CN108676300A - A kind of preparation method of low haze polyvinyl butyral film - Google Patents
A kind of preparation method of low haze polyvinyl butyral film Download PDFInfo
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- CN108676300A CN108676300A CN201810685348.7A CN201810685348A CN108676300A CN 108676300 A CN108676300 A CN 108676300A CN 201810685348 A CN201810685348 A CN 201810685348A CN 108676300 A CN108676300 A CN 108676300A
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- Prior art keywords
- plasticizer
- preparation
- polyvinyl butyral
- refractive index
- film
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
-
- 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
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
-
- 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
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
Abstract
The invention belongs to the technical fields of laminated glass intermediate coat, it is related to a kind of preparation method of low haze polyvinyl butyral film, the method is that the polyvinyl butyral resin of part acetalation is plasticized with plasticizer, the plasticizer is mixed plasticizer, including at least plasticizer A and plasticizer B, refractive index≤1.46 of the plasticizer A, the refractive index ＞ 1.48 of the plasticizer B and≤1.54；The refractive index of above-mentioned mixed plasticizer is 1.45-1.52；Above-mentioned plasticizer A is selected from two positive heptanoate of two tricaprylate of triethylene glycol, dioctyl sebacate or tetraethylene glycol；The plasticizer B is selected from diisononyl phthalate, repefral or phthalic acid phenyl dibutyl ester.The preparation method of low haze polyvinyl butyral film provided by the invention can prepare the polyvinyl butyral film that mist degree is less than 0.3, its mist degree can reach 0.2 or less in the preferred case.
Description
Technical field
The invention belongs to the technical fields of laminated glass intermediate coat, are related to a kind of system of low haze polyvinyl butyral film
Preparation Method.
Background technology
Laminated glass is usually made of two glass sheets with the intermediate film for bonding the glass plate.It is presently used for interlayer glass
The intermediate film of glass is mainly polyvinyl butyral film (PVB film), and PVB films are by polyvinyl butyral resin, plasticizer
With auxiliary agent by screw extruder mixing extrusion machine-shaping, the laminated glass of PVB films production is widely used in automotive field, gear
In wind glass, building field, facade component, or for manufacturing photovoltaic module.
Mist degree is one of the important element for evaluating laminated glass optical property.The big PVB films of mist degree are being used for automobile, are building
When building equal fields, prodigious influence is produced on the perception of laminated glass, even meeting when being especially employed in windshield
Influence the safety of driving.Requirement in national standard to laminated glass-use polyvinyl butyral intermediate coat at present be
Mist degree≤0.7 under the thickness specification of 0.76mm.The product level of haze of the manufacturer of PVB films both domestic and external is generally 0.4-
0.6, it is difficult to reach 0.3 or less.Expand year by year with the dosage of PVB films, there is an urgent need to markets to release the PVB with more low haze
Film product.
The mist degree of PVB films is influenced by polyvinyl butyral resin mist degree itself and plasticizer.The addition of plasticizer
The glass transition temperature for reducing PVB films improves the processing flowability of PVB films, and it is tough to provide the good low temperature of PVB films
Property, improve the shock resistance of PVB films.Chinese patent CN104497176B provides a kind of manufacture low haze polyvinyl alcohol contracting
The method of butyral resin powder.It obtains with the film compared with low haze being one by reducing the mist degree of polyvinyl butyral resin powder
The more directly easy method of kind, but since the production technology of polyvinyl butyral resin powder causes more or less can all exist
Impurity (predominantly inorganic salts) residual of mist degree is caused, mist degree quality is difficult to be improved again.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of preparation methods of low haze polyvinyl butyral film, lead to
The polyvinyl butyral resin and mixed plasticizer for crossing part acetalation are plasticized, and the poly- second that mist degree is less than 0.3 is prepared
Enol butyral film.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of low haze polyvinyl butyral film, the method are that the polyvinyl alcohol of part acetalation contracts
Butyral resin is plasticized with plasticizer, and the plasticizer is mixed plasticizer, includes at least plasticizer A and plasticizer B, described
Refractive index≤1.46 of plasticizer A, the refractive index ＞ 1.48 of the plasticizer B and≤1.54.
Above-mentioned mixed plasticizer can be the mixing of two kinds of plasticizer of plasticizer A and plasticizer B, can also be three kinds or more
The mixing of plasticizer, including plasticizer A, plasticizer B and other plasticizer.
Preferably, the refractive index of above-mentioned mixed plasticizer is 1.45-1.52.
As a further preference, the refractive index of above-mentioned mixed plasticizer is 1.47-1.50.
Preferably, above-mentioned plasticizer A is selected from two positive enanthic acid of two tricaprylate of triethylene glycol, dioctyl sebacate or tetraethylene glycol
Ester；The plasticizer B is selected from diisononyl phthalate, repefral or phthalic acid phenyl dibutyl ester.
As a further preference, above-mentioned plasticizer A is dioctyl sebacate, and the plasticizer B is phthalic acid two
Methyl esters.
Preferably, the mass ratio of above-mentioned polyvinyl butyral resin and mixed plasticizer is 72：28.
The preparation method of above-mentioned polyvinyl butyral film can be added well known by persons skilled in the art other in the preparation
Additive, such as UV- absorbents, antioxidant, cell adhesion modulating agent, surface tension modifier, organic or inorganic nano particle, stabilization
Agent.
Polyvinyl butyral film in above-mentioned preparation method is molded by screw extruder mixing extrusion.
Its specific preparation method is as follows:
PVB resin powder, mixed plasticizer, auxiliary agent are put into a manner of measuring in double screw extruder, draw ratio is
36：1, processing temperature is set between 160-190 DEG C, and fusion plastification under conditions of screw speed 80RPM passes through opening
The T-die of 0.5mm -0.8mm forms the PVB films that thickness is 0.76mm and is batched as finished product through cooling and shaping.
The principle that the present invention can reduce polyvinyl butyral film is：The film that polyvinyl butyral resin is processed exists
Performance on mist degree between by plasticizer and polyvinyl butyral resin refractive index difference influenced.Phthalate is plasticized
Although agent has with refractive index similar in polyvinyl butyral resin, the polyvinyl butyral film being individually plasticized due to it
Low temperature impact strength is poor, cannot be used alone, referring to US2527793A and US4144217A about phthalate
The description of the polyvinyl butyral resin low temperature impact strength of elasticizer plasticizing.Therefore, ensureing polyvinyl butyral
While resin raw material is had compared with low haze, two or more plasticizer is mixed by a certain percentage, passes through increasing
The adjusting of modeling agent refractive index can further improve the mist degree of PVB films.
The present invention having the beneficial effect that compared with the existing technology：
The present invention can prepare the low haze polyvinyl alcohol contracting fourth that mist degree is less than 0.3 by adjusting the formula of plasticizer
Aldehyde film, in the preferred case its mist degree can reach 0.2 hereinafter, being significantly better than the polyethylene of 0.4-0.6 mist degrees in the prior art
Butyral film.The reduction of mist degree makes the transparency of laminated glass and perception be improved, especially by the polyethylene of low haze
When butyral film is used for windshield, the safety of running car is substantially increased.
Specific implementation mode
Below by the description of specific implementation mode, the invention will be further described, but this is not the limit to the present invention
System, those skilled in the art's basic thought according to the present invention, various modifications may be made or improves, but without departing from
The basic thought of the present invention, is all within the scope of the present invention.
Various raw materials and reagents used in the embodiment of the present invention are commercially available purchase unless otherwise instructed.
The test method of film mist degree in the embodiment of the present invention：The method provided according to standard GB/T/T 32020-2015
It measures.
The test method of refractive index in the embodiment of the present invention：It is surveyed according to standard GB/T/T 6488-2008 methods provided
It is fixed.
Embodiment：
The polyvinyl butyral resin of part acetalation mixes extrusion with plasticizer and is cast into PVB films, and specific steps are such as
Under：
PVB resin powder, mixed plasticizer, auxiliary agent are put into a manner of measuring in double screw extruder, draw ratio is
36：1, processing temperature is set between 160-190 DEG C, and fusion plastification under conditions of screw speed 80RPM passes through opening
The T-die of 0.5mm -0.8mm forms the PVB films that thickness is 0.76mm and is batched as finished product through cooling and shaping.
On the basis of choosing in industry representative 28% as mixed plasticizer and accounting for the quality % of film, under
Extrusion molding obtains film, and the mist degree of test film to the mixture composition that table provides in aforementioned manners.
Wherein：Quality % indicates that plasticizer accounts for the mass percent of film total material composition.
3G8 indicates two tricaprylate of triethylene glycol；
DOS indicates dioctyl sebacate；
4G7 indicates two positive heptanoate of tetraethylene glycol；
DINP indicates diisononyl phthalate；
DMP indicates repefral；
BBP indicates phthalic acid phenyl dibutyl ester.
Pass through comparative example 1, it may be said that the composition of the bright typical mixture for being used for preparing PVB films (PVB of 72 mass % and
The 3G8 of 28 mass %) film of extrusion molding is unable to get the low haze less than 0.3.
Pass through comparative example 2, it may be said that the mixed plasticizer of the bright plasticizer two kinds of low-refractions being mixed to get is used for
The plasticising lower PVB resin of mist degree cannot still obtain the low haze film less than 0.3.
Embodiment 1-6 proves there is the low haze characteristic for being less than 0.3 according to the obtained film given to this invention that is formulated.Its
The refractive index of mixed plasticizer used in middle embodiment 1-6 increases successively, obtains the haze value of corresponding membrane and first reduces, after increase,
Illustrating the refractive index of mixed plasticizer, there are an advantageous ranges for the reduction of haze value.In numerous embodiments, embodiment 4
In film show minimum mist degree, this illustrates that the refractive index of its mixed plasticizer matches the most with PVB resin, is embodiment
In optimal proportion.
Claims (7)
1. a kind of preparation method of low haze polyvinyl butyral film, the method is the polyvinyl alcohol contracting fourth of part acetalation
Urea formaldehyde is plasticized with plasticizer, which is characterized in that the plasticizer is mixed plasticizer, includes at least plasticizer A and increasing
Mould agent B, refractive index≤1.46 of the plasticizer A, the refractive index ＞ 1.48 of the plasticizer B and≤1.54.
2. preparation method according to claim 1, which is characterized in that the refractive index of the mixed plasticizer is 1.45-
1.52。
3. preparation method according to claim 2, which is characterized in that the refractive index of the mixed plasticizer is 1.47-
1.50。
4. preparation method according to claim 1, which is characterized in that the plasticizer A be selected from two tricaprylate of triethylene glycol,
Two positive heptanoate of dioctyl sebacate or tetraethylene glycol；The plasticizer B is selected from diisononyl phthalate, phthalic acid two
Methyl esters or phthalic acid phenyl dibutyl ester.
5. preparation method according to claim 4, which is characterized in that the plasticizer A is dioctyl sebacate, the increasing
It is repefral to mould agent B.
6. preparation method according to claim 1, which is characterized in that the polyvinyl butyral resin with mix plasticising
The mass ratio of agent is 72：28.
7. according to the preparation method described in any one of claim 1-6, which is characterized in that the polyethylene in the preparation method
Butyral film is molded by screw extruder mixing extrusion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810685348.7A CN108676300B (en) | 2018-06-28 | 2018-06-28 | Preparation method of low-haze polyvinyl butyral film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810685348.7A CN108676300B (en) | 2018-06-28 | 2018-06-28 | Preparation method of low-haze polyvinyl butyral film |
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| Publication Number | Publication Date |
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| CN108676300A true CN108676300A (en) | 2018-10-19 |
| CN108676300B CN108676300B (en) | 2021-02-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810685348.7A Active CN108676300B (en) | 2018-06-28 | 2018-06-28 | Preparation method of low-haze polyvinyl butyral film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699017A (en) * | 2019-11-29 | 2020-01-17 | 安徽皖维皕盛新材料有限责任公司 | Polyvinyl butyral ultra-white transparent film and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2710263A (en) * | 1951-02-02 | 1955-06-07 | Minnesota Mining & Mfg | Heat-sensitive copying-paper |
| CN104497176A (en) * | 2014-12-12 | 2015-04-08 | 安徽皖维集团有限责任公司 | Preparation method of low-haze polyvinyl butyral resin |
| CN105622969A (en) * | 2015-11-26 | 2016-06-01 | 陈庆江 | Technology for producing polyvinyl butyral intermediate film |
| CN107141675A (en) * | 2017-06-22 | 2017-09-08 | 合肥钢骨玻璃制品有限公司 | A kind of intermediate film for laminated glasses and preparation method thereof |
-
2018
- 2018-06-28 CN CN201810685348.7A patent/CN108676300B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2710263A (en) * | 1951-02-02 | 1955-06-07 | Minnesota Mining & Mfg | Heat-sensitive copying-paper |
| CN104497176A (en) * | 2014-12-12 | 2015-04-08 | 安徽皖维集团有限责任公司 | Preparation method of low-haze polyvinyl butyral resin |
| CN105622969A (en) * | 2015-11-26 | 2016-06-01 | 陈庆江 | Technology for producing polyvinyl butyral intermediate film |
| CN107141675A (en) * | 2017-06-22 | 2017-09-08 | 合肥钢骨玻璃制品有限公司 | A kind of intermediate film for laminated glasses and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699017A (en) * | 2019-11-29 | 2020-01-17 | 安徽皖维皕盛新材料有限责任公司 | Polyvinyl butyral ultra-white transparent film and preparation method thereof |
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| CN108676300B (en) | 2021-02-02 |
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