CN102873954B - A kind of polyester film that can directly seal and preparation method - Google Patents
A kind of polyester film that can directly seal and preparation method Download PDFInfo
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- CN102873954B CN102873954B CN201210375748.0A CN201210375748A CN102873954B CN 102873954 B CN102873954 B CN 102873954B CN 201210375748 A CN201210375748 A CN 201210375748A CN 102873954 B CN102873954 B CN 102873954B
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- 229920006267 polyester film Polymers 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000010410 layer Substances 0.000 claims abstract description 209
- 229920000728 polyester Polymers 0.000 claims abstract description 140
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 claims abstract description 37
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 238000007493 shaping process Methods 0.000 claims abstract description 13
- 238000002425 crystallisation Methods 0.000 claims abstract description 9
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 239000012792 core layer Substances 0.000 claims abstract description 8
- 239000011162 core material Substances 0.000 claims abstract description 4
- 238000003851 corona treatment Methods 0.000 claims abstract description 4
- 238000001514 detection method Methods 0.000 claims abstract description 4
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 claims description 78
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 60
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 58
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000000377 silicon dioxide Substances 0.000 claims description 29
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 18
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 239000004408 titanium dioxide Substances 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 13
- ORLQHILJRHBSAY-UHFFFAOYSA-N [1-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1(CO)CCCCC1 ORLQHILJRHBSAY-UHFFFAOYSA-N 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims description 10
- 239000011733 molybdenum Substances 0.000 claims description 10
- 150000002148 esters Chemical group 0.000 claims description 9
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004246 zinc acetate Substances 0.000 claims description 8
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 7
- 238000005266 casting Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 7
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000005453 pelletization Methods 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000006068 polycondensation reaction Methods 0.000 claims description 6
- 238000004513 sizing Methods 0.000 claims description 6
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 4
- 229940071125 manganese acetate Drugs 0.000 claims description 4
- 239000011565 manganese chloride Substances 0.000 claims description 4
- 229940099607 manganese chloride Drugs 0.000 claims description 4
- 235000002867 manganese chloride Nutrition 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 3
- 239000010408 film Substances 0.000 description 31
- 238000005259 measurement Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 10
- 230000032050 esterification Effects 0.000 description 8
- 238000005886 esterification reaction Methods 0.000 description 8
- 239000010409 thin film Substances 0.000 description 7
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 238000009966 trimming Methods 0.000 description 4
- 229920002799 BoPET Polymers 0.000 description 3
- 239000005041 Mylar™ Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 239000005022 packaging material Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 235000021485 packed food Nutrition 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229920001634 Copolyester Polymers 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Laminated Bodies (AREA)
Abstract
The present invention relates to polyester film and preparation method thereof, disclose a kind of polyester film that can directly seal and preparation method.Polyester film comprises ABC three-decker, and described B layer is intermediate core layer, and material is that PET surpasses bright PET chips; A layer is top layer heat-sealable layer, and material is copolymerization PETG polyester slice; C layer is anti-stick interconnect layer, and material comprises the section of PET antiblocking agent masterbatch and surpasses bright PET chips with PET.Manufacture craft comprises the corresponding polyester slice of preparation, then extrudes stretching by extruder, and the step such as cooling and shaping, crystallization, traction removing slitter edge, sided corona treatment, detection thickness completes.
Description
Technical field
The present invention relates to polyester film and preparation method thereof, particularly relate to a kind of polyester film that can directly seal and preparation method.
Background technology
Along with the raising of socioeconomic development and people's living standard, more and more higher to the requirement of the packaging material of environment-friendly type.PET (polyester) is universally acknowledged environment-friendly and green material.And through the polyester film that can directly seal that modification raw material and special producing technique are made, be a kind of high-performance economizing type and the environment-friendly type new product of China's film industry and heat-sealing film Industry Innovation.Common mylar product, existence cannot seal defect certainly, and in order to the occasion for sealing, it needs to carry out loaded down with trivial details and expensive compound working procedure with other resins usually, thus significantly limit its application.
Because common BOPET mylar does not possess heat sealability, have to adopt the problem method of BOPET and CPP or PE film compound being solved packaging seal.Such as, adopt the complex method such as BOPET/CPP or BOPET/PE or BOPET/VMCPP, so not only make packing cost greatly improve, and because the existence of compound tense residual solvent, thus the health of packaged food can be affected.
Summary of the invention
The present invention is directed to common mylar product in prior art, existence cannot seal defect certainly, in order to the occasion for sealing, it needs to carry out loaded down with trivial details and expensive compound working procedure with other resins usually, provide one and can carry out heat sealing at 120 degree of temperature, not only save the loaded down with trivial details and expensive compound working procedure that conventional polyester film and other resins carry out, save the use waste of resource, also reduce the cost of whole packaging material for food simultaneously, and health more a kind of polyester film that can directly seal and preparation method.
In order to solve the problems of the technologies described above, the present invention is solved by following technical proposals:
The polyester film that can directly seal, comprises ABC three-decker, and described B layer is intermediate core layer, and material is that PET surpasses bright PET chips; A layer is top layer heat-sealable layer, and material is copolymerization PETG polyester slice; C layer is anti-stick interconnect layer, and material comprises the section of PET antiblocking agent masterbatch and surpasses bright PET chips with PET; C layer is anti-stick interconnect layer, and material has the component of following mass percent: the PET antiblocking agent masterbatch section of 30% ~ 60% and 40% ~ 70%PET surpass bright PET chips.In polyester slice, " having light greatly ", " half delustring " and " having light " for be titanium dioxide TiO in polyester slice
2content." have light greatly " polyester slice is also called " super have light " polyester slice, the content of titanium dioxide in its polyester slice is zero; Content of titanium dioxide in the polyester slice that " has light " is about 0.10%; Content of titanium dioxide in " half delustring " polyester slice is (0.32 ± 0.03) %; Content of titanium dioxide in " full-dull " polyester slice is 2.4% ~ 2.5%.Film has ABC type three-decker, and B layer is intermediate core layer, is extruded by main extruder single screw extrusion machine, and extruded material is that 100%PET surpasses bright PET chips; A layer is top layer heat-sealable layer, is extruded by subsidiary extruder double screw extruder, and extruded material is 100% copolymerization PETG polyester slice; C layer is anti-stick interconnect layer, is extruded by subsidiary extruder double screw extruder, and extruded material has the component of following mass percent: PET antiblocking agent masterbatch section 30% ~ 60% and 40% ~ 70%PET surpass bright PET chips.B layer thickness accounts for 70% ~ 80%, A layer thickness and accounts for 10% ~ 20%, C layer thickness and account for 10% ~ 20%.
As preferably, described B layer thickness accounts for 70% ~ 80%, A layer thickness and accounts for 10% ~ 20%, C layer thickness and account for 10% ~ 20%.
As preferably, the copolymerization PETG polyester slice of described A layer top layer heat-sealable layer is by the product of dimethyl terephthalate (DMT) DMT, ethylene glycol EG, silica SiO2 and 1,4-CHDM CHDM totally four kinds of monomer ester-interchange methods polycondensation.
As preferably, in the described anti-stick interconnect layer of C layer, the section of PET antiblocking agent masterbatch is for containing silica SiO
2polyester slice, silica SiO
2particle diameter is 2 ~ 3um, and content is 3000ppm.
A manufacture craft for the polyester film that can directly seal as described in any one of claim 1-4, comprises the steps:
A, the A layer copolymerization PETG polyester slice of preparation, B layer PET surpassed bright PET chips and C layer PET surpasses bright PET chips and the section of PET antiblocking agent masterbatch, send into three-layer co-extruded biaxial tension equipment respectively, wherein A layer copolymerization PETG polyester slice sends into subsidiary extruder---double screw extruder, B layer PET surpasses bright PET chips and sends into main extruder---single screw extrusion machine, and C layer PET surpasses bright PET chips and subsidiary extruder---double screw extruder is sent in the section of PET antiblocking agent masterbatch;
B, ABC tri-layers of polyester slice are extruded melting at 240 ~ 280 DEG C, melt generates PET sheet through less than 30 DEG C cooling slabs;
C, the PET sheet of casting are through 80 ~ 100 DEG C of preheating longitudinal stretchings and less than 35 DEG C temperature cooling and shapings;
PET sheet after d, sizing is again by 86 ~ 110 DEG C of preheating cross directional stretch and 180 ~ 200 DEG C of sizing crystallization treatment;
E, eventually pass traction removing slitter edge, sided corona treatment, detection thickness carry out again rolling batch the one side of obtained thickness 15um ~ 30um can the polyester film of direct heat sealing.
In the heat-sealable layer of A layer top layer, copolymerization PETG polyester slice preparation method is:
A, by 100 parts of dimethyl terephthalate (DMT) DMT, 25 ~ 35 parts of ethylene glycol EG, 1 ~ 5 part of silica SiO
2be uniformly mixed after sending into polymeric kettle with 20 ~ 30 parts of Isosorbide-5-Nitrae cyclohexanedimethanol CHDM;
B, add the antimony oxide Sb of 2 ~ 4 parts again
2o
3with the phosphorous acid triphen C of 2 ~ 4 parts
18h
15o
3p is as catalyst and stabilizing agent;
C, polymeric kettle is airtight after, control polymerization temperature in the kettle and pressure at 170 ~ 210 DEG C and 500 ~ 700pa under, use nitrogen N
2carry out 0.5 ~ 1.5h ester exchange reaction;
D, then will be warming up to 240 ~ 280 DEG C in polymeric kettle, polymeric kettle is vacuumized, then under the effect of composite catalyst, carries out polycondensation reaction 2 ~ 4h in high vacuum;
E, discharging, cooling, pelletizing, obtained copolymerization PETG polyester slice;
Composite catalyst is the composition containing titanium dioxide, silica, compound, zinc acetate and compd A containing molybdenum.
As preferably, described B layer is intermediate core layer, by main extruder---single screw extrusion machine is extruded; A layer is top layer heat-sealable layer, by subsidiary extruder---double screw extruder is extruded; C layer is anti-stick interconnect layer, by subsidiary extruder---double screw extruder is extruded, and A layer subsidiary extruder, B layer main extruder, C layer subsidiary extruder polyester slice are extruded mass ratio and be: 10 ~ 20:65 ~ 80:10 ~ 20.
As preferably, in described step a, be first 20 ~ 30 parts of Isosorbide-5-Nitrae cyclohexanedimethanol CHDM and mass content by mass content be 1 ~ 5 part of silica SiO
2join 25 ~ 35 parts of ethylene glycol EG, dispersed with stirring, then through supersonic oscillations dispersion, after making each composition high speed dispersion homogenizing, send into polymeric kettle; Then add 100 parts of dimethyl terephthalate (DMT) DMT to be uniformly mixed.
As preferably, in described step c, after polymeric kettle is airtight, carry out ester exchange reaction nitrogen N
2carry out displacement 3 times, after ester exchange reaction terminates, reclaim unnecessary ethylene glycol EG, in steps d, composite catalyst is: the composition of titanium dioxide, silica, compound, zinc acetate and compd A containing molybdenum, and compd A takes from any one in manganese acetate or manganese chloride or both mixtures.Composite catalyst composition composite catalyst is the composition containing titanium dioxide, silica, compound, zinc acetate and compd A containing molybdenum.Wherein the weight ratio of titanium dioxide and silica is 100: (6 ~ 9.5); Titanium dioxide is 100 with the weight ratio of the compound containing molybdenum: (5 ~ 40); The weight ratio of titanium dioxide and zinc acetate is 100: (5 ~ 115), the weight ratio of titanium dioxide and compd A is 100: (5 ~ 115), and the weight ratio of titanium dioxide and zinc acetate and compd A total amount is 100: (50 ~ 120).Compound containing molybdenum takes from any one in the oxide of molybdenum or the sulfide of molybdenum or both mixtures; Compd A takes from any one in manganese acetate or manganese chloride or both mixtures.The advantage of this catalyst is that course of reaction side reaction is few, and the polyester obtained has better color and luster.
Of the present invention can direct existing Isosorbide-5-Nitrae cyclohexanedimethanol CHDM in heat-sealable polyester thin film system, have again and add antiblocking agent SiO
2, then adopt two-step method preparation can direct heat-sealable polyester film.For containing silica SiO
2the PETG copolyester of particle, in order to prevent the film blocking produced, must add a certain amount of SiO in film surface layer
2particle, adds SiO
2particle, can reduce heat-seal strength to a certain extent.By to the proportioning of Third monomer and Isosorbide-5-Nitrae cyclohexanedimethanol CHDM and SiO in PETG preparation process
2not only the ratio of particle adjusts, and meets heat sealability requirement to produce but also can prevent heat-sealing polyester film from wrapup procedure, producing adhesion.And must at the enterprising Row sum-equal matrix of production structure for the polyester film that can directly seal, we adopt three-layer co-extruded stretch processes, control the main and auxiliary extruder ratio of film, control thin film crystallization speed, by stretching, shaping and last handling process, with obtained heat-sealing appropriate thickness and SiO
2the rational polyester heat sealing film of opening agent content, simultaneously in order to control the production stability of film, we adjust the ratio of longitudinal stretching, cross directional stretch, temperature and the concrete technology parameter such as air quantity, infrared heating power, finally to obtain the polyester film product that can directly seal of target call.
The present invention can directly be compared with conventional polyester film by heat-sealable polyester film by preparation, except the every good characteristic possessing conventional polyester film, be provided with especially can at 120 degree of temperature the function of heat sealing.This not only can save the loaded down with trivial details and expensive compound working procedure that conventional polyester film and other resins carry out, and saves the use waste of resource, thus reduces the cost of whole packaging material for food.And directly use heat-sealing polyester film can also effectively prevent general thin because of the existence of compound tense residual solvent, and then affect packaged food hygiene and the health affecting people, therefore biaxially oriented polyester film of the present invention can direct heat sealing performance, raising people are produced and living standard significant.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail:
Embodiment 1
The polyester film that can directly seal, comprises ABC three-decker, and described B layer is intermediate core layer, and material is that PET surpasses bright PET chips; A layer is top layer heat-sealable layer, and material is copolymerization PETG polyester slice; C layer is anti-stick interconnect layer, and material comprises the section of PET antiblocking agent masterbatch and surpasses bright PET chips with PET.
The anti-stick interconnect layer of C layer, material has the component of following mass percent: the PET antiblocking agent masterbatch section of 30% ~ 60% and 40% ~ 70%PET surpass bright PET chips.
B layer thickness accounts for 70% ~ 80%, A layer thickness and accounts for 10% ~ 20%, C layer thickness and account for 10% ~ 20%.
The copolymerization PETG polyester slice of A layer top layer heat-sealable layer is by dimethyl terephthalate (DMT) DMT, ethylene glycol EG, silica SiO
2with 1,4-CHDM CHDM totally four kinds of monomers product of ester-interchange method polycondensation.
In the anti-stick interconnect layer of C layer, the section of PET antiblocking agent masterbatch is for containing silica SiO
2polyester slice, silica SiO
2particle diameter is 2 ~ 3um, and content is 3000ppm.
The polyester film manufacture craft that can directly seal, comprises the polyester film described in claim 1-5, comprises the steps:
A, the A layer copolymerization PETG polyester slice of preparation, B layer PET surpassed bright PET chips and C layer PET surpasses bright PET chips and the section of PET antiblocking agent masterbatch, send into three-layer co-extruded biaxial tension equipment respectively, wherein A layer copolymerization PETG polyester slice sends into subsidiary extruder---double screw extruder, B layer PET surpasses bright PET chips and sends into main extruder---single screw extrusion machine, and C layer PET surpasses bright PET chips and subsidiary extruder---double screw extruder is sent in the section of PET antiblocking agent masterbatch;
B, ABC tri-layers of polyester slice are extruded melting at 240 ~ 280 DEG C, melt generates PET sheet through less than 30 DEG C cooling slabs;
C, the PET sheet of casting are through 80 ~ 100 DEG C of preheating longitudinal stretchings and less than 35 DEG C temperature cooling and shapings;
PET sheet after d, sizing is again by 86 ~ 110 DEG C of preheating cross directional stretch and 180 ~ 200 DEG C of sizing crystallization treatment;
E, eventually pass traction removing slitter edge, sided corona treatment, detection thickness carry out again rolling batch the one side of obtained thickness 15um ~ 30um can the polyester film of direct heat sealing.
B layer is intermediate core layer, by main extruder---single screw extrusion machine is extruded; A layer is top layer heat-sealable layer, by subsidiary extruder---double screw extruder is extruded; C layer is anti-stick interconnect layer, by subsidiary extruder---double screw extruder is extruded, and A layer subsidiary extruder, B layer main extruder, C layer subsidiary extruder polyester slice are extruded mass ratio and be: 10 ~ 20:65 ~ 80:10 ~ 20.
In the heat-sealable layer of A layer top layer, copolymerization PETG polyester slice preparation method is:
A, by 100 parts of dimethyl terephthalate (DMT) DMT, 25 ~ 35 parts of ethylene glycol EG, 1 ~ 5 part of silica SiO
2be uniformly mixed after sending into polymeric kettle with 20 ~ 30 parts of Isosorbide-5-Nitrae cyclohexanedimethanol CHDM;
B, add the antimony oxide Sb of 2 ~ 4 parts again
2o
3with the phosphorous acid triphen C of 2 ~ 4 parts
18h
15o
3p is as catalyst and stabilizing agent;
C, polymeric kettle is airtight after, control polymerization temperature in the kettle and pressure at 170 ~ 210 DEG C and 500 ~ 700pa under, use nitrogen N
2carry out 0.5 ~ 1.5h ester exchange reaction;
D, then will be warming up to 240 ~ 280 DEG C in polymeric kettle, polymeric kettle is vacuumized, then under the effect of composite catalyst, carries out polycondensation reaction 2 ~ 4h in high vacuum;
E, discharging, cooling, pelletizing, obtained copolymerization PETG polyester slice.
In step a, be first 20 ~ 30 parts of Isosorbide-5-Nitrae cyclohexanedimethanol CHDM and mass content by mass content be 1 ~ 5 part of silica SiO
2join 25 ~ 35 parts of ethylene glycol EG, dispersed with stirring, then through supersonic oscillations dispersion, after making each composition high speed dispersion homogenizing, send into polymeric kettle; Then add 100 parts of dimethyl terephthalate (DMT) DMT to be uniformly mixed.
In step c, after polymeric kettle is airtight, carry out ester exchange reaction nitrogen N
2carry out displacement 3 times, after ester exchange reaction terminates, reclaim unnecessary ethylene glycol EG, in steps d, composite catalyst is: the composition of titanium dioxide, silica, compound, zinc acetate and compd A containing molybdenum, and compd A takes from any one in manganese acetate or manganese chloride or both mixtures.The advantage of this catalyst is that course of reaction side reaction is few, and the polyester obtained has better color and luster.
Embodiment 2
A preparation method for the polyester film that can directly seal, by weight: to be the Isosorbide-5-Nitrae cyclohexanedimethanol CHDM of 22 parts and mass content by mass content the be silica SiO of 3 parts
2join in the ethylene glycol EG of 23 parts, dispersed with stirring, then through high speed dispersion homogenizing, after adopting supersonic oscillations dispersion, send in main reaction systematic polymerization still; Add 100 parts of dimethyl terephthalate (DMT) DMT to be uniformly mixed, then add antimony oxide and the triphenyl phosphite of 2 parts (PTA weight), after airtight, use nitrogen N
2replace 3 times.In still, pressure is under 600Pa, is warming up to 180 DEG C, esterification 0.8h, after esterification terminates, reclaims unnecessary ethylene glycol EG; Then 260 DEG C are warming up to, polyase 13 .4h discharging, cooling, pelletizing under vacuumized conditions, obtained copolymerization PETG polyester slice.
By the copolymerization PETG polyester slice of preparation by mass percentage 100% measured by accurate weighing-appliance after join auxiliary double screw extruder and carry out extruding (A layer); The pulp furnish of main extruder (B layer) is 100% surpass bright PET chips by mass percentage, and raw material is extruded by sending into main extruder after accurate measurement; The pulp furnish of auxiliary double screw extruder (C layer) is 60% surpass bright PET chips and 40% antiblocking agent masterbatch polyester slice by mass percentage, and raw material is extruded by sending into extruder after accurate measurement mixing.The mass ratio of main extruder and two auxiliary double screw extruders is 10:75:15,20um film A layer heat-sealable layer thickness be 2.0um, C layer anti-sticking layer thickness is 3.0um.Polyester slice is melt extruded at 270 DEG C, melt becomes sheet material through less than 30 DEG C cooling slabs, longitudinal stretching is carried out to the PET sheet of casting, longitudinal stretching preheating, draft temperature is 90 DEG C, stretching ratio is 3.5 times, after longitudinal stretching below 35 DEG C temperature cooling and shaping, then cross directional stretch is carried out, cross directional stretch preheating, draft temperature is 110 DEG C, stretching ratio is 3.7 times, at 190 DEG C of temperature, shaping film crystallization treatment is carried out respectively after biaxial tension, cool under 80 DEG C and normal temperature wind again, the film cooled down is by Traction Station flash trimming, corona, detect the last rolling such as thickness obtain gross thickness be 20um can direct heat-sealable polyester film, this can heat-sealable polyester film top layer (A layer) be directly heat-sealable layer, containing 100% copolymerization PETG polyester slice, intermediate layer (B layer) is containing 100% surpassing bright PET chips, anti-stick top layer (C layer) is containing 60% surpassing bright PET chips and 40% antiblocking agent masterbatch polyester slice.
Embodiment 3
The difference of the present embodiment and embodiment 2 is that the mass ratio of main extruder and two auxiliary double screw extruder extruded materials be 15:70:15,20um film A layer heat-sealable layer thickness be 3.0um, C layer anti-sticking layer thickness is 3.0um.
Embodiment 4
The difference of the present embodiment and embodiment 2 is that the mass ratio of main extruder and two auxiliary double screw extruder extruded materials be 20:65:15,20um film A layer heat-sealable layer thickness be 4.0um, C layer anti-sticking layer thickness is 3.0um.
The present invention obtain can the correlated performance of direct heat-sealable polyester film according to ASTM D standard, adopt German MAHR company model HSG-C to seal measuring instrument; The haze meter adopting German BYK-Gardner GmbH company to produce, Grossmeters carry out the measurement of mist degree and glossiness; The tensilometer adopting company of LLOYD company of Britain to produce is measured hot strength; PX (J)-1 type baking oven adopting domestic Yancheng chemical fibre equipment factory to produce is measured percent thermal shrinkage
Table 1: adopt the synthesis copolymerization PETG polyester slice of good cost performance to produce same thin film thickness and production technology, different heat-sealable layer thickness structure distribution production can direct heat-sealable polyester thin-film examples comparison sheet;
Table 1
Embodiment 5
The preparation method of a kind of polyester film that can directly seal of the present invention, by weight:
(1), to be the Isosorbide-5-Nitrae cyclohexanedimethanol CHDM of 28 parts and mass content by mass content the be silica SiO of 3 parts
2join in the ethylene glycol EG of 32 parts, dispersed with stirring, then after high speed dispersion homogenizing (supersonic oscillations dispersion), send into main reaction system (polymeric kettle); Add 100 parts of dimethyl terephthalate (DMT) DMT to be uniformly mixed, then add antimony oxide and the triphenyl phosphite of 2 parts (PTA weight), after airtight, use N
2replace 3 times.In still, pressure is under 650Pa, is warming up to 190 DEG C, esterification 1.5h, after esterification terminates, reclaims unnecessary ethylene glycol EG; Then 260 DEG C are warming up to, polyase 13 .2h discharging, cooling, pelletizing under vacuumized conditions, obtained copolymerization PETG polyester slice.
(2), by the copolymerization PETG polyester slice of preparation by mass percentage 100% measured by accurate weighing-appliance after join auxiliary double screw extruder and carry out extruding (A layer); The pulp furnish of main extruder (B layer) is 100% surpass bright PET chips by mass percentage, and raw material is extruded by sending into main extruder after accurate measurement; The pulp furnish of auxiliary double screw extruder (C layer) is 60% surpass bright PET chips and 40% antiblocking agent masterbatch polyester slice by mass percentage, and raw material is extruded by sending into extruder after accurate measurement mixing.The mass ratio that main extruder and two auxiliary double screw extruder materials are extruded is 15:75:15,18um film A layer heat-sealable layer thickness be 2.7um, C layer anti-sticking layer thickness is 2.7um.For polyester slice is extruded melting at 240 ~ 280 DEG C, melt becomes sheet material through less than 30 DEG C cooling slabs, longitudinal stretching is carried out to the PET sheet of casting, longitudinal stretching preheating, draft temperature is 100 DEG C, stretching ratio is 3.5 times, after longitudinal stretching below 35 DEG C temperature cooling and shaping, then cross directional stretch is carried out, cross directional stretch preheating, draft temperature is 89 DEG C, stretching ratio is 3.7 times, at 178 DEG C of temperature, shaping film crystallization treatment is carried out respectively after biaxial tension, cool under 80 DEG C and normal temperature wind again, the film cooled down is by Traction Station flash trimming, corona, detect the last rolling such as thickness obtain gross thickness be 18um can direct heat-sealable polyester film, this can heat-sealable polyester film top layer (A layer) be directly heat-sealable layer, containing 100% copolymerization PETG polyester slice, intermediate layer (B layer) is containing 100% surpassing bright PET chips, anti-stick top layer (C layer) is containing 60% surpassing bright PET chips and 40% antiblocking agent masterbatch polyester slice.
Embodiment 6
The difference of the present embodiment and embodiment 5 be to prepare gross thickness be 18um can direct heat-sealable polyester film, mass ratio extruded by the material of main extruder and two auxiliary double screw extruders is 15:75:15,18um film A layer heat-sealable layer thickness is 2.7um, C layer anti-sticking layer thickness is 2.7um.
Embodiment 7
The difference of the present embodiment and embodiment 5 be to prepare gross thickness be 25um can direct heat-sealable polyester film, mass ratio extruded by the material of main extruder and two auxiliary double screw extruders is 15:75:15,25um film A layer heat-sealable layer thickness is 3.75um, C layer anti-sticking layer thickness is 3.75um.
Embodiment 8
The difference of the present embodiment and embodiment 5 be to prepare gross thickness be 30um can direct heat-sealable polyester film, mass ratio extruded by the material of main extruder and two auxiliary double screw extruders is 15:75:15,30um film A layer heat-sealable layer thickness is 4.5um, C layer anti-sticking layer thickness is 4.5um.
Table 2: adopt the synthesis copolymerization PETG polyester of good cost performance to cut and produce same structure mass ratio layering and same production technology, different film thickness is produced can direct heat-sealable polyester thin-film examples comparison sheet,
Table 2
Embodiment 9
The preparation method of a kind of polyester film that can directly seal of the present invention, by weight:
Preparation 20um film, the quality of materials of main extruder and two auxiliary double screw extruders is than being 3.0um for 15:70:15,20um film A layer heat-sealable layer thickness, and C layer anti-sticking layer thickness is 3.0um.
(1), by mass content is 21 parts 1,4 cyclohexanedimethanol CHDM and mass content are that the silica SiO2 of 1 part joins in the ethylene glycol EG of 34 parts, dispersed with stirring, again after high speed dispersion homogenizing (supersonic oscillations dispersion), send into main reaction system (polymeric kettle); Add 100 parts of dimethyl terephthalate (DMT) DMT to be uniformly mixed, then add antimony oxide and 4 portions of triphenyl phosphites of 4 parts (PTA weight), airtight rear N2 replaces 3 times.In still, pressure is under 700Pa, is warming up to 176 DEG C, esterification 1.2h, after esterification terminates, reclaims unnecessary ethylene glycol EG; Then be warming up to 276 DEG C, under vacuumized conditions, be polymerized 4h discharging, cooling, pelletizing, obtained copolymerization PETG polyester slice.
(2), by the copolymerization PETG polyester slice of preparation by mass percentage 100% measured by accurate weighing-appliance after join auxiliary double screw extruder and carry out extruding (A layer); The pulp furnish of main extruder (B layer) is 100% surpass bright PET chips by mass percentage, and raw material is extruded by sending into main extruder after accurate measurement; The pulp furnish of auxiliary double screw extruder (C layer) is 60% surpass bright PET chips and 40% antiblocking agent masterbatch polyester slice by mass percentage, and raw material is extruded by sending into extruder after accurate measurement mixing.The quality of materials of main extruder and two auxiliary double screw extruders is 3.0um than being 15:70:15,20um film A layer heat-sealable layer thickness, and C layer anti-sticking layer thickness is 3.0um.Special process production process is that polyester slice is extruded melting at 220 ~ 240 DEG C, melt becomes sheet material through less than 28 DEG C cooling slabs, longitudinal stretching is carried out to the PET sheet of casting, longitudinal stretching preheating, draft temperature is 60 ~ 90 DEG C, stretching ratio is 3.5 times, after longitudinal stretching below 35 DEG C temperature cooling and shaping, then cross directional stretch is carried out, cross directional stretch preheating, draft temperature is 65 ~ 95 DEG C, stretching ratio is 3.7 times, at 160 DEG C ~ 180 DEG C temperature, shaping film crystallization treatment is carried out respectively after biaxial tension, cool under 60 DEG C and normal temperature wind again, the film cooled down is by Traction Station flash trimming, corona, detect the last rolling such as thickness obtain gross thickness be 20um can direct heat-sealable polyester film, this can heat-sealable polyester film top layer (A layer) be directly heat-sealable layer, containing 100% copolymerization PETG polyester slice, intermediate layer (B layer) is containing 100% surpassing bright PET chips, anti-stick top layer (C layer) is containing 60% surpassing bright PET chips and 40% antiblocking agent masterbatch polyester slice.
Embodiment 10
The difference of the present embodiment and embodiment 9 is: when preparing 20um film, and mass ratio extruded by the material of main extruder and two auxiliary double screw extruders be 15:70:15,20um film A layer heat-sealable layer thickness be 3.0um, C layer anti-sticking layer thickness is 3.0um.
Embodiment 11
The preparation method of a kind of polyester film that can directly seal of the present invention, by weight:
(1), to be the Isosorbide-5-Nitrae cyclohexanedimethanol CHDM of 25 parts and mass content by mass content the be silica SiO of 1 part
2join in the ethylene glycol EG of 30 parts, dispersed with stirring, then after high speed dispersion homogenizing (supersonic oscillations dispersion), send into main reaction system (polymeric kettle); Add 100 parts of dimethyl terephthalate (DMT) DMT to be uniformly mixed, then add antimony oxide and the triphenyl phosphite of 2 parts (PTA weight), airtight rear N2 replaces 3 times.In still, pressure is under 500 ~ 700Pa, is warming up to 170 ~ 210 DEG C, esterification 0.5 ~ 1.5h, after esterification terminates, reclaims unnecessary ethylene glycol EG; Then be warming up to 240 ~ 280 DEG C, under vacuumized conditions, be polymerized 2 ~ 4h discharging, cooling, pelletizing, obtained copolymerization PETG polyester slice.
(2), by the copolymerization PETG polyester slice of preparation by mass percentage 100% measured by accurate weighing-appliance after join auxiliary double screw extruder and carry out extruding (A layer); The pulp furnish of main extruder (B layer) is 100% surpass bright PET chips by mass percentage, and raw material is extruded by sending into main extruder after accurate measurement; The pulp furnish of auxiliary double screw extruder (C layer) is 60% surpass bright PET chips and 40% antiblocking agent masterbatch polyester slice by mass percentage, and raw material is extruded by sending into extruder after accurate measurement mixing.The mass ratio of main extruder and two auxiliary double screw extruders is 15:70:15,20um film A layer heat-sealable layer thickness be 3.0um, C layer anti-sticking layer thickness is 3.0um.Special process production process is that polyester slice is extruded melting at 260 ~ 280 DEG C, melt becomes sheet material through less than 28 DEG C cooling slabs, longitudinal stretching is carried out to the PET sheet of casting, longitudinal stretching preheating, draft temperature is 70 ~ 115 DEG C, stretching ratio is 3.5 times, after longitudinal stretching below 35 DEG C temperature cooling and shaping, then cross directional stretch is carried out, cross directional stretch preheating, draft temperature is 86 ~ 125 DEG C, stretching ratio is 3.7 times, at 200 DEG C ~ 220 DEG C temperature, shaping film crystallization treatment is carried out respectively after biaxial tension, cool under 60 DEG C and normal temperature wind again, the film cooled down is by Traction Station flash trimming, corona, detect the last rolling such as thickness obtain gross thickness be 20um can direct heat-sealable polyester film, this can heat-sealable polyester film top layer (A layer) be directly heat-sealable layer, containing 100% copolymerization PETG polyester slice, intermediate layer (B layer) is containing 100% surpassing bright PET chips, anti-stick top layer (C layer) is containing 60% surpassing bright PET chips and 40% antiblocking agent masterbatch polyester slice.
The present invention obtain can the correlated performance of direct heat-sealable polyester film according to ASTM D standard, adopt German MAHR company model HSG-C to seal measuring instrument; The haze meter adopting German BYK-Gardner GmbH company to produce, Grossmeters carry out the measurement of mist degree and glossiness; The tensilometer adopting company of LLOYD company of Britain to produce is measured hot strength; PX (J)-1 type baking oven adopting domestic Yancheng chemical fibre equipment factory to produce is measured percent thermal shrinkage.
Table 3: adopt the synthesis copolymerization PETG polyester slice of good cost performance, produce same composition of raw materials and same thin film thickness, different production technologies can direct heat-sealable polyester thin-film examples comparison sheet:
Table 3
In a word, the foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to the covering scope of patent of the present invention.
Claims (8)
1. the polyester film that can directly seal, comprises ABC three-decker, it is characterized in that: described B layer is intermediate core layer, and material is that PET surpasses bright PET chips; A layer is top layer heat-sealable layer, and material is copolymerization PETG polyester slice; C layer is anti-stick interconnect layer, and material comprises the section of PET antiblocking agent masterbatch and surpasses bright PET chips with PET; The anti-stick interconnect layer of C layer, material has the component of following mass percent: the PET antiblocking agent masterbatch section of 30% ~ 60% and 40% ~ 70%PET surpass bright PET chips.
2. a kind of polyester film that can directly seal according to claim 1, is characterized in that: described B layer thickness accounts for 70% ~ 80%, A layer thickness and accounts for 10% ~ 20%, C layer thickness and account for 10% ~ 20%.
3. a kind of polyester film that can directly seal according to claim 1, is characterized in that: the copolymerization PETG polyester slice of described A layer top layer heat-sealable layer is by dimethyl terephthalate (DMT) DMT, ethylene glycol EG, silica SiO
2with 1,4-CHDM CHDM totally four kinds of monomers product of ester-interchange method polycondensation.
4. a kind of polyester film that can directly seal according to claim 1, is characterized in that: in the described anti-stick interconnect layer of C layer, and the section of PET antiblocking agent masterbatch is for containing silica SiO
2polyester slice, silica SiO
2particle diameter is 2 ~ 3um, and content is 3000ppm.
5. a manufacture craft for the polyester film that can directly seal as described in any one of claim 1-4, is characterized in that: comprise the steps:
A, the A layer copolymerization PETG polyester slice of preparation, B layer PET surpassed bright PET chips and C layer PET surpasses bright PET chips and the section of PET antiblocking agent masterbatch, send into three-layer co-extruded biaxial tension equipment respectively, wherein A layer copolymerization PETG polyester slice sends into subsidiary extruder---double screw extruder, B layer PET surpasses bright PET chips and sends into main extruder---single screw extrusion machine, and C layer PET surpasses bright PET chips and subsidiary extruder---double screw extruder is sent in the section of PET antiblocking agent masterbatch;
B, ABC tri-layers of polyester slice are extruded melting at 240 ~ 280 DEG C, melt generates PET sheet through less than 30 DEG C cooling slabs;
C, the PET sheet of casting are through 80 ~ 100 DEG C of preheating longitudinal stretchings and less than 35 DEG C temperature cooling and shapings;
PET sheet after d, sizing is again by 86 ~ 110 DEG C of preheating cross directional stretch and 180 ~ 200 DEG C of sizing crystallization treatment;
E, eventually pass traction removing slitter edge, sided corona treatment, detection thickness carry out again rolling batch the one side of obtained thickness 15um ~ 30um can the polyester film of direct heat sealing;
In the heat-sealable layer of A layer top layer, copolymerization PETG polyester slice preparation method is:
A, by 100 parts of dimethyl terephthalate (DMT) DMT, 25 ~ 35 parts of ethylene glycol EG, 1 ~ 5 part of silica SiO
2be uniformly mixed after sending into polymeric kettle with 20 ~ 30 parts of Isosorbide-5-Nitrae cyclohexanedimethanol CHDM;
B, add the antimony oxide Sb of 2 ~ 4 parts again
2o
3with the phosphorous acid triphen C of 2 ~ 4 parts
18h
15o
3p is as catalyst and stabilizing agent;
C, polymeric kettle is airtight after, control polymerization temperature in the kettle and pressure at 170 ~ 210 DEG C and 500 ~ 700pa under, use nitrogen N
2carry out 0.5 ~ 1.5h ester exchange reaction;
D, then will be warming up to 240 ~ 280 DEG C in polymeric kettle, polymeric kettle is vacuumized, then under the effect of composite catalyst, carries out polycondensation reaction 2 ~ 4h in high vacuum;
E, discharging, cooling, pelletizing, obtained copolymerization PETG polyester slice; Composite catalyst is the composition containing titanium dioxide, silica, compound, zinc acetate and compd A containing molybdenum.
6. a kind of polyester film manufacture craft that can directly seal according to claim 5, is characterized in that: described B layer is intermediate core layer, by main extruder---single screw extrusion machine is extruded; A layer is top layer heat-sealable layer, by subsidiary extruder---double screw extruder is extruded; C layer is anti-stick interconnect layer, by subsidiary extruder---double screw extruder is extruded, and A layer subsidiary extruder, B layer main extruder, C layer subsidiary extruder polyester slice are extruded mass ratio and be: 10 ~ 20:65 ~ 80:10 ~ 20.
7. a kind of polyester film manufacture craft that can directly seal according to claim 6, is characterized in that: in described step a, be first 20 ~ 30 parts of Isosorbide-5-Nitrae cyclohexanedimethanol CHDM and mass content by mass content is 1 ~ 5 part of silica SiO
2join 25 ~ 35 parts of ethylene glycol EG, dispersed with stirring, then through supersonic oscillations dispersion, after making each composition high speed dispersion homogenizing, send into polymeric kettle; Then add 100 parts of dimethyl terephthalate (DMT) DMT to be uniformly mixed.
8. a kind of polyester film manufacture craft that can directly seal according to claim 6, is characterized in that: in described step c, carries out ester exchange reaction nitrogen N after polymeric kettle is airtight
2carry out displacement 3 times, after ester exchange reaction terminates, reclaim unnecessary ethylene glycol EG, in steps d, composite catalyst is: the composition of titanium dioxide, silica, compound, zinc acetate and compd A containing molybdenum, and compd A takes from any one in manganese acetate or manganese chloride or both mixtures.
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