CN106398071A - Manufacturing method of polyvinyl butyral film - Google Patents
Manufacturing method of polyvinyl butyral film Download PDFInfo
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- CN106398071A CN106398071A CN201610911267.5A CN201610911267A CN106398071A CN 106398071 A CN106398071 A CN 106398071A CN 201610911267 A CN201610911267 A CN 201610911267A CN 106398071 A CN106398071 A CN 106398071A
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- polyvinyl butyral
- condensation
- manufacture method
- butyral resin
- reaction
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/37—Thiols
- C08K5/372—Sulfides, e.g. R-(S)x-R'
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/28—Condensation with aldehydes or ketones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Joining Of Glass To Other Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a manufacturing method of a polyvinyl butyral film. The manufacturing method is characterized by comprising the following steps: pretreating polyvinyl alcohol and n-butanal raw materials to reduce impurities in the raw materials; then performing a condensation reaction, and performing washing and solvent soaking on generated polyvinyl butyral resin after the reaction to remove side reactions generated by the condensation reaction and residual impurities; and finally, performing heating melt plasticization and tape casting on the dried polyvinyl butyral resin together with a plasticizer, an antioxidant and an auxiliary agent in an extruding machine, thereby obtaining the polyvinyl butyral film. According to the manufacturing method disclosed by the invention, by reducing the impurities in the raw materials, the polyvinyl butyral resin with relatively high transparency is obtained, and by adding the antioxidant and the auxiliary agent, the polyvinyl butyral film can avoid aging discoloration in processing and using processes.
Description
Technical field
The present invention relates to a kind of manufacture method of polyvinyl butyral film.
Background technology
Polyvinyl butyral resin (PVB) film is a kind of plasticizing thin film with PVB resin as substrate, and PVB resin is by gathering
Vinyl alcohol and hutanal carry out the product of condensation reaction, have good light resistance, tolerance to cold, resistance to water, the transparency, anti-
Impact and film property, and nontoxic, odorless, corrosion-free performance, have good to timber, pottery, metal, leather and glass etc.
Adhesive property, its application is widely.
PVB film is a kind of macromolecular material by PVB resin through plasticizer extrusion molding, is translucent diaphragm, has
Cold-resistant, heat-resisting, transparent, characteristic, surfacing, the free from admixture such as mechanical strength is high, has certain roughness and good flexibility
Can, unorganic glass is had with good cohesive force, is widely used in the product manufacturing in the fields such as safety glass, photovoltaic industry, especially
It makes PVB film have and develops faster in the use of safety glass.
Current high-grade in the world PVB film, only several transnational enterprises such as the U.S., Germany, Japan have this skill
Art, China is slow in PVB film field development speed, and the quality level of product is not high, now with building industry, automobile industry,
The development of photovoltaic industry, increasing to high-end PVB film demand, to its prescription also more and more higher, domestic enterprise gives birth to
The film producing can not meet it and use standard, rely primarily on import at present.One major influence factors of PVB film are exactly PVB
The discoloration problem of film, in the production process of PVB film, the degraded of PVB resin, oxidation, autohemagglutination, impurities left, processing work
Skill is all to cause the factor of PVB film variable color, and this problem governs the development of PVB film.
Content of the invention
The present invention is intended to provide a kind of manufacture method of polyvinyl butyral film, manufactured with solving PVB film
Produced problem in journey, improves the white quality of PVB film product.
The present invention solves technical problem, adopts the following technical scheme that：
A kind of manufacture method of polyvinyl butyral film, its feature is to carry out as follows：
(1) polyvinyl alcohol is used deionized water wash, being then configured to mass concentration with deionized water is 12 ± 2%
Poly-vinyl alcohol solution, being heated to 100 ± 10 DEG C makes it be completely dissolved, and pressure filtration obtains poly-vinyl alcohol solution；Hutanal is entered
Row vacuum distillation remove impurity, the hutanal obtaining pretreatment is stand-by with inert gas seal；
(2) with poly-vinyl alcohol solution and hutanal as raw material, under inert gas shielding, condensation is carried out by catalyst anti-
Should, reaction is washed after terminating and is dried to obtain polyvinyl butyral resin；
(3) polyvinyl butyral resin is mixed homogeneously with plasticizer, antioxidant, auxiliary agent, gained mixture by plus
Material system uniformly feeds extruder, becomes molten condition by the plasticizing of extruder homogeneous heating, is flowed out by die lip after filtering, cold
But shape, be shaped to polyvinyl butyral film.
The average degree of polymerization of described polyvinyl alcohol is 400-5000, alcoholysis degree >=99.5%, degree of polymerization distribution are 1-5.
Described noble gases are helium, neon, argon, Krypton or nitrogen.
Described catalyst can be inorganic for hydrochloric acid, sulphuric acid, formic acid, acetic acid, trimethyl formic acid, para-methylbenzenepyridinsulfonate sulfonate etc.
Acid, organic acid or Barbiturates catalyst, can be a kind of acid catalyst or two or more combination.
Condensation reaction described in step (2) adopts two step condensations, is followed successively by low temperature condensation and insulation strengthening condensation；Described low
Temperature condensation be by poly-vinyl alcohol solution send into condensation kettle in, when condensation kettle temperature be 0 DEG C when, add 40%-60% butyraldehyde and
Catalyst, insulation reaction 0.5 hour, add remaining hutanal, then in 2-4 hour, be uniformly heating to 20-45 DEG C, continue
Isothermal reaction 2-4h；Described insulation strengthening condensation is will to deliver to strengthening kettle through the resin that low temperature condensation separates out, and strengthening kettle is from initial
40 DEG C are warming up to 80 DEG C, and heating rate is 5 DEG C/20min, then will strengthen kettle thermostatic at 80 DEG C, and strengthening condensation reaction is total
3 hours time, after question response reaches terminal, add alkali liquor terminating reaction, and then improve the acetal of polyvinyl butyral resin
Degree.
Washing described in step (2) is first to wash condensation reaction gained polyvinyl butyral resin product to neutrality, then
(methyloxetane is 1 with the mass ratio of water to soak the aqueous solution containing methyloxetane:3-7 hour in 10-20), finally
It is washed with deionized 3-5 time again；Because soak has preferable permeability and the microsolubility to resin, can preferably go
Except surface and the inside impurity of PVB resin is so that the PVB resin purity producing is higher.
Drying described in step (2) is 5-40min to be dried at 80-110 DEG C, can for vacuum drying, hot-air flow be dried,
Infrared drying.
Transparency >=95.5% in wavelength 490nm for step (2) the gained polyvinyl butyral resin, in wavelength
Transparency >=98.5% during 660nm.
Plasticizer described in step (3) is 2,2'-ethylenedioxybis(ethanol). two tricaprylate, the new ester of phthalic acid two or tricresyl phosphate,
The addition of described plasticizer is the 0.2-0.8% of polyvinyl butyral resin quality；Antioxidant described in step (3) is
Antioxidant DLTP, the addition of described antioxidant is the 0.05-0.5% of polyvinyl butyral resin quality；Step (3)
Described auxiliary agent is sodium soap, sodium alkyl sulfonate, sodium alklyarylsulfonate anionic auxiliary, or is ethylene oxide nonionic
Type auxiliary agent；The addition of described auxiliary agent is the 0.02-0.08% of polyvinyl butyral resin quality.
In step (3), extruder melt temperature scope is at 110-130 DEG C.
Yellow colour index≤5 in thickness 0.76mm for the gained polyvinyl butyral film of the present invention, light transmittance >=90%,
Mist degree≤0.5%.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1st, the present invention carries out technological improvement from the raw material process of PVB film, by refined, washing to PVB raw material, reduces
Impurity in PVB resin, improves the transparency of PVB resin, makes PVB resin color more pure white.
2nd, in the present invention, in the process for making of PVB film, add antioxidant, so that PVB film in processing and is used
During, it is to avoid the appearance of catabiosis, effectively prevent the outward appearance of PVB film from producing metachromatism, and then improve the pure of product
White effect.
Specific embodiment
Embodiment 1
The present embodiment prepares polyvinyl butyral resin as follows：
(1) dissolving of polyvinyl alcohol
By the degree of polymerization be 1700, alcoholysis degree 99.8%, molecular weight distribution be that 2.5 polyvinyl alcohol uses deionized water wash
3 times, then it is configured to the poly-vinyl alcohol solution that mass concentration is 24% with deionized water, after being heated to 80 DEG C of insulations 1 hour, then
Being warming up to 100 DEG C makes it be completely dissolved, and then to 12%, pressure filtration obtains poly-vinyl alcohol solution to dilute concentration.
(2) pretreatment of hutanal
Hutanal is carried out vacuum distillation remove impurity, obtain pretreatment hutanal carried out with nitrogen sealing stand-by.
(3) PVB resin synthesis
With the 400g poly-vinyl alcohol solution after process and 240g hutanal as raw material, the nitre being 35% with 60g mass concentration
Acid is catalyst, under nitrogen protection, carries out condensation reaction, the mass ratio of each raw material is polyvinyl alcohol：Hutanal：Nitric acid=
10：6：1).Specific as follows：
Low temperature is condensed：Poly-vinyl alcohol solution is sent in condensation kettle, when condensation kettle temperature is 0 DEG C, adds 50% fourth
Aldehyde and catalyst, insulation reaction 0.5 hour, add remaining hutanal, be then uniformly heating to 35 DEG C in 3 hours, continue
Isothermal reaction 3h；
Insulation strengthening condensation：Strengthening kettle will be delivered to through the resin that low temperature condensation separates out, strengthening kettle is warming up to from initial 40 DEG C
80 DEG C, heating rate is 5 DEG C/20min, then will strengthen kettle thermostatic at 80 DEG C, strengthens 3 hours condensation reaction total times,
After question response reaches terminal, add alkali liquor terminating reaction, and then improve the acetalizing degree of polyvinyl butyral resin.
(4) PVB resin post processing
The polyvinyl butyral resin obtaining through condensation reaction is washed to neutrality, is then immersed in containing methyl epoxy
(mass ratio is methyloxetane to the aqueous solution of propane：Water=1:10) 5 hours in, finally it is washed with deionized 4 times again, so
Afterwards by the PVB resin after washing, high grade of transparency PVB resin is filtered out by gas solid separation, be re-fed into 100 DEG C of hot-air flow formulas and do
Dry oven drying 20min, is obtained pure PVB resin.
Other conditions are constant, the mass ratio of adjustment methyloxetane and water, obtain PVB resin by above-mentioned identical method
Product；
Other conditions are constant, and methyloxetane is changed to methyl oxirane, obtain PVB tree by above-mentioned identical method
Fat product；
Other conditions are constant, the condensation reaction of step (3) is changed to a step condensation, only carries out low temperature condensation, do not carry out
Insulation strengthening condensation, obtains PVB resin product.
Under the conditions of each, the performance of gained PVB resin is as shown in table 1.
The performance of gained PVB resin under the conditions of table 1 is each
As can be seen from Table 1, under condensation step the same terms, methyloxetane and water ratio are 1:During 10-20,
PVB resin loss rate is relatively low, and PVB resin transparency is also preferable, when methyloxetane and water ratio are less than 1:When 10 although
PVB resin transparency is higher, can meet product quality and require, but the loss rate of PVB resin is larger, yield reduction, produce larger
Waste, affect economic benefit, when ratio is more than 1:When 20, the transmittance of PVB resin is unsatisfactory for product index and requires.In condensation step
Under rapid the same terms, soak methyloxetane is close to resin loss rate compared with soak methyl oxirane, but soak
Methyloxetane is preferable to resin transparent degree.Compared with soak under liquid proportional the same terms, two step condensations are condensed with a step,
PVB resin loss rate is close, but two step condensations are compared with a step condensation on the impact of resin transparent degree more preferably.
Embodiment 2
By corresponding PVB resin 400g of product 1 in embodiment 1 and plasticizer 2,2'-ethylenedioxybis(ethanol). two tricaprylate 2g, antioxidant
DLTP 0.8g, auxiliary agent dodecyl aryl sulfonic acid sodium 0.2g, mix homogeneously, gained mixed liquor is uniformly fed by charging system and squeezes
Go out machine, by extruder be heated to 120 DEG C homogenous plasticized become molten condition, flowed out by die lip after filtering, cooling and shaping, become
Type is the PVB film of 0.76mm.
Other conditions are constant, the quality of change plasticizer, antioxidant and auxiliary agent, or change heating-up temperature, by above-mentioned phase
Same method manufactures PVB film.
Under the conditions of each, the performance of gained PVB film is as shown in table 2.
The performance of gained PVB film under the conditions of table 2 is each
See from table 2 to draw, the ultrawhite PVB film being obtained by the present invention is in plasticizer loading 0.2-0.8%, antioxygen
When agent content 0.05-0.5%, auxiliary agent content 0.02-0.08% and 110-130 DEG C of extruder temperature, effect is optimum.
Claims (10)
1. a kind of manufacture method of polyvinyl butyral film is it is characterised in that carry out as follows：
(1) polyvinyl alcohol is used deionized water wash, be then configured to the poly- second that mass concentration is 12 ± 2% with deionized water
Enolate solution, being heated to 100 ± 10 DEG C makes it be completely dissolved, and pressure filtration obtains poly-vinyl alcohol solution；Hutanal is subtracted
Pressure distillation remove impurity, the hutanal obtaining pretreatment is stand-by with inert gas seal；
(2) with poly-vinyl alcohol solution and hutanal as raw material, under inert gas shielding, condensation reaction is carried out by catalyst,
Reaction is washed after terminating and is dried to obtain polyvinyl butyral resin；
(3) polyvinyl butyral resin is mixed homogeneously with plasticizer, antioxidant, auxiliary agent, gained mixture by feeding is
System uniformly feeds extruder, becomes molten condition by the plasticizing of extruder homogeneous heating, is flowed out by die lip after filtering, cooling is fixed
Type, is shaped to polyvinyl butyral film.
2. manufacture method according to claim 1 it is characterised in that：The average degree of polymerization of described polyvinyl alcohol is 400-
5000th, alcoholysis degree >=99.5%, degree of polymerization distribution are 1-5.
3. manufacture method according to claim 1 it is characterised in that：Described noble gases are helium, neon, argon, krypton
Gas or nitrogen.
4. manufacture method according to claim 1 it is characterised in that：The described catalyst of step (2) is hydrochloric acid, sulphuric acid, first
At least one in acid, acetic acid, trimethyl formic acid or para-methylbenzenepyridinsulfonate sulfonate.
5. the manufacture method according to claim 1 it is characterised in that：Condensation reaction described in step (2) adopts two steps
Condensation, is followed successively by low temperature condensation and insulation strengthening condensation；
Described low temperature condensation is to send into poly-vinyl alcohol solution in condensation kettle, when condensation kettle temperature is 0 DEG C, adds 40%-
60% butyraldehyde and catalyst, insulation reaction 0.5 hour, add remaining hutanal, be then uniformly heating in 2-4 hour
20-45 DEG C, continue isothermal reaction 2-4h；
Described insulation strengthening condensation is will to deliver to strengthening kettle through the resin that low temperature condensation separates out, and strengthening kettle is warming up to from initial 40 DEG C
80 DEG C, heating rate is 5 DEG C/20min, then will strengthen kettle thermostatic at 80 DEG C, strengthens 3 hours condensation reaction total times,
After question response reaches terminal, add alkali liquor terminating reaction, and then improve the acetalizing degree of polyvinyl butyral resin.
6. manufacture method according to claim 1 it is characterised in that：Washing described in step (2) is first by condensation reaction
Gained polyvinyl butyral resin product washs to neutrality, is then immersed in by methyloxetane and water in mass ratio 1:10-20
3-7 hour in the mixed liquor constituting, is finally washed with deionized again；
Drying described in step (2) is 5-40min to be dried at 80-110 DEG C.
7. the manufacture method according to claim 1 it is characterised in that：Step (2) gained polyvinyl butyral resin
Transparency >=98.5% in wavelength 660nm.
8. the manufacture method according to claim 1 it is characterised in that：Plasticizer described in step (3) is 2,2'-ethylenedioxybis(ethanol). two
Tricaprylate, the new ester of phthalic acid two or tricresyl phosphate, the addition of described plasticizer is polyvinyl butyral resin tree
The 0.2-0.8% of lipid amount；
Antioxidant described in step (3) is antioxidant DLTP, and the addition of described antioxidant is polyvinyl butyral resin
The 0.05-0.5% of resin quality；
Auxiliary agent described in step (3) is sodium soap, sodium alkyl sulfonate, sodium alklyarylsulfonate anionic auxiliary, or is epoxy
Ethane nonionic auxiliary agent；The addition of described auxiliary agent is the 0.02-0.08% of polyvinyl butyral resin quality.
9. the manufacture method according to claim 1 it is characterised in that：In step (3), extruder melt temperature scope exists
110-130℃.
10. the manufacture method according to claim 1 it is characterised in that：Gained polyvinyl butyral film is in thickness
Yellow colour index≤5 during 0.76mm, light transmittance >=90%, mist degree≤0.5%.
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| CN201610911267.5A CN106398071A (en) | 2016-10-19 | 2016-10-19 | Manufacturing method of polyvinyl butyral film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589729A (en) * | 2017-02-20 | 2017-04-26 | 苏州聚冠复合材料有限公司 | Modified PVB slice and preparing method thereof |
| CN106947335A (en) * | 2017-04-28 | 2017-07-14 | 成都玉龙化工有限公司 | A kind of solvent resistant polyvinyl butyral resin formula and preparation method thereof |
| CN110903585A (en) * | 2019-12-11 | 2020-03-24 | 江西省宏丰塑胶有限公司 | Modified PVB resin and preparation method thereof |
| CN111499780A (en) * | 2020-05-26 | 2020-08-07 | 河南省科学院化学研究所有限公司 | Synthetic method of polyvinyl butyral resin |
| CN112533962A (en) * | 2018-08-16 | 2021-03-19 | Skc株式会社 | Method for producing polyvinyl butyral resin composition, and film for glass bonding comprising same |
| CN113861315A (en) * | 2021-09-18 | 2021-12-31 | 忠信（清远）光伏材料科技有限公司 | Polyvinyl butyral with sound insulation performance and preparation method thereof |
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| CN102827314A (en) * | 2012-09-05 | 2012-12-19 | 安徽皖维集团有限责任公司 | Preparation method of high transparency polyvinyl butyral resin |
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| CN101108532A (en) * | 2006-07-18 | 2008-01-23 | 浙江利丰塑胶有限公司 | Method for preparing polyvinyl butyral rubber sheet |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589729A (en) * | 2017-02-20 | 2017-04-26 | 苏州聚冠复合材料有限公司 | Modified PVB slice and preparing method thereof |
| CN106947335A (en) * | 2017-04-28 | 2017-07-14 | 成都玉龙化工有限公司 | A kind of solvent resistant polyvinyl butyral resin formula and preparation method thereof |
| CN112533962A (en) * | 2018-08-16 | 2021-03-19 | Skc株式会社 | Method for producing polyvinyl butyral resin composition, and film for glass bonding comprising same |
| CN112533962B (en) * | 2018-08-16 | 2023-09-19 | 爱思开迈克沃有限公司 | Method for producing polyvinyl butyral resin composition and film for glass bonding comprising same |
| CN110903585A (en) * | 2019-12-11 | 2020-03-24 | 江西省宏丰塑胶有限公司 | Modified PVB resin and preparation method thereof |
| CN111499780A (en) * | 2020-05-26 | 2020-08-07 | 河南省科学院化学研究所有限公司 | Synthetic method of polyvinyl butyral resin |
| CN111499780B (en) * | 2020-05-26 | 2023-01-24 | 河南省科学院化学研究所有限公司 | Synthetic method of polyvinyl butyral resin |
| CN113861315A (en) * | 2021-09-18 | 2021-12-31 | 忠信（清远）光伏材料科技有限公司 | Polyvinyl butyral with sound insulation performance and preparation method thereof |
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Application publication date: 20170215 |