of tungsten
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/16Applications 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

A kind of sound insulation PVB films and preparation method thereof
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.
CN201610975475.1A 2016-11-07 2016-11-07 A kind of sound insulation PVB film and preparation method thereof Active CN106543612B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610975475.1A CN106543612B (en) 2016-11-07 2016-11-07 A kind of sound insulation PVB film and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610975475.1A CN106543612B (en) 2016-11-07 2016-11-07 A kind of sound insulation PVB film and preparation method thereof

Publications (2)

Publication Number Publication Date
CN106543612A true CN106543612A (en) 2017-03-29
CN106543612B CN106543612B (en) 2019-02-12

Family

ID=58394179

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610975475.1A Active CN106543612B (en) 2016-11-07 2016-11-07 A kind of sound insulation PVB film and preparation method thereof

Country Status (1)

Country Link
CN (1) CN106543612B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
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

Also Published As

Publication number Publication date
CN106543612B (en) 2019-02-12

Similar Documents

Publication Publication Date Title
CN106543927B (en) A kind of modified PVB resin powder and preparation method thereof
CN106543612A (en) A kind of sound insulation PVB films and preparation method thereof
CN108148517B (en) Packaging adhesive film for solar cell and preparation method and application thereof
CN102636832B (en) Retardation film for retardation plate manufacture
CN109135625B (en) A kind of radiation resistance, glass sandwich film of the high grade of transparency and preparation method thereof
CN105283314A (en) Polymer interlayers having improved optical properties
CN108892906A (en) A kind of the PVB intermediate coat and preparation method of infrared barrier
US11173693B2 (en) Vinylidene fluoride-based resin multi-layered film
ITMI20101237A1 (en) MATERIAL BASED ON CELLULOSE ACETATE WITH PLASTICIZERS AND MANUFACTURE OBTAINED WITH THIS PRODUCT.
CN109762490B (en) Heat-insulating PVB film and preparation method thereof
US20140370263A1 (en) Plasticizable heat-insulating composition, transparent heat-insulating intermediate sheet and transparent heat-insulating sandwich-structured panel
CA2379380A1 (en) Polypropylene base porous film and production process for the same
CN102181208A (en) Heat reflection heat insulation coating for outer wall
DE112012006554T5 (en) Highly miscible polymer blends and their use
CN107118481A (en) A kind of outdoor section bar composite protection film and preparation method thereof
CN108503892A (en) A kind of sericite composite material and preparation method in plastic, transparent masterbatch
CN102993613A (en) Photochromic material as well as preparation method and application of photochromic material
CN107323056A (en) A kind of PVB films and preparation method with sound insulation value
KR101315512B1 (en) (meth)acrylic resin composition and optical film comprising the same
CN106957621A (en) A kind of PVB films preparation method and applications of nano heat-insulating dispersion
CN111572139B (en) Colorful high-brightness high-transmittance antibacterial polyester film for packaging printing and preparation method thereof
CN105924905B (en) A kind of polyester film
CN107955304A (en) A kind of photovoltaic PVB resin and its production method and the method using resin-oatmeal production photovoltaic PVB films
CN107033509A (en) PVB films of infrared high-barrier high transmission rate and preparation method thereof in a kind of
CN110699017B (en) Polyvinyl butyral ultra-white transparent film and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: A sound insulation PVB film and its preparation method

Effective date of registration: 20200909

Granted publication date: 20190212

Pledgee: Zheshang Bank Limited by Share Ltd. Taizhou branch

Pledgor: ZHEJIANG DECENT NEW MATERIAL Co.,Ltd.

Registration number: Y2020330000682

PE01 Entry into force of the registration of the contract for pledge of patent right