CN106752995B - A kind of polyvinyl butyral film and preparation method thereof - Google Patents

A kind of polyvinyl butyral film and preparation method thereof Download PDF

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Publication number
CN106752995B
CN106752995B CN201611121206.5A CN201611121206A CN106752995B CN 106752995 B CN106752995 B CN 106752995B CN 201611121206 A CN201611121206 A CN 201611121206A CN 106752995 B CN106752995 B CN 106752995B
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resin
pvb
film
preparation
polyvinyl butyral
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CN106752995A (en
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朱金凤
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Faithful (qingyuan) Photovoltaic Mstar Technology Ltd
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Faithful (qingyuan) Photovoltaic Mstar Technology Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • 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
    • B32B7/00Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04Interconnection of layers
    • B32B7/12Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J129/00Adhesives 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
    • C09J129/14Homopolymers 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
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Joining Of Glass To Other Materials (AREA)

Abstract

The present invention relates to a kind of polyvinyl butyral film and preparation method thereof.Methods described is characterised by, including 5 preparation polyvinyl butyral resin, batch mixing, plasticizing extrusion, cooling and shaping and winding, cutting and winding steps.After the method for the invention is by using two kinds of resin mixing technologies, the mobility of resin has greatly improved;When the film produced using this method does roll-in, roll-in speed can be improved to 1.5m/min from 1.2m/min, can improve the production efficiency of glass laminating processing, reduces production cost;Application method production film can not only save the dosage of a resin, reduce production cost, and its film performance produced also is improved to 95% with a resin property without significant difference, the repair rate of glass laminating from the 85% of the typically resin doubling containing recovery.

Description

A kind of polyvinyl butyral film and preparation method thereof
Technical field
The invention belongs to thermoplastic macromolecule material technical field, and in particular to a kind of polyvinyl butyral film and its Preparation method.
Background technology
Polyvinyl alcohol contracting butanol (Polyvinyl Butyral, PVB) be by polyvinyl alcohol (Polyvinyl Alcohol, PVA) the product being condensed with butyraldehyde under acid environment catalysis.PVB is due to containing compared with long-chain branch, having and the material such as glass, metal Very high bonding force.PVB not only has the bonding force excellent with the material of many classifications, also with excellent transparency, well Dissolubility, and superior fast light, water-fast, heat-resisting, cold-resistant and film forming., can be by HMW according to these characteristics After PVB resin adds plasticizer, film is squeezed into, the sandwich material as safety glass.When safety glass is by foreign body During shock, only irregular rayed split can be formed in rum point, glass fragment is still firmly sticked on PVB intermediate coats and protected Hold and do not disperse, do not fall off so as to avoid making one causing injury, and in the case of not influenceing sight within a certain period of time, can continue to make With.Therefore, PVB especially turns into a kind of indispensable synthetic resin material in manufacture laminated safety glass field.At present, the world Upper more than 80% PVB resin is used for the sandwich material of safety glass.
Due to the block of PVB film production technologies, PVB production in the world is concentrated mainly on the U.S., Japan and Germany etc. Several national trans-corporations, such as Meng Shan all, Du Pont, Dynamit Nobel AG, electrochemically with ponding chemistry.There is number the country The producer of ten production PVB films, but the PVB films producer of most domestic is produced using reclaimed materials, use is pure The producer of PVB resin production is seldom.Due to material by heating for multiple times down to Partial digestion, the reclaimed rubber for using reclaimed materials to produce The softening point of piece is relatively low, glass factory's roll-in technological requirement than relatively low, but it is this regeneration film performance it is relatively low, glass clamp The repair rate of glue is higher.The PVB films produced using pure PVB resin are due to being a resin, and film performance is secure, but glue Piece cost is high, and its rolling process requires higher, and roll-in speed is relatively low, low production efficiency.How the performance and glue of PVB film is balanced The requirement of piece rolling process is those skilled in the art's technical issues that need to address.
The content of the invention
In order to solve, prior art is unable to the performance of active balance polyvinyl butyral film and film rolling process will The problem of asking, it is an object of the invention to provide a kind of preparation method of polyvinyl butyral film, it is characterised in that including with Lower step:
(1) preparation polyvinyl butyral resin:Viscosity solution is used to obtain viscosity with recovery resin-made as 50-100cp/20 DEG C PVB-1 resins, use viscosity solution and a resin-made to obtain viscosity as 250-300cp/20 DEG C of PVB-2 resins, wherein The viscosity solution is 3-7wt% butanol solution;
(2) batch mixing:5-15 part PVB-1 resins and 100 parts of PVB-2 resins are carried out circulating batch mixing to be made within 2 hours and mix PVB Resin;
(3) plasticizing extrusion:Squeezed by weight 1 part of plasticizer is mixed into the mixed merga pass extruder of PVB resin with 3 parts Go out, the temperature wherein inside extruder is warming up to 165 DEG C of outlet temperature for 45 DEG C by inlet temperature;
(4) cooling and shaping:The PVB film cooling and shapings of extrusion, wherein water temperature are maintained at 20-25 using water-cooling process ℃;
(5) using winder by the PVB film rolls after sizing around, cut and wind.
Further, the hydroxy radical content of the recovery resin and a resin is 19-22wt%.
Further, the viscosity solution is preferably 5wt% butanol solution.
It is a further object of the present invention to provide a kind of polyvinyl butyral film, it is characterised in that by any of the above-described poly- The preparation method of vinyl butyral film obtains.
Further, the polyvinyl butyral film can be used for the interlayer of manufacture laminated glass.
A resin of the present invention refers to the product being condensed by direct polyvinyl alcohol and butyraldehyde under acid environment catalysis, I.e. without the resin of recycling.
The preparation method of polyvinyl butyral film of the present invention compared with prior art the advantages of be:
(1) after using two kinds of resin mixing technologies, the melt index of resin carries from the 0.4-0.7g/10min of a resin Up to 0.8-1.3g/10min, the mobility of resin have greatly improved;
(2) when the film produced using this preparation method does roll-in, roll-in speed can be improved from 1.2m/min to 1.5m/ Min, the production efficiency of glass laminating processing can be improved, reduce production cost;
(3) dosage of a resin can be not only saved using preparation method production film, reduces production cost, it is produced The film performance gone out is also with a resin property without significant difference, and the repair rate of glass laminating is from the typically resin doubling containing recovery 85% improves to 95%.
Brief description of the drawings
Fig. 1 is a kind of overall flow figure of the preparation method of polyvinyl butyral film of the embodiment of the present invention.
Embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings.The refer to the attached drawing The embodiment of description is exemplary, is only used for explaining the present invention, and can not be considered as limitation of the present invention.In order to avoid need not Strategic point obscures the embodiment, and this part to some techniques knowns, i.e., is aobvious to those skilled in the art And the technology being clear to, it is not described in detail.
Preparation method embodiment 1
A kind of preparation method of polyvinyl butyral film, it is characterised in that comprise the following steps:
(1) preparation polyvinyl butyral resin:Use recovery resin-made of the viscosity solution with hydroxy radical content for 22wt% The PVB-1 resins that viscosity is 75cp/20 DEG C are obtained, use viscosity solution to obtain viscosity with hydroxy radical content for a 19wt% resin-made For 261cp/20 DEG C of PVB-2 resins, wherein the viscosity solution is 5wt% butanol solution;
(2) batch mixing:10 parts of PVB-1 resins and 100 parts of PVB-2 resins are carried out to circulate batch mixing 2 hours;
(3) plasticizing extrusion:Squeezed by weight 1 part of plasticizer is mixed into the mixed merga pass extruder of PVB resin with 3 parts Go out, the temperature wherein inside extruder is warming up to 165 DEG C of outlet temperature for 45 DEG C by inlet temperature;
(4) cooling and shaping:Using water-cooling process by the PVB film cooling and shapings of extrusion, wherein, water temperature is maintained at 25 DEG C;
(5) using winder by the PVB film rolls after sizing around, cut and wind.
Preparation method embodiment 2
A kind of preparation method of polyvinyl butyral film, it is characterised in that comprise the following steps:
(1) preparation polyvinyl butyral resin:Use recovery resin-made of the viscosity solution with hydroxy radical content for 21wt% Viscosity is 90cp/20 DEG C of PVB-1 resins, use viscosity solution hydroxy radical content to obtain viscosity for a 20wt% resin-made to be 285cp/20 DEG C of PVB-2 resins, wherein the viscosity solution is 7wt% butanol solution;
(2) batch mixing:15 parts of PVB-1 resins and 100 parts of PVB-2 resins are carried out to circulate batch mixing 2 hours;
(3) plasticizing extrusion:Squeezed by weight 1 part of plasticizer is mixed into the mixed merga pass extruder of PVB resin with 3 parts Go out, the temperature wherein inside extruder is warming up to 165 DEG C of outlet temperature for 45 DEG C by inlet temperature;
(4) cooling and shaping:Using water-cooling process by the PVB film cooling and shapings of extrusion, wherein, water temperature is maintained at 21 DEG C;
(5) using winder by the PVB film rolls after sizing around, cut and wind.
Preparation method embodiment 3
A kind of preparation method of polyvinyl butyral film, it is characterised in that comprise the following steps:
(1) preparation polyvinyl butyral resin:Use recovery resin-made of the viscosity solution with hydroxy radical content for 25wt% The PVB-1 resins that viscosity is 60cp/20 DEG C are obtained, use viscosity solution to obtain viscosity with hydroxy radical content for a 15wt% resin-made For 250cp/20 DEG C of PVB-2 resins, wherein the viscosity solution is 4wt% butanol solution;
(2) batch mixing:5 parts of PVB-1 resins and 100 parts of PVB-2 resins are carried out to circulate batch mixing 2 hours;
(3) plasticizing extrusion:Squeezed by weight 1 part of plasticizer is mixed into the mixed merga pass extruder of PVB resin with 3 parts Go out, the temperature wherein inside extruder is warming up to 165 DEG C of outlet temperature for 45 DEG C by inlet temperature;
(4) cooling and shaping:Using water-cooling process by the PVB film cooling and shapings of extrusion, wherein, water temperature is maintained at 23 DEG C;
(5) using winder by the PVB film rolls after sizing around, cut and wind.
Preparation method comparative example 1
A kind of preparation method of polyvinyl butyral film, it will be replaced by the hybrid resin obtained by step 1 and step 2 It is changed to outside recovery resin, other steps or parameter are identical with the preparation method described in embodiment 1.
Preparation method comparative example 2
A kind of preparation method of polyvinyl butyral film, it will be replaced by the hybrid resin obtained by step 1 and step 2 It is changed to outside a resin, other steps or parameter are identical with the preparation method described in embodiment 1.
Preparation method comparative example 3
A kind of preparation method of polyvinyl butyral film, except the hydroxy radical content that will reclaim resin is 30%, PVB-1's Number is adjusted to the butanol concentration of 40 parts and viscosity solution and is adjusted to outside 10wt%, other steps or parameter and the institute of embodiment 1 The preparation method stated is identical.
Experimental example 1
Prepare 30 chip size identical PVB films respectively according to embodiment 1-3 and comparative example 1-3 preparation method.
According to national building material industry standard:Laminated glass-use polyvinyl butyral resin (PVB) film (JC/T2166-2013) Properties test listed by table one is carried out to above-mentioned film, test result is as shown in Table 1.
Table one:Film performance
By data shown in table one, it can be found that the items by the PVB films prepared by the preparation method of the present invention Quality is superior to the national standard of PVB films, and the performance of its properties and a PVB film is without significant difference.And use pair The multinomial performance of film obtained by ratio 1 or 3 does not meet the national standard of national PVB films, also with the property of a PVB film Can have notable difference, especially tensile strength, percussion value, moisture content and mist degree, the reduction of these performances can cause it to be made Laminated glass security and service life decay.
Experimental example 2
Preparation method according to embodiment 1,2 and comparative example 1,2 prepares 30 chip size identical PVB films respectively, and adopts 30 block size identical laminated glass are made with identical manufacture craft, identical glass and above-mentioned 30 PVB films.
According to national standard -- safety glass third portion for building:Laminated glass (GB15763.3-2009) is to above-mentioned system The laminated glass obtained carries out properties test listed by table two, and test result is as shown in Table 2.
Table two:The performance of the laminated glass containing film
By data shown in table two, it can be found that containing the PVB films prepared by the preparation method by the present invention The properties of laminated glass are with the performance containing the once laminated glass of PVB films without significant difference.And made containing comparative example 1 The multinomial performance of the laminated glass of the PVB films obtained has obvious with the multinomial performance containing the once laminated glass of PVB films Difference, especially canister shot bag impact property, radioresistance and moisture-proof, the reduction of these performances can cause laminated glass security And service life decay.
Experimental example 3
Preparation method according to embodiment 1,2 and comparative example 1,2 prepares PVB films respectively, to make the PVB films prepared Performance meet or close to JC/T2166-2013 standards, inventor is keeping adjusting roller on the premise of other preparation flows are constant Parameter is pressed, obtains the result shown in table three.
Table three:Resin Flow and roll-in parameter in prepared by film
By data shown in table three, it can be found that the preparation method of the present invention can effectively improve the mobility of PVB resin, So as to reduce roll temperature and improve roll-in speed, this, which not only reduces rolling process requirement, can also improve production efficiency, reduce Production cost.It is important to note that the roll-in speed of comparative example 3 is especially low, that is the resin film forming because comparative example 3 Bad, roll-in excessive velocities can cause PVB film faces uneven or have the flaws such as aperture.

Claims (4)

1. a kind of preparation method of polyvinyl butyral film, it is characterised in that comprise the following steps:
(1) preparation polyvinyl butyral resin:Viscosity solution is used to obtain viscosity with recovery resin-made as 50-100cp/20 DEG C PVB-1 resins, viscosity solution and a resin-made is used to obtain viscosity as 250-300cp/20 DEG C of PVB-2 resins, wherein described Viscosity solution is 3-7wt% butanol solution;
(2) batch mixing:5-15 part PVB-1 resins and 100 parts of PVB-2 resins are carried out circulating batch mixing to be made within 2 hours and mix PVB trees Fat;
(3) plasticizing extrusion:Merga pass extruder extrusion is mixed by weight 1 part of plasticizer is mixed into PVB resin with 3 parts, its Temperature inside middle extruder is warming up to 165 DEG C of outlet temperature for 45 DEG C by inlet temperature;
(4) cooling and shaping:The PVB film cooling and shapings of extrusion, wherein water temperature are maintained at 20-25 DEG C using water-cooling process;
(5) using winder by the PVB film rolls after sizing around, cut and wind;
The hydroxy radical content of the recovery resin and a resin is 19-22wt%.
2. the preparation method according to right wants 1, it is characterised in that:The viscosity solution is 5wt% butanol solution.
3. a kind of polyvinyl butyral film, it is characterised in that pass through the polyvinyl butyral film of claim 1 or 2 Preparation method obtain.
4. polyvinyl butyral film according to claim 3, it is characterised in that for manufacturing the interlayer of laminated glass.
CN201611121206.5A 2016-12-08 2016-12-08 A kind of polyvinyl butyral film and preparation method thereof Active CN106752995B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106752995B (en) * 2016-12-08 2017-12-22 忠信(清远)光伏材料科技有限公司 A kind of polyvinyl butyral film and preparation method thereof
CN112018203B (en) * 2020-09-09 2022-05-13 嘉兴福盈复合材料有限公司 Method for efficiently preparing polyvinyl butyral photovoltaic module
WO2022098237A1 (en) 2020-11-04 2022-05-12 Redeahold Apeldoorn B.V. Upgrading recycled polyvinyl butyral

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1743765A2 (en) * 2000-03-02 2007-01-17 Sekisui Chemical Co., Ltd. Interlayer film for laminated glass and laminated glass
CN101302301A (en) * 2008-07-03 2008-11-12 上海市塑料研究所 High temperature resistant polyvinyl butyral film for glass sandwich and preparation thereof
CN102585414A (en) * 2012-01-10 2012-07-18 江苏科技大学 Refractory glass sandwich layer film and preparation method thereof
CN103275449A (en) * 2013-01-22 2013-09-04 温州市奎达塑料科技有限公司 Recycled PVB film and preparation technology thereof
CN105733146A (en) * 2014-12-08 2016-07-06 池州市英派科技有限公司 Preparation method of PVB middle film for laminated glass
CN106752995A (en) * 2016-12-08 2017-05-31 忠信(清远)光伏材料科技有限公司 A kind of polyvinyl butyral film and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1743765A2 (en) * 2000-03-02 2007-01-17 Sekisui Chemical Co., Ltd. Interlayer film for laminated glass and laminated glass
CN101302301A (en) * 2008-07-03 2008-11-12 上海市塑料研究所 High temperature resistant polyvinyl butyral film for glass sandwich and preparation thereof
CN102585414A (en) * 2012-01-10 2012-07-18 江苏科技大学 Refractory glass sandwich layer film and preparation method thereof
CN103275449A (en) * 2013-01-22 2013-09-04 温州市奎达塑料科技有限公司 Recycled PVB film and preparation technology thereof
CN105733146A (en) * 2014-12-08 2016-07-06 池州市英派科技有限公司 Preparation method of PVB middle film for laminated glass
CN106752995A (en) * 2016-12-08 2017-05-31 忠信(清远)光伏材料科技有限公司 A kind of polyvinyl butyral film and preparation method thereof

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