CN108676300B - Preparation method of low-haze polyvinyl butyral film - Google Patents
Preparation method of low-haze polyvinyl butyral film Download PDFInfo
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- CN108676300B CN108676300B CN201810685348.7A CN201810685348A CN108676300B CN 108676300 B CN108676300 B CN 108676300B CN 201810685348 A CN201810685348 A CN 201810685348A CN 108676300 B CN108676300 B CN 108676300B
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- plasticizer
- polyvinyl butyral
- haze
- film
- refractive index
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- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000004014 plasticizer Substances 0.000 claims abstract description 65
- 229920005989 resin Polymers 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 20
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical group COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims abstract description 12
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Chemical group CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229960001826 dimethylphthalate Drugs 0.000 claims abstract description 6
- MIMDHDXOBDPUQW-UHFFFAOYSA-N dioctyl decanedioate Chemical compound CCCCCCCCOC(=O)CCCCCCCCC(=O)OCCCCCCCC MIMDHDXOBDPUQW-UHFFFAOYSA-N 0.000 claims abstract description 6
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical group CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 claims abstract description 5
- SSKNCQWPZQCABD-UHFFFAOYSA-N 2-[2-[2-(2-heptanoyloxyethoxy)ethoxy]ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOCCOC(=O)CCCCCC SSKNCQWPZQCABD-UHFFFAOYSA-N 0.000 claims abstract description 4
- -1 phenyl dibutyl phthalate Chemical group 0.000 claims abstract description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N phthalic acid di-n-butyl ester Natural products CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 5
- MUGSTXRSLGJVOB-UHFFFAOYSA-N 2-[2-[2-(6-methylheptanoyloxy)ethoxy]ethoxy]ethyl 6-methylheptanoate Chemical compound C(CCCCC(C)C)(=O)OCCOCCOCCOC(CCCCC(C)C)=O MUGSTXRSLGJVOB-UHFFFAOYSA-N 0.000 claims description 3
- 239000005340 laminated glass Substances 0.000 abstract description 7
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 10
- 239000011521 glass Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 102100035474 DNA polymerase kappa Human genes 0.000 description 1
- 101710108091 DNA polymerase kappa Proteins 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- VJHINFRRDQUWOJ-UHFFFAOYSA-N dioctyl sebacate Chemical compound CCCCC(CC)COC(=O)CCCCCCCCC(=O)OCC(CC)CCCC VJHINFRRDQUWOJ-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
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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
-
- 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
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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)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Joining Of Glass To Other Materials (AREA)
Abstract
The invention belongs to the technical field of laminated glass intermediate films, and relates to a preparation method of a low-haze polyvinyl butyral film, which is characterized in that a part of acetalized polyvinyl butyral resin and a plasticizer are plasticized, wherein the plasticizer is a mixed plasticizer and at least comprises a plasticizer A and a plasticizer B, the refractive index of the plasticizer A is less than or equal to 1.46, and the refractive index of the plasticizer B is more than 1.48 and less than or equal to 1.54; the refractive index of the mixed plasticizer is 1.45-1.52; the plasticizer A is selected from triethylene glycol diisocaprylate, dioctyl sebacate or tetraethylene glycol di-n-heptanoate; the plasticizer B is selected from diisononyl phthalate, dimethyl phthalate or phenyl dibutyl phthalate. The preparation method of the low-haze polyvinyl butyral film provided by the invention can be used for preparing the polyvinyl butyral film with the haze lower than 0.3, and the haze of the polyvinyl butyral film can be less than 0.2 under the optimal condition.
Description
Technical Field
The invention belongs to the technical field of interlayer glass intermediate films, and relates to a preparation method of a low-haze polyvinyl butyral film.
Background
Laminated glass is generally composed of two glass plates and an intermediate film that bonds the glass plates. At present, an intermediate film for laminated glass is mainly a polyvinyl butyral film (PVB film), the PVB film is formed by mixing, extruding and processing polyvinyl butyral resin, a plasticizer and an auxiliary agent through a screw extruder, and the laminated glass produced by the PVB film is widely used in the automobile field, the windshield glass, the building field and the facade parts or used for manufacturing photovoltaic modules.
Haze is one of the important elements for evaluating the optical properties of laminated glass. When the PVB film with high haze is used in the fields of automobiles, buildings and the like, the appearance of the interlayer glass is greatly influenced, and particularly when the PVB film is used in automobile windshields, the driving safety is even influenced. The current national standard requires that the polyvinyl butyral intermediate film for laminated glass has a haze of less than or equal to 0.7 under a thickness specification of 0.76 mm. The haze level of products of home and abroad PVB film manufacturers is generally 0.4-0.6, and is difficult to reach below 0.3. As the amount of PVB film used has expanded year by year, there is an urgent need for the market to deliver PVB film products with lower haze.
The haze of a PVB film is affected by the haze of the polyvinyl butyral resin itself as well as the plasticizer. The plasticizer reduces the glass transition temperature of the PVB film, improves the processing flow property of the PVB film, provides good low-temperature toughness of the PVB film, and improves the shock resistance of the PVB film. Chinese patent CN104497176B provides a method for manufacturing low haze polyvinyl butyral resin powder. Obtaining a film with lower haze by reducing the haze of the polyvinyl butyral resin powder is a relatively straightforward and simple method, but the haze quality is hardly improved any more because the process for producing the polyvinyl butyral resin powder leaves more or less impurities (mainly inorganic salts) that contribute to the haze.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a low-haze polyvinyl butyral film, which is used for preparing the polyvinyl butyral film with the haze lower than 0.3 by plasticizing a part of acetalized polyvinyl butyral resin and a mixed plasticizer.
The purpose of the invention is realized by the following technical scheme:
the method for preparing the low-haze polyvinyl butyral film is characterized in that the partially acetalized polyvinyl butyral resin and a plasticizer are plasticized, the plasticizer is a mixed plasticizer and at least comprises a plasticizer A and a plasticizer B, the refractive index of the plasticizer A is less than or equal to 1.46, and the refractive index of the plasticizer B is more than 1.48 and less than or equal to 1.54.
The mixed plasticizer can be a mixture of two plasticizers, namely the plasticizer A and the plasticizer B, or a mixture of more than three plasticizers, including the plasticizer A, the plasticizer B and other plasticizers.
Preferably, the refractive index of the mixed plasticizer is 1.45 to 1.52.
More preferably, the refractive index of the mixed plasticizer is 1.47 to 1.50.
Preferably, the plasticizer A is selected from triethylene glycol diisooctanoate, dioctyl sebacate or tetraethylene glycol di-n-heptanoate; the plasticizer B is selected from diisononyl phthalate, dimethyl phthalate or phenyl dibutyl phthalate.
More preferably, the plasticizer a is dioctyl sebacate, and the plasticizer B is dimethyl phthalate.
Preferably, the mass ratio of the polyvinyl butyral resin to the mixed plasticizer is 72: 28.
the above-mentioned method for preparing the polyvinyl butyral film may be prepared by adding other additives known to those skilled in the art, such as UV-absorbers, antioxidants, adhesion modifiers, surface tension modifiers, organic or inorganic nanoparticles, and stabilizers.
The polyvinyl butyral film in the preparation method is mixed and extruded and molded by a screw extruder.
The specific preparation method comprises the following steps:
putting PVB resin powder, a mixed plasticizer and an auxiliary agent into a double-screw extruder in a metering mode, wherein the length-diameter ratio is 36: 1, setting the processing temperature between 160 ℃ and 190 ℃, melting and plasticizing under the condition of screw rotating speed of 80RPM, forming a PVB film with the thickness of 0.76mm through a T-shaped die with an opening of 0.5 mm-0.8 mm, cooling and shaping, and coiling to obtain a finished product.
The principle of the invention for reducing the polyvinyl butyral film is as follows: the appearance of haze in a film produced from a polyvinyl butyral resin is affected by the difference in refractive index between the plasticizer and the polyvinyl butyral resin. Phthalate plasticizers, while having a refractive index close to that of polyvinyl butyral resins, cannot be used alone because of their poor low temperature impact strength of polyvinyl butyral films plasticized alone, see US2527793A and US4144217A for a description of low temperature impact strength of polyvinyl butyral resins plasticized with phthalate plasticizers. Therefore, the raw material of the polyvinyl butyral resin is ensured to have lower haze, and two or more than two plasticizers are mixed according to a certain proportion, so that the haze of the PVB film can be further improved by adjusting the refractive index of the plasticizer.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, by adjusting the formula of the plasticizer, the low-haze polyvinyl butyral film with the haze lower than 0.3 can be prepared, and the haze of the low-haze polyvinyl butyral film can reach below 0.2 under the optimal condition, which is greatly superior to the polyvinyl butyral film with the haze of 0.4-0.6 in the prior art. The reduction of the haze improves the transparency and the appearance of the laminated glass, and particularly greatly improves the driving safety of an automobile when the polyvinyl butyral film with low haze is used for the windshield of the automobile.
Detailed Description
The present invention is further described in the following description of the specific embodiments, which is not intended to limit the invention, but various modifications and improvements can be made by those skilled in the art based on the basic idea of the invention, but the scope of the invention is within the scope of the invention as long as they do not depart from the basic idea of the invention.
The various starting materials and reagents used in the examples of the present invention were all commercially available unless otherwise specified.
The method for testing the haze of the film in the embodiment of the invention comprises the following steps: measured according to the method provided by the national standard GB/T32020-.
The method for testing the refractive index in the embodiment of the invention comprises the following steps: measured according to the method provided by the national standard GB/T6488-.
Example (b):
the PVB film is prepared by mixing, extruding and casting a part of acetalized polyvinyl butyral resin and a plasticizer, and comprises the following specific steps:
putting PVB resin powder, a mixed plasticizer and an auxiliary agent into a double-screw extruder in a metering mode, wherein the length-diameter ratio is 36: 1, setting the processing temperature between 160 ℃ and 190 ℃, melting and plasticizing under the condition of screw rotating speed of 80RPM, forming a PVB film with the thickness of 0.76mm through a T-shaped die with an opening of 0.5 mm-0.8 mm, cooling and shaping, and coiling to obtain a finished product.
On the basis of selecting an industry-representative 28% as a mixed plasticizer in mass% of the film, a film was obtained by extrusion molding in the above-described manner according to the composition of the mixture given in the following table, and the haze of the film was measured.
Wherein: mass% means the mass percentage of the plasticizer to the total material composition of the film.
3G8 represents triethylene glycol diisooctanoate;
DOS for dioctyl sebacate;
4G7 represents tetraethyleneglycol di-n-heptanoate;
DINP represents diisononyl phthalate;
DMP represents dimethyl phthalate;
BBP represents phenyl dibutyl phthalate.
By way of comparative example 1, it can be shown that a typical composition of the mixture used to prepare a PVB film (72 mass% PVB and 28 mass% 3G8) does not result in a low haze of less than 0.3 for an extruded film.
By way of comparative example 2, it can be shown that the use of a blended plasticizer obtained by blending two low index plasticizers to plasticize a PVB resin having a lower haze still fails to provide a low haze film of less than 0.3.
Examples 1-6 demonstrate that films obtained according to the formulations specified in the present invention have low haze characteristics of less than 0.3. In which the refractive indices of the mixed plasticizers used in examples 1 to 6 were increased in the order in which the haze values of the corresponding films were reduced and then increased, indicate that the refractive indices of the mixed plasticizers had a favorable range for the reduction of the haze values. In many examples, the film of example 4 exhibited the lowest haze, indicating that its blend plasticizer index was the closest match to the PVB resin, which is the optimum blend in the examples.
Claims (6)
1. The preparation method of the low-haze polyvinyl butyral film is characterized in that the plasticizer is a mixed plasticizer and at least comprises a plasticizer A and a plasticizer B, the refractive index of the plasticizer A is less than or equal to 1.46, the refractive index of the plasticizer B is greater than 1.48 and less than or equal to 1.54, the refractive index of the mixed plasticizer is 1.45-1.52, and the refractive index is measured according to the method provided by the national standard GB/T6488-2008.
2. The method according to claim 1, wherein the mixed plasticizer has a refractive index of 1.47 to 1.50.
3. The method of claim 1, wherein the plasticizer A is selected from triethylene glycol diisooctanoate, dioctyl sebacate, and tetraethylene glycol di-n-heptanoate; the plasticizer B is selected from diisononyl phthalate, dimethyl phthalate or phenyl dibutyl phthalate.
4. The method according to claim 3, wherein the plasticizer A is dioctyl sebacate and the plasticizer B is dimethyl phthalate.
5. The production method according to claim 1, wherein the mass ratio of the polyvinyl butyral resin to the mixed plasticizer is 72: 28.
6. the production method according to any one of claims 1 to 5, wherein the polyvinyl butyral film in the production method is kneaded and extruded by a screw extruder.
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 |
|---|---|
| CN108676300A CN108676300A (en) | 2018-10-19 |
| CN108676300B true 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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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110699017B (en) * | 2019-11-29 | 2021-09-10 | 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 |
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Denomination of invention: A preparation method for low haze polyvinyl butyral film Granted publication date: 20210202 Pledgee: China CITIC Bank Co.,Ltd. Taizhou Linhai Branch Pledgor: ZHEJIANG DECENT NEW MATERIAL CO.,LTD. Registration number: Y2024330000918 |
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