CN105400110A - Preparation method of polyvinyl butyral (PVB) film with improved adhesion stress - Google Patents
Preparation method of polyvinyl butyral (PVB) film with improved adhesion stress Download PDFInfo
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- CN105400110A CN105400110A CN201510959533.7A CN201510959533A CN105400110A CN 105400110 A CN105400110 A CN 105400110A CN 201510959533 A CN201510959533 A CN 201510959533A CN 105400110 A CN105400110 A CN 105400110A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions 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; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/14—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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/204—Applications use in electrical or conductive gadgets use in solar cells
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Abstract
The invention belongs to the technical field of thermoplastic high-molecular material, and more specifically relates to a preparation method and applications of polyvinyl butyral (PVB) film with improved adhesion stress. According to the invention, PVB resin, a plasticizer mixture, and an aqueous solution of a potassium salt and a magnesium salt are delivered into an extruder for extrusion, stretching, sizing, trimming, and coiling so as to obtain the PVB film. In the preparation method, the potassium salt and the magnesium salt which are capable of adjusting film adhesion stress are added so that the obtained PVB film possesses adhesion stress of about three grade when water content is controlled to be 1.0%, and at the same time a certain amount of silicone oil is added so as to avoid the decrease of safety performance of safety glass caused by film drawing.
Description
Technical field
The invention belongs to thermoplastic macromolecule material technical field, be specifically related to a kind of polyvinyl butyral acetal (PVB) the film preparation method and the application thereof that improve cohesive force.
Background technology
PVB film also known as PVB film, due to have transparent, fast light, heat-resisting, soft, low temperature is non-sclerous, and and the excellent properties such as glass and metal good bonding and be applied to shatter proof glass, when being particularly subject to great impact, do not cause glass fragment outwards to disperse.Just pvb film is used for the windshield of car as far back as some developed countries of 1820s (beautiful, moral), thus substantially increases the safety coefficient of transportation industry.Up to the present, the application of shatter proof glass is quite extensive, except car, also generally adopts in fields such as aircraft manufacturing, subway door and window, bank counter, building trade, solar cell films.
Because the complete processing of pvb film is complicated, add the external blockade to PVB film production technology, only have several the International FDIs such as the U.S., Japan, Germany to have this technology at present in the world.And the researchdevelopment starting of domestic PVB is comparatively slow, film can't meet the requirement of client in some performance, and especially domestic film is large with the impact of film water ratio on the cohesive force of glass, easily causes shatter proof glass to come unstuck after film water suction.Therefore most domestic PVB film market still by the U.S. and Japan major part capture.An application number is the patent of invention of CN201110052776, disclose a kind of formula preparing high strength PVB sheet material, by adding high boiling solvent lignin amine as bonding strength conditioning agent, not only achieve and utilize the high efficiente callback of PVB film edge corner material regenerative ratio PVB sheet material to utilize, reasonably regulate again the adhesiveproperties between PVB film and unorganic glass; An application number is the patent of invention of 200810050100X, discloses a kind of PVB film for laminated glass, this film by the polyvinyl butyral acetal of 74-85 weight part, the low polarity plasticizer of 14-25 weight part and the silane coupling agent of 0.2-1.0 weight part.The PVB film for laminated glass of the program meets requirement to different cohesive strength by adjusting the add-on of coupling agent.
Aforementioned patents disclose and improve PVB film cohesive strength by adding high boiling solvent lignin amine as bonding strength conditioning agent, silane coupling agent.And the present inventor is by long-term theory and experimental studies have found that, film face moisture is one of important factor affecting film bonding strength, especially when film water ratio is high, film easily comes unstuck, the present invention breaks through tradition, by adding the sylvite and magnesium salts that regulate film cohesive force, guarantees that film cohesive force under the condition of different in moisture can both reach requirement, film can be made not come unstuck, after synthetic glass, meet the mechanical property of shatter proof glass simultaneously.
Summary of the invention
One object of the present invention is to improve film face moisture affects performance to cohesive force, guarantee that film cohesive force under the condition of different in moisture can both reach requirement, film can be made not come unstuck, meet the mechanical property of shatter proof glass simultaneously after synthetic glass, improve the market competitiveness of domestic PVB film.
Another object of the present invention is to prepare in PVB film technique and keeps film to still have the cohesive force of about 3 grades when 1.0% water ratio by adding the sylvite that regulates film cohesive force and magnesium salts, also adds a certain amount of silicone oil minimizing film simultaneously and causes the safety performance of shatter proof glass to decline at membrane technology.
In order to reach foregoing invention object, the present invention by the following technical solutions:
Improve polyvinyl butyral acetal (PVB) film preparation method for cohesive force, particular content is as follows:
The preparation of sylvite and magnesium salt solution: add a certain proportion of sylvite and magnesium salts in pure water, is configured to the aqueous solution containing sylvite and magnesium salts; Described sylvite and magnesium salts miscible in pure water according to the ratio of 1:3 ~ 1:1, solvent temperature 70 DEG C.
The preparation of softening agent fluid mix: uv-absorbing agent, oxidation inhibitor, chainextender, silane coupling agent, silicone oil, white dyes are added in softening agent be warming up to 60 DEG C allow it fully dissolve after be cooled to 40 DEG C to make softening agent fluid mix stand-by, the weight percent of various material is: UV light absorber 1.4-1.5%, oxidation inhibitor 0.32-0.35%, chainextender 0.60-0.70%, silane coupling agent 2.0-3.0%, silicone oil 0.1-0.2%, white dyes 0.13-0.14%, surplus are softening agent %, wherein, fluid mix meter 100 % by weight.Wherein UV light absorber is UVP-327; Oxidation inhibitor is antioxidant 1076; Chainextender is Tetra hydro Phthalic anhydride; Silane coupling agent is methacryloxypropyl trimethoxy silane; Silicone oil is methyl-silicone oil; White dyes is fluorescent whitening agent OB; Softening agent is triglycol two 2-ethylhexoate.
The preparation of film: PVB resin and softening agent fluid mix are sent into forcing machine according to the ratio of weight part 100: 20-35, preferred 100:30, add sylvite and the magnesium salt solution of certain part by weight simultaneously, through heating, mixing, mixing, compression, filter, extruder temperature be 150-165 DEG C, die head temperature extrudes film under being the condition of 145 DEG C, draw speed controls film stock thickness, is shaped by film in cold rinse bank, then trimming, rolling can obtain film.
Further, sylvite and magnesium salts are that 150 ~ 550ppm adds in film according to total addition level, and the addition of silicone oil is 100 ~ 400ppm.
Further, one or both of potassium formiate, potassium acetate selected by sylvite; Magnesium acetate selected by magnesium salts.
Further, select hydroxy radical content be 18 ~ 22% PVB resin.
Further, extruder temperature preferably 155 DEG C.
Further, described film stock thickness is 0.60-0.80mm.
Another object of the present invention is to provide the PVB obtained by above-mentioned preparation method film.
Another object of the present invention is the encapsulation for solar cell of the PVB film that obtained by above-mentioned preparation method.
The technique effect that the present invention is useful is: by adding Tetra hydro Phthalic anhydride chainextender, realize the lifting of PVB film mechanical property; By adding the silicone oil of certain consumption, sylvite and magnesium salts, reducing the impact that film causes the safety performance of shatter proof glass to decline at membrane technology, and keeping film to still have the cohesive force of about 3 grades when 1.0% water ratio, minimizing shatter proof glass comes unstuck situation.
Embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1
Improve polyvinyl butyral acetal (PVB) film preparation method for cohesive force, particular content is as follows:
The preparation of sylvite and magnesium salt solution: add a certain proportion of potassium formiate and magnesium acetate in pure water, is configured to the aqueous solution containing sylvite and magnesium salts; Described sylvite and magnesium salts miscible in pure water according to the ratio of 1:2, solvent temperature 70 DEG C, described concentration of aqueous solution is 2%.
The preparation of softening agent fluid mix: uv-absorbing agent, oxidation inhibitor, chainextender, silane coupling agent, silicone oil, white dyes are added in softening agent be warming up to 60 DEG C allow it fully dissolve after be cooled to 40 DEG C to make softening agent fluid mix stand-by, the weight percent of various material is: UV light absorber 1.45%, oxidation inhibitor 0.33%, chainextender 0.65%, silane coupling agent 2.5%, silicone oil 0.15%, white dyes 0.135%, surplus are softening agent %, wherein, fluid mix meter 100 % by weight.Wherein UV light absorber is UVP-327; Oxidation inhibitor is antioxidant 1076; Chainextender is Tetra hydro Phthalic anhydride; Silane coupling agent is methacryloxypropyl trimethoxy silane; Silicone oil is methyl-silicone oil; White dyes is fluorescent whitening agent OB; Softening agent is triglycol two 2-ethylhexoate.
The preparation of film: by 100 weight part hydroxyl values be 20% PVB resin and 30 parts by weight of plasticizer fluid mix send into forcing machine, add sylvite and the magnesium salt solution of 2.0 weight parts simultaneously, through heating, mixing, mixing, compression, filter, extruder temperature be 155 DEG C, die head temperature extrudes film under being the condition of 145 DEG C, draw speed controls film stock thickness, is shaped by film in cold rinse bank, then trimming, rolling can obtain film, and thickness is 0.76mm.
Embodiment 2
Improve polyvinyl butyral acetal (PVB) film preparation method for cohesive force, particular content is as follows:
The preparation of sylvite and magnesium salt solution: add a certain proportion of potassium acetate and magnesium acetate in pure water, is configured to the aqueous solution containing sylvite and magnesium salts; Described sylvite and magnesium salts miscible in pure water according to the ratio of 1:2, solvent temperature 70 DEG C, described concentration of aqueous solution is 2%.
The preparation of softening agent fluid mix: uv-absorbing agent, oxidation inhibitor, chainextender, silane coupling agent, silicone oil, white dyes are added in softening agent be warming up to 60 DEG C allow it fully dissolve after be cooled to 40 DEG C to make softening agent fluid mix stand-by, the weight percent of various material is: UV light absorber 1.45%, oxidation inhibitor 0.33%, chainextender 0.65%, silane coupling agent 2.5%, silicone oil 0.15%, white dyes 0.135%, surplus are softening agent %, wherein, fluid mix meter 100 % by weight.Wherein UV light absorber is UVP-327; Oxidation inhibitor is antioxidant 1076; Chainextender is Tetra hydro Phthalic anhydride; Silane coupling agent is methacryloxypropyl trimethoxy silane; Silicone oil is methyl-silicone oil; White dyes is fluorescent whitening agent OB; Softening agent is triglycol two 2-ethylhexoate.
The preparation of film: by 100 weight part hydroxyl values be 20% PVB resin and 35 parts by weight of plasticizer fluid mix send into forcing machine, add sylvite and the magnesium salt solution of 2.5 weight parts simultaneously, through heating, mixing, mixing, compression, filter, extruder temperature be 155 DEG C, die head temperature extrudes film under being the condition of 145 DEG C, draw speed controls film stock thickness, is shaped by film in cold rinse bank, then trimming, rolling can obtain film, and thickness is 0.76mm.
Comparative example 1
The preparation of softening agent fluid mix: uv-absorbing agent, oxidation inhibitor, chainextender, silane coupling agent, silicone oil, white dyes are added in softening agent be warming up to 60 DEG C allow it fully dissolve after be cooled to 40 DEG C to make softening agent fluid mix stand-by, the weight percent of various material is: UV light absorber 1.45%, oxidation inhibitor 0.33%, chainextender 0.65%, silane coupling agent 2.5%, silicone oil 0.15%, white dyes 0.135%, surplus are softening agent %, wherein, fluid mix meter 100 % by weight.Wherein UV light absorber is UVP-327; Oxidation inhibitor is antioxidant 1076; Chainextender is Tetra hydro Phthalic anhydride; Silane coupling agent is methacryloxypropyl trimethoxy silane; Silicone oil is methyl-silicone oil; White dyes is fluorescent whitening agent OB; Softening agent is triglycol two 2-ethylhexoate.
The preparation of film: by 100 weight part hydroxyl values be 20% PVB resin and 30 parts by weight of plasticizer fluid mix send into forcing machine, through heating, mixing, mixing, compression, filter, extruder temperature be 155 DEG C, die head temperature extrudes film under being the condition of 145 DEG C, draw speed controls film stock thickness, in cold rinse bank, film is shaped, then trimming, rolling can obtain film, and thickness is 0.76mm.
The properties index obtaining PVB film according to above-mentioned technique is as shown in the table:
| Project | Embodiment 1 | Embodiment 2 | Comparative example 1 |
| Thickness (mm) | 0.76 | 0.76 | 0.76 |
| Mist degree (%) | 0.5 | 0.5 | 0.3 |
| Tensile strength (Mpa) | 25.3 | 25.0 | 24.6 |
| Elongation at break (%) | 210 | 219 | 215 |
| Water ratio (%) | 1.0 | 1.0 | 1.0 |
| Cohesive force | 3 grades | 3 grades | Come unstuck |
Claims (7)
1. improve polyvinyl butyral acetal (PVB) film preparation method for cohesive force, it is characterized in that:
The preparation of sylvite and magnesium salt solution: add a certain proportion of sylvite and magnesium salts in pure water, is configured to the aqueous solution containing sylvite and magnesium salts; Described sylvite and magnesium salts miscible in pure water according to the ratio of 1:3 ~ 1:1, solvent temperature 70 DEG C.
The preparation of softening agent fluid mix: uv-absorbing agent, oxidation inhibitor, chainextender, silane coupling agent, silicone oil, white dyes are added in softening agent be warming up to 60 DEG C allow it fully dissolve after be cooled to 40 DEG C to make softening agent fluid mix stand-by, the weight percent of various material is: UV light absorber 1.4-1.5%, oxidation inhibitor 0.32-0.35%, chainextender 0.60-0.70%, silane coupling agent 2.0-3.0%, silicone oil 0.1-0.2%, white dyes 0.13-0.14%, surplus are softening agent %, wherein, fluid mix meter 100 % by weight.Wherein UV light absorber is UVP-327; Oxidation inhibitor is antioxidant 1076; Chainextender is Tetra hydro Phthalic anhydride; Silane coupling agent is methacryloxypropyl trimethoxy silane; Silicone oil is methyl-silicone oil; White dyes is fluorescent whitening agent OB; Softening agent is triglycol two 2-ethylhexoate.
The preparation of film: PVB resin and softening agent fluid mix are sent into forcing machine according to the ratio of weight part 100: 20-35, preferred 100:30, add sylvite and the magnesium salt solution of certain part by weight simultaneously, through heating, mixing, mixing, compression, filter, extruder temperature be 150-165 DEG C, die head temperature extrudes film under being the condition of 145 DEG C, draw speed controls film stock thickness, is shaped by film in cold rinse bank, then trimming, rolling can obtain film.Wherein, sylvite and magnesium salts are that 150 ~ 550ppm adds in film according to total addition level, and the addition of silicone oil is 100 ~ 400ppm.
2. a kind of polyvinyl butyral acetal (PVB) film preparation method improving cohesive force as claimed in claim 1, is characterized in that: sylvite select potassium formiate, potassium acetate one or both; Magnesium acetate selected by magnesium salts.
3. a kind of polyvinyl butyral acetal (PVB) film preparation method improving cohesive force as claimed in claim 1, is characterized in that: select hydroxy radical content be 18 ~ 22% PVB resin.
4. a kind of polyvinyl butyral acetal (PVB) film preparation method improving cohesive force as claimed in claim 1, is characterized in that: extruder temperature preferably 155 DEG C.
5. a kind of polyvinyl butyral acetal (PVB) film preparation method improving cohesive force as claimed in claim 1, is characterized in that: described film stock thickness is 0.60-0.80mm.
6. a PVB film, is characterized in that being obtained by the preparation method of the claims 1-5 arbitrary described polyvinyl butyral acetal (PVB) film.
7. claim 1-6 arbitrary described polyvinyl butyral acetal (PVB) film is used for the encapsulation of solar cell.
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| CN201510959533.7A CN105400110A (en) | 2015-12-21 | 2015-12-21 | Preparation method of polyvinyl butyral (PVB) film with improved adhesion stress |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106079751A (en) * | 2016-08-04 | 2016-11-09 | 浙江飞越洁具制造有限公司 | A kind of antifog glass |
| CN107298947A (en) * | 2017-08-09 | 2017-10-27 | 山东方鼎安全玻璃科技有限公司 | A kind of SGP films and preparation method thereof |
| CN111347748A (en) * | 2020-03-23 | 2020-06-30 | 苏州奥罗丹新材料有限公司 | Optical film material with heat storage function |
| CN111944173A (en) * | 2020-08-24 | 2020-11-17 | 安徽皖维皕盛新材料有限责任公司 | Method for improving dispersity of PVB film viscosity regulator |
| CN114058144A (en) * | 2020-07-30 | 2022-02-18 | 张安雄 | Polyvinyl butyral modified material and preparation method and application thereof |
| CN114867786A (en) * | 2020-03-26 | 2022-08-05 | 积水化学工业株式会社 | Polyvinyl acetal resin composition and adhesive |
| CN115746752A (en) * | 2022-12-13 | 2023-03-07 | 长春工业大学 | Polyvinyl butyral sound insulation film and preparation method thereof |
| US11639437B2 (en) | 2020-09-14 | 2023-05-02 | An-Hsiung Chang | Modified polyvinyl butyral material, and preparation and applications thereof |
| CN116875225A (en) * | 2023-07-04 | 2023-10-13 | 奎达高分子材料科技(宜兴)有限公司 | PVB adhesive film with excellent adhesive property and preparation method thereof |
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| US20050256258A1 (en) * | 2001-10-11 | 2005-11-17 | Uwe Keller | PVB Film for Composite Safety Glass and Composite Safety Glass |
| CN101519502A (en) * | 2008-02-29 | 2009-09-02 | 住友化学株式会社 | Method for manufacturing polarizing film, polarizing sheet and optical laminate |
| CN102675788A (en) * | 2012-05-03 | 2012-09-19 | 浙江圣瑞塑胶有限公司 | Processing aid for photovoltaic-grade polyvinyl butyral |
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| US20050256258A1 (en) * | 2001-10-11 | 2005-11-17 | Uwe Keller | PVB Film for Composite Safety Glass and Composite Safety Glass |
| CN101519502A (en) * | 2008-02-29 | 2009-09-02 | 住友化学株式会社 | Method for manufacturing polarizing film, polarizing sheet and optical laminate |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106079751A (en) * | 2016-08-04 | 2016-11-09 | 浙江飞越洁具制造有限公司 | A kind of antifog glass |
| CN107298947A (en) * | 2017-08-09 | 2017-10-27 | 山东方鼎安全玻璃科技有限公司 | A kind of SGP films and preparation method thereof |
| CN111347748A (en) * | 2020-03-23 | 2020-06-30 | 苏州奥罗丹新材料有限公司 | Optical film material with heat storage function |
| CN114867786A (en) * | 2020-03-26 | 2022-08-05 | 积水化学工业株式会社 | Polyvinyl acetal resin composition and adhesive |
| CN114867786B (en) * | 2020-03-26 | 2024-05-03 | 积水化学工业株式会社 | Polyvinyl acetal resin composition and adhesive |
| CN114058144A (en) * | 2020-07-30 | 2022-02-18 | 张安雄 | Polyvinyl butyral modified material and preparation method and application thereof |
| CN111944173A (en) * | 2020-08-24 | 2020-11-17 | 安徽皖维皕盛新材料有限责任公司 | Method for improving dispersity of PVB film viscosity regulator |
| US11639437B2 (en) | 2020-09-14 | 2023-05-02 | An-Hsiung Chang | Modified polyvinyl butyral material, and preparation and applications thereof |
| US11732122B2 (en) | 2020-09-14 | 2023-08-22 | An-Hsiung Chang | Modified polyvinyl butyral material, and preparation and applications thereof |
| CN115746752A (en) * | 2022-12-13 | 2023-03-07 | 长春工业大学 | Polyvinyl butyral sound insulation film and preparation method thereof |
| CN116875225A (en) * | 2023-07-04 | 2023-10-13 | 奎达高分子材料科技(宜兴)有限公司 | PVB adhesive film with excellent adhesive property and preparation method thereof |
| CN116875225B (en) * | 2023-07-04 | 2024-06-14 | 奎达高分子材料科技(宜兴)有限公司 | PVB adhesive film with excellent adhesive property and preparation method thereof |
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