CN102602005B - Method for manufacturing PETG (polyethylene terephthalate glycol) heat-shrink film - Google Patents
Method for manufacturing PETG (polyethylene terephthalate glycol) heat-shrink film Download PDFInfo
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- CN102602005B CN102602005B CN201210070446.2A CN201210070446A CN102602005B CN 102602005 B CN102602005 B CN 102602005B CN 201210070446 A CN201210070446 A CN 201210070446A CN 102602005 B CN102602005 B CN 102602005B
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Abstract
The invention discloses a method for manufacturing a PETG (polyethylene terephthalate glycol)-1,4-cyclohexylene dimethylene terephthalate heat-shrink film with low shrink stress, high transverse shrink rate, low longitudinal shrink rate and low haze. PETG materials are plasticized and melted in an extruder after being dried and are extruded into a uniform membrane by a T-shaped die head. The membrane is quenched and shaped on a cooling roller, and is longitudinally stretched by the ratio of 1:1.1-1.5 after being preheated by seven preheating rollers. The membrane is cooled and shaped by four cooling rollers, is transversely stretched by the ratio of 1:3-6 after being longitudinally stretched and preheated, and then is cooled and shaped by the cooling rollers, trimmed, treated by means of corona and coiled into a finished product.
Description
Technical field
The present invention relates to a kind of manufacture method of packing with heat-shrinkable film material, the manufacture method of specifically polyethylene terephthalate-Isosorbide-5-Nitrae-cyclohexanedimethanol ester (PETG) heat-shrinkable film.
Background technology
PETG is the condensation polymer of terephthalic acid (TPA), ethylene glycol, Isosorbide-5-Nitrae-cyclohexanedimethanol, and in its production process, because the ethylene glycol of some is replaced by Isosorbide-5-Nitrae-cyclohexanedimethanol, polymer can prevent crystallization, is a kind of amorphism copolyester.
Along with improving constantly of scientific and technological progress and people's living standard, people require more and more higher to the external packing of expensive goods.PETG heat shrink films has nontoxic, tasteless, high strength, and percent thermal shrinkage is high, and packing effect is attractive in appearance.The advantage of PETG mylar maximum is that heat sealing performance is good, easy to operate when involution, and involution is effective and easily use glue bonding, and optical property and mechanical extensibility are all fine simultaneously.PETG about Food Contact standard, can be applied to the packing in the field such as food and individual health care articles for use, medical and health equipment food by U.S. FDA, also can be used for electronic device packing, and meets environmental protection recovery demand.
The PETG heat-shrinkable film of being made up of the biaxial tension of PETG material is a kind of high-performance shrink film, final shrinkage factor can be greater than 70%, can be made into the packing of complex appearance container, there is high plastic uptake power, the high grade of transparency, high glaze, low haze, is easy to printing, difficult drop-off, the low advantage of natural shrinking rate when storage, is applied to the shrink label of shrink wrapping and the electronic product etc. of beverage bottle, foods and cosmetics.Compared with PVC shrink film, PETG shrink film also has advantages of environmental protection.So PETG heat-shrinkable film is widely applied at packaging field.Only have in the world at present this product of minority enterprise energy processing, and these product percent thermal shrinkages are still not high, product transparency is also lower, mist degree reaches more than 5%, shrinkage stress is large, improves percent thermal shrinkage and the transparency of product, and reducing shrinkage stress is the technical barrier that this area will be captured.
Summary of the invention
The object of this invention is to provide one and there is low shrinkage stress, horizontal high shrinkage, longitudinal low-shrinkage, the manufacture method of polyethylene terephthalate-Isosorbide-5-Nitrae-cyclohexanedimethanol ester (PETG) heat-shrinkable film of low haze.
The present invention includes the following step:
A. select inherent viscosity 0.55 ~ 0.85dL/g, 60 ~ 90 ℃ of Vicat softening points, ethylene glycol and 1 in polymer, the mol ratio of 4-cyclohexanedimethanol monomer is the PETG material of 1 ︰ 4 ~ 7, after oven dry in extruder plastifying fusion, extrude the even diaphragm that forms 0.2 ~ 0.5 millimeter of thickness through the T shape die head of 260 ~ 280 ℃, diaphragm is chilling sizing on the chill roll of 20 ~ 60 ℃;
B. diaphragm carries out the longitudinal stretching of 1.1 ~ 1.5 times of l ︰ after the preheat roll preheating of 70 ~ 90 ℃, then uses the chill roll cooling and shaping of 40 ~ 65 ℃;
C. the diaphragm after longitudinal stretching carries out the cross directional stretch of 3 ~ 6 times of l ︰ after the preheating of 75 ~ 90 ℃, then uses 50 ~ 70 ℃ of chill roll cooling and shapings, trimming, and sided corona treatment, rolling becomes finished product.
In PETG resin of the present invention, the mol ratio of ethylene glycol and Isosorbide-5-Nitrae cyclohexanedimethanol monomer is preferably 1 ︰ 4.5 ~ 5.5.
The upper and lower surface of diaphragm can also respectively have adherent layer, the material of adherent layer is made up of 90 ~ 97% PETG material and 3 ~ 10% PETG antitack agent by weight percentage, and adherent layer is closed and extruded by the sizing surface layer of die lip by the flow-rate ratio of upper 0.5 ~ 1.2 ︰ 10 ︰ 0.5 ~ 1.2 of lower floor after injection machine melting in T shape die head.
Also can in diaphragm PETG material, add 2 ~ 5% PETG antitack agent of PETG material weight.
Longitudinal stretching is 1.1 ~ 1.2 times of preferred l ︰; Cross directional stretch ratio is for being preferably 4 ~ 5 times of l ︰.
PETG antitack agent of the present invention is that be weight percentage 2 ~ 3% nano-kaoline and surplus is the blend composition of PETG material.
The present invention makes polymer molecular chain in this both direction elongation, orientation at vertical and horizontal drawing process, make product there is (99 ℃ of very high lateral shrinkages, 10 seconds, laterally >=78%), lower longitudinal contraction rate (≤0.5%), transparency high (mist degree≤1.5), there is good machinery special, intensity is high, firmness is large, elastic modelling quantity large (longitudinally MD >=2000MPa, laterally TD >=4000MPa), hot strength high (longitudinally MD >=50MPa, laterally TD >=200MPa).
Especially the product shrinkage stress that, the present invention produces can be low to moderate 6MPa.The advantage of low convergent force is the packaged product that can be applied to thinning, process in shrink wrapping is more even, can be used as the high-quality base material of the industrial circles such as high-grade packing, printing, electronic apparatus, dressing of cable, insulating materials, and the external application label such as various canned polyester bottles, various containers.
The specific embodiment
Embodiment 1
Material therefor: PETG: transparent, inherent viscosity 0.7dL/g, 69 ℃ of Vicat softening points;
PETG antitack agent: inherent viscosity 0.62dL/g, 69 ℃ of Vicat softening points, kaolin content 2wt%.
Above-mentioned material is prepared intermediate layer material by weight: 100 parts of PETG; Upper and lower surface layer material: 95 parts of PETG, 5 parts of PETG antitack agents.
After intermediate layer material and skin-material evenly mix respectively, deliver to respectively 65 ℃ of continuous dryers and dry (approximately 6 hours time), remove raw material surface moisture, then pass through apparatus for separating metals, by the metal fillings of carrying secretly in material or particle separation out, deliver to separately again an extruder plastifying fusion, 275 ℃ of melt temperatures, melt is evenly mixing and conveying of quilt under screw rod High Rotation Speed.At course of conveying, the lower-molecular substance gasifying in melt and decompose gas out and moisture by the steam vent of extruder, be pumped into condenser system by vavuum pump, lower-molecular substance etc. is separated.Refilter and remove plasticizing bad material and impurity, guarantee that the height of melt is pure.Melt is closed and is extruded by the sizing surface layer of die lip by the flow-rate ratio of upper 3 ︰ 34 ︰ 3 of lower floor in T shape die head, through highly bright and clean, temperature is the chill roll chilling sizing of 35 ℃, becomes by three layers and forms again, thickness is the even diaphragm of 0.22 millimeter, and diaphragm thickness is regulated and determined by die head.
Diaphragm after chilling sizing is through the multiple tracks preheat roll preheating of 80 ℃, utilizes the speed of roller and quick roll at a slow speed poor by the stretching ratio one-off drawing moulding of 1 ︰ 1.2, through 60 ℃ of chill roll cooling and shapings, completes longitudinal stretching.
In diaphragm baking oven after longitudinal stretching, be preheated to 85 ℃, utilize adjustable track by chain folder traction diaphragm, complete cross directional stretch by the stretching ratio of 1 ︰ 4.5, then use 50 ℃ of cooling and shapings.
Stretched film, first excises its both sides with bead cutter, then carries out high-frequency corona processing with corona machine, to increase adhesive force and the frictional force of printing-ink.The rolling on winder of film after sided corona treatment is bundled, then naturally places a period of time, carries out Ageing Treatment, makes the performance trend of product stable.
Biaxial tension PETG film after Ageing Treatment, utilizes cutting machine to cut into the specification that user requires, and then packs, and obtains biaxial tension PETG heat-shrinkable film finished product.
Above-mentioned finished product after testing, thickness 40.7 μ m, the wherein each approximately 3 μ m of upper and lower two surface layer thicknesses, percent thermal shrinkage (99 ℃, 10 seconds) is (TD) 79% laterally, longitudinally (MD) 0.5%, mist degree 1.2%, glossiness (45 °) 126.4%, hot strength: longitudinally (MD) 57.8MPa, laterally (TD) 223.7MPa, elastic modelling quantity: longitudinally (MD) 2180MPa, laterally (TD) 4360MPa, shrinkage stress 6MPa, is the good PETG heat-shrinkable film of performance.
Embodiment 2
Material therefor:
PETG: transparent, inherent viscosity 0.7dL/g, 69 ℃ of Vicat softening points; PETG antitack agent: inherent viscosity 0.62dL/g, 69 ℃ of Vicat softening points, kaolin content 2wt%.
Above-mentioned material is batching by weight, individual layer: 97 parts, and PETG, 3 parts of PETG antitack agents.
Extruded the individual layer diaphragm that forms 0.20 millimeters thick by a double screw extruder plastifying fusion, other processing step is identical with EXAMPLE l, stretching condition:
40 ℃ of chill-roll temperature after T shape die head is extruded;
78 ℃ of longitudinal stretching preheat roll temperature, stretching ratio 1 ︰ 1.15, longitudinal stretching cooling and shaping temperature 45 C;
82 ℃ of cross directional stretch preheat temperatures, stretching ratio 1 ︰ 4.4,65 ℃ of cross directional stretch cooling and shaping temperature.
Above-mentioned finished product after testing, thickness 39.6 μ m; Percent thermal shrinkage (99 ℃, 10 seconds): laterally TD:78.2%, longitudinally MD:0.3%; Mist degree 1.4%; Glossiness (45 °) 121.5%; Hot strength: longitudinally MD:52.6MPa, laterally TD:208.8MPa; Elastic modelling quantity: longitudinally MD:2093MPa, laterally (TD) 4210MPa, shrinkage stress 6MPa, is the good PETG heat-shrinkable film of performance.
Claims (6)
1. a manufacture method for PETG heat-shrinkable film, is characterized in that, comprises the following steps:
A. select inherent viscosity 0.55 ~ 0.85dL/g, 60 ~ 90 ℃ of Vicat softening points, ethylene glycol and 1 in polymer, the mol ratio of 4-cyclohexanedimethanol monomer is the PETG material of 1 ︰ 4 ~ 7, after oven dry in extruder plastifying fusion, extrude the even diaphragm that forms 0.2 ~ 0.5 millimeter of thickness through the T shape die head of 260 ~ 280 ℃, diaphragm is chilling sizing on the chill roll of 20 ~ 60 ℃;
B. diaphragm carries out the longitudinal stretching of 1.1 ~ 1.5 times of l ︰ after the preheat roll preheating of 70 ~ 90 ℃, then uses the chill roll cooling and shaping of 40 ~ 65 ℃;
C. the diaphragm after longitudinal stretching carries out the cross directional stretch of 3 ~ 6 times of l ︰ after the preheating of 75 ~ 90 ℃, then uses 50 ~ 70 ℃ of chill roll cooling and shapings, trimming, and sided corona treatment, rolling becomes finished product.
2. the manufacture method of PETG heat-shrinkable film according to claim 1, is characterized in that, in described PETG resin, the mol ratio of ethylene glycol and Isosorbide-5-Nitrae-cyclohexanedimethanol monomer is 1 ︰ 4.5 ~ 5.5.
3. according to the manufacture method of PETG heat-shrinkable film described in claim 1 or 2, it is characterized in that, in steps A, the upper and lower surface of diaphragm also respectively has adherent layer, and adherent layer material is made up of 90 ~ 97% PETG material and 3 ~ 10% PETG antitack agent by weight percentage; Adherent layer material after injection machine melting in T shape die head by the flow-rate ratio of upper 0.5 ~ 1.2 ︰ 10 ︰ 0.5 ~ 1.2 of lower floor the sizing face by die lip and diaphragm laminated extruding simultaneously.
4. according to the manufacture method of PETG heat-shrinkable film described in claim 1 or 2, it is characterized in that, in described diaphragm, add 2 ~ 5% PETG antitack agent of PETG material weight.
5. according to the manufacture method of PETG heat-shrinkable film described in claim 1 or 2, it is characterized in that, longitudinal stretching is than being 1.1 ~ 1.3 times of l ︰.
6. according to the manufacture method of PETG heat-shrinkable film described in claim 1 or 2, it is characterized in that, cross directional stretch is than being 4 ~ 5 times of l ︰.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210070446.2A CN102602005B (en) | 2012-03-17 | 2012-03-17 | Method for manufacturing PETG (polyethylene terephthalate glycol) heat-shrink film |
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| CN201210070446.2A CN102602005B (en) | 2012-03-17 | 2012-03-17 | Method for manufacturing PETG (polyethylene terephthalate glycol) heat-shrink film |
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| CN102602005A CN102602005A (en) | 2012-07-25 |
| CN102602005B true CN102602005B (en) | 2014-05-21 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102848581B (en) * | 2012-10-03 | 2014-12-24 | 广东华业包装材料有限公司 | Tape casting method for thin film made of 3-hydroxybutyrate-4-hydroxybutyrate copolymer |
| CN102848569B (en) * | 2012-10-03 | 2014-12-10 | 广东华业包装材料有限公司 | Production method of two-way stretched thin film made of 3-hydroxybutyrate-4-hydroxybutyrate copolymer |
| CN103483785B (en) * | 2013-09-29 | 2016-03-30 | 太仓卡斯特姆新材料有限公司 | A kind of PETG heat-shrinkable film and preparation method thereof |
| CN103522713A (en) * | 2013-10-10 | 2014-01-22 | 宁波东旭成新材料科技有限公司 | Low-shrinkage rate bidirectional stretching plastic thin film and preparation method thereof |
| CN107610585B (en) * | 2017-09-18 | 2021-04-20 | 江苏景宏新材料科技有限公司 | Preparation of washable transparent heat-shrinkable beer bottle label and label washing process thereof |
| CN108044919B (en) * | 2017-12-08 | 2022-08-12 | 无锡宏义高分子材料科技有限公司 | Secondary extension process of PVC (polyvinyl chloride) adhesive tape and application thereof |
| CN115260707B (en) * | 2022-07-02 | 2023-10-27 | 福建晋江宏洋新材料科技有限责任公司 | High-toughness heat-shrinkable battery label film and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| EP1839849A1 (en) * | 2005-01-11 | 2007-10-03 | Mitsubishi Plastics Inc. | Heat-shrinkable layered film, molded article comprising the film, and heat-shrinkable label and container |
| CN101838445A (en) * | 2010-04-30 | 2010-09-22 | 宜兴市光辉包装材料有限公司 | PETG blow molding film and preparation method thereof |
| CN102152585A (en) * | 2010-12-16 | 2011-08-17 | 浙江强盟实业股份有限公司 | Twistable polyester film and preparation method thereof |
| CN102196908A (en) * | 2008-10-24 | 2011-09-21 | 埃克森美孚石油公司 | Multilayer shrink, films, labels made therefrom and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5059027B2 (en) * | 2006-01-27 | 2012-10-24 | コーロン インダストリーズ インク | Heat-shrinkable polyester film |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1839849A1 (en) * | 2005-01-11 | 2007-10-03 | Mitsubishi Plastics Inc. | Heat-shrinkable layered film, molded article comprising the film, and heat-shrinkable label and container |
| CN102196908A (en) * | 2008-10-24 | 2011-09-21 | 埃克森美孚石油公司 | Multilayer shrink, films, labels made therefrom and use thereof |
| CN101838445A (en) * | 2010-04-30 | 2010-09-22 | 宜兴市光辉包装材料有限公司 | PETG blow molding film and preparation method thereof |
| CN102152585A (en) * | 2010-12-16 | 2011-08-17 | 浙江强盟实业股份有限公司 | Twistable polyester film and preparation method thereof |
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Denomination of invention: Method for manufacturing PETG (polyethylene terephthalate glycol) heat-shrink film Effective date of registration: 20150215 Granted publication date: 20140521 Pledgee: Bank of Communications Ltd Chaozhou branch Pledgor: Huaye Packing Materials Co., Ltd., Guangdong Registration number: 2015990000151 |
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Date of cancellation: 20210120 Granted publication date: 20140521 Pledgee: Bank of Communications Ltd Chaozhou branch Pledgor: GUANGDONG HUAYE PACKING MATERIAL Co.,Ltd. Registration number: 2015990000151 |
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