CN106752995A - A kind of polyvinyl butyral film and preparation method thereof - Google Patents
A kind of polyvinyl butyral film and preparation method thereof Download PDFInfo
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- CN106752995A CN106752995A CN201611121206.5A CN201611121206A CN106752995A CN 106752995 A CN106752995 A CN 106752995A CN 201611121206 A CN201611121206 A CN 201611121206A CN 106752995 A CN106752995 A CN 106752995A
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- polyvinyl butyral
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
-
- 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
- B32B7/00—Layered 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
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J129/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
- C09J129/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer 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 prepares polyvinyl butyral resin, batch mixing, plasticizing extrusion, cooling and shaping and winding, cuts and wind 5 steps.After using two kinds of resin mixing technologies, the mobility of resin has greatly improved the method for the invention；When the film produced using the 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, reduce production cost；Application method produces film and can not only save a consumption for resin, reduces production cost, and also with a resin property without significant difference, the repair rate of glass laminating is improved to 95% the film performance that it is produced from general containing reclaim resin doubling 85%.
Description
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 under acid environment catalysis with butyraldehyde.PVB due to containing compared with long-chain branch, with the material such as glass, metal
Bonding force very high.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.According to these characteristics, can be by HMW
After PVB resin adds plasticizer, film is squeezed into, as the sandwich material of safety glass.When safety glass is subject to 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 to cause injury, and in the case of not influenceing sight line 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, the production of PVB 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
Ten producers of production PVB films, but the PVB films producer of most domestic is produced using reclaimed materials, using pure
The producer of PVB resin production is little.Because material is 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 the performance of this regeneration film 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 high cost, its rolling process requirement is 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 asked, 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：It is 50-100cp/20 to use viscosity solution to obtain viscosity with recovery resin-made
DEG C PVB-1 resins, use viscosity solution and a resin-made to obtain the PVB-2 resins that viscosity is for 250-300cp/20 DEG C, wherein
The viscosity solution is the butanol solution of 3-7wt%；
(2) batch mixing：5-15 parts of PVB-1 resin and 100 parts of PVB-2 resins are circulated batch mixing and are obtained for 2 hours and mixes 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, wherein the temperature 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 that will be extruded using water-cooling process, wherein water temperature is maintained at 20-25
℃；
(5) using winder by the PVB film rolls after sizing around, cut and wind.
Further, the recovery resin and a hydroxy radical content for resin are 19-22wt%.
Further, the viscosity solution is preferably the butanol solution of 5wt%.
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 is obtained.
Further, the polyvinyl butyral film can be used to manufacture the interlayer of laminated glass.
A resin of the present invention refers to the product being condensed under acid environment catalysis by direct polyvinyl alcohol and butyraldehyde,
I.e. without the resin of recycling.
The preparation method of polyvinyl butyral film of the present invention advantage compared with prior art is：
(1) using after two kinds of resin mixing technologies, the melt index of resin is carried from the 0.4-0.7g/10min of a resin
Up to 0.8-1.3g/10min, the mobility of resin has greatly improved；
(2) when the film produced using this preparation method does roll-in, roll-in speed can be improved to 1.5m/ from 1.2m/min
Min, can improve the production efficiency of glass laminating processing, reduce production cost；
(3) producing film using preparation method can not only save a consumption for resin, reduce production cost, its production
, also with a resin property without significant difference, the repair rate of glass laminating is from typically containing recovery resin doubling for the film performance for going out
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.
Specific 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 to those skilled in the art aobvious
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：It is the recovery resin-made of 22wt% to use viscosity solution and hydroxy radical content
The PVB-1 resins that viscosity is for 75cp/20 DEG C are obtained, uses viscosity solution with hydroxy radical content for a resin-made of 19wt% obtains viscosity
It is 261cp/20 DEG C of PVB-2 resins, wherein butanol solution of the viscosity solution for 5wt%；
(2) batch mixing：10 parts of PVB-1 resins and 100 parts of PVB-2 resins are circulated 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, wherein the temperature 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 that will be extruded using water-cooling process, 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：It is the recovery resin-made of 21wt% to use viscosity solution and hydroxy radical content
Viscosity is 90cp/20 DEG C of PVB-1 resins, use the viscosity solution hydroxy radical content to be for a resin-made of 20wt% obtains viscosity
285cp/20 DEG C of PVB-2 resins, wherein butanol solution of the viscosity solution for 7wt%；
(2) batch mixing：15 parts of PVB-1 resins and 100 parts of PVB-2 resins are circulated 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, wherein the temperature 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 that will be extruded using water-cooling process, 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：It is the recovery resin-made of 25wt% to use viscosity solution and hydroxy radical content
The PVB-1 resins that viscosity is for 60cp/20 DEG C are obtained, uses viscosity solution with hydroxy radical content for a resin-made of 15wt% obtains viscosity
It is 250cp/20 DEG C of PVB-2 resins, wherein butanol solution of the viscosity solution for 4wt%；
(2) batch mixing：5 parts of PVB-1 resins and 100 parts of PVB-2 resins are circulated 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, wherein the temperature 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 that will be extruded using water-cooling process, 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, 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, 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
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
Preparation method according to embodiment 1-3 and comparative example 1-3 prepares 30 chip size identical PVB films respectively.
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 by the items of the PVB films prepared by preparation method of the invention
Quality is superior to the national standard of PVB films, and its properties and a performance for PVB films are without significant difference.And using right
The multinomial performance of the film obtained by ratio 1 or 3 does not meet the national standard of national PVB films, with a property for PVB films yet
The reduction can with notable difference, especially tensile strength, percussion value, moisture content and mist degree, these performances can cause it to be obtained
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 obtained 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 for obtaining carries out properties test listed by table two, and test result is as shown in Table 2.
Table two：Performance containing film laminated glass
By data shown in table two, it can be found that containing by the PVB films prepared by preparation method of the invention
The properties of laminated glass are with the performance containing the once laminated glass of PVB films without significant difference.And contain comparative example 1 and make
The multinomial performance of the laminated glass of the PVB films for obtaining 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
Pressure parameter, obtains the result shown in table three.
Table three：Resin Flow and roll-in parameter in film preparation
By data shown in table three, it can be found that preparation method of the invention can effectively improve the mobility of PVB resin,
So as to reduce roll temperature and improve roll-in speed, this not only reduces rolling process requirement can also improve production efficiency, reduction
Production cost.It is important to note that the roll-in speed of comparative example 3 is especially low, that is because the resin film forming of comparative example 3
Bad, roll-in excessive velocities can cause PVB film faces uneven or have the flaws such as aperture.
Claims (5)
1. a kind of preparation method of polyvinyl butyral film, it is characterised in that comprise the following steps：
(1) preparation polyvinyl butyral resin：It is 50-100cp/20 DEG C to use viscosity solution to obtain viscosity with recovery resin-made
PVB-1 resins, use viscosity solution and a resin-made to obtain the PVB-2 resins that viscosity is for 250-300cp/20 DEG C, wherein described
Viscosity solution is the butanol solution of 3-7wt%；
(2) batch mixing：5-15 parts of PVB-1 resin and 100 parts of PVB-2 resins are circulated batch mixing and are obtained for 2 hours and mixes PVB trees
Fat；
(3) plasticizing extrusion：Mix the mixed merga pass extruder extrusion of PVB resin with 3 parts by weight by 1 part of plasticizer, 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 that will be extruded using water-cooling process, wherein water temperature is maintained at 20-25 DEG C；
(5) using winder by the PVB film rolls after sizing around, cut and wind.
2. preparation method according to claim 1, it is characterised in that：It is described to reclaim resin and a hydroxy radical content for resin
It is 19-22wt%.
3. the preparation method according to right wants 1, it is characterised in that：The viscosity solution is the butanol solution of 5wt%.
4. a kind of polyvinyl butyral film, it is characterised in that by any polyvinyl butyral resins of claim 1-4
The preparation method of film is obtained.
5. polyvinyl butyral film according to claim 4, it is characterised in that the interlayer for manufacturing laminated glass.
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| CN201611121206.5A CN106752995B (en) | 2016-12-08 | 2016-12-08 | A kind of polyvinyl butyral film and preparation method thereof |
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| CN201611121206.5A CN106752995B (en) | 2016-12-08 | 2016-12-08 | A kind of polyvinyl butyral film and preparation method thereof |
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Cited By (3)
| 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 |
| CN112018203A (en) * | 2020-09-09 | 2020-12-01 | 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 |
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| 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 |
Family Cites Families (1)
| 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 |
-
2016
- 2016-12-08 CN CN201611121206.5A patent/CN106752995B/en active Active
Patent Citations (5)
| 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 |
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Cited By (5)
| 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 |
| CN112018203A (en) * | 2020-09-09 | 2020-12-01 | 嘉兴福盈复合材料有限公司 | Method for efficiently preparing polyvinyl butyral photovoltaic module |
| 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 |
| EP4240791A1 (en) * | 2020-11-04 | 2023-09-13 | Dakip B.V. | Upgrading recycled polyvinyl butyral |
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| CN106752995B (en) | 2017-12-22 |
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