CN102873954A - Polyester film capable of being subjected to heat seal directly and preparation method - Google Patents
Polyester film capable of being subjected to heat seal directly and preparation method Download PDFInfo
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- CN102873954A CN102873954A CN2012103757480A CN201210375748A CN102873954A CN 102873954 A CN102873954 A CN 102873954A CN 2012103757480 A CN2012103757480 A CN 2012103757480A CN 201210375748 A CN201210375748 A CN 201210375748A CN 102873954 A CN102873954 A CN 102873954A
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- 229920006267 polyester film Polymers 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000010410 layer Substances 0.000 claims abstract description 208
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 122
- 229920000728 polyester Polymers 0.000 claims abstract description 68
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 claims abstract description 37
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 239000012792 core layer Substances 0.000 claims abstract description 8
- 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
- 239000000463 material Substances 0.000 claims description 39
- 238000007334 copolymerization reaction Methods 0.000 claims description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 27
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 13
- 239000004408 titanium dioxide Substances 0.000 claims description 13
- 150000002148 esters Chemical class 0.000 claims description 12
- 238000007493 shaping process Methods 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- ORLQHILJRHBSAY-UHFFFAOYSA-N [1-(hydroxymethyl)cyclohexyl]methanol Chemical class OCC1(CO)CCCCC1 ORLQHILJRHBSAY-UHFFFAOYSA-N 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 7
- 230000010355 oscillation Effects 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
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 6
- 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
- 239000004246 zinc acetate Substances 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 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
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 3
- 239000011162 core material Substances 0.000 claims description 3
- 238000003851 corona treatment 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
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 75
- 229920000139 polyethylene terephthalate Polymers 0.000 abstract description 75
- -1 polyethylene terephthalate Polymers 0.000 abstract 2
- 241001354243 Corona Species 0.000 abstract 1
- 239000002981 blocking agent Substances 0.000 abstract 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 1
- 239000010408 film Substances 0.000 description 31
- 239000002994 raw material Substances 0.000 description 18
- 238000007789 sealing Methods 0.000 description 12
- 238000005259 measurement Methods 0.000 description 10
- 230000032050 esterification Effects 0.000 description 8
- 238000005886 esterification reaction Methods 0.000 description 8
- 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
- 230000008569 process Effects 0.000 description 5
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical class OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 4
- 229910000410 antimony oxide Inorganic materials 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 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
- 230000036541 health Effects 0.000 description 3
- 239000005022 packaging material Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 230000002950 deficient 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
- 239000000126 substance Substances 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
- 238000010438 heat treatment Methods 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
Landscapes
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to a polyester film and a preparation method thereof and particularly discloses a polyester film capable of being subjected to heat seal direction and a preparation method. The polyester film comprises a layer A, a layer B and a layer C, wherein the layer B is a middle core layer and made of a PET (polyethylene terephthalate) ultra-glazed polyester slice, the layer A is a surface heat-seal layer and made of a copolymerized PETG (polyethylene terephthalate glycol) polyester slice, and the layer C is an anti-blocking layer and made of a PET anti-blocking agent master batch slice and a PET ultra-glazed polyester slice. The preparation method includes steps of preparing corresponding polyester slices, extruding and drawing via an extruder, forming with cooling, crystallizing, drawing to remove scrap edges, treating coronas, detecting the thickness and the like.
Description
Technical field
The present invention relates to polyester film and preparation method thereof, relate in particular 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.The PET(polyester) is universally acknowledged environment-friendly and green material.And the polyester film that can directly seal that process modification raw material and special producing technique are made is 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 can't seal defective certainly, and in order to be used for the occasion of heat-sealing, it need to carry out loaded down with trivial details and expensive compound working procedure with other resins usually, thereby has greatly limited its application.
Because common BOPET mylar do not possess heat sealability, have to adopt the problem that BOPET and CPP or the compound method of PE film is solved packaging seal.For example, adopt BOPET/CPP or the complex methods such as BOPET/PE or BOPET/VMCPP, packing cost is improved greatly, and because the existence of compound tense residual solvent, thereby can affect the health of packaged food.
Summary of the invention
The present invention is directed to common mylar product in the prior art, existence can't seal defective certainly, in order to be used for the occasion of heat-sealing, it need to carry out loaded down with trivial details and expensive compound working procedure with other resins usually, provide a kind of and can under 120 degree temperature, carry out heat sealing, not only saved the loaded down with trivial details and expensive compound working procedure that conventional polyester film and other resins carry out, saved the use waste of resource, also reduce simultaneously the cost of whole packaging material for food, and more a kind of polyester film that can directly seal and the preparation method of health.
In order to solve the problems of the technologies described above, the present invention is solved by following technical proposals:
A kind of polyester film that can directly seal comprises the ABC three-decker, and described B layer is intermediate core layer, and material is the super bright PET chips of PET; The A layer is the top layer heat-sealable layer, and material is copolymerization PETG polyester slice; The C layer is anti-adhering layer, and material comprises the section of PET antiblocking agent masterbatch and the super bright PET chips of PET.In polyester slice, " light is arranged greatly ", " half delustring " and " light is arranged " for be titanium dioxide (TiO2) content in the polyester slice." light is arranged greatly " polyester slice also is 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 " light arranged " 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 the B layer is intermediate core layer, is extruded by the main extruder single screw extrusion machine, and extruded material is the super bright PET chips of 100%PET; The A layer is the top layer heat-sealable layer, is extruded by auxiliary extruder double-screw extruder, and extruded material is 100% copolymerization PETG polyester slice; The C layer is anti-adhering layer, is extruded by auxiliary extruder double-screw extruder, and extruded material has the component of following mass percent: the section 30%～60% of PET antiblocking agent masterbatch and the super bright PET chips of 40%～70%PET.The 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 C layer is anti-adhering layer, and material has the component of following mass percent: 30%～60% the section of PET antiblocking agent masterbatch and the super bright PET chips of 40%～70%PET.
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, be by dimethyl terephthalate (DMT) (DMT), ethylene glycol (EG), silica (SiO2) and 1,4-CHDM (CHDM) totally four kinds of monomers with the product of ester-interchange method polycondensation.
As preferably, in the anti-adhering layer of described C layer, PET antiblocking agent masterbatch is cut into slices as containing silica (SiO2) polyester slice, and silica (SiO2) particle diameter is 2～3um, and content is 3000ppm.
A kind of polyester film manufacture craft that can directly seal comprises the described polyester film of claim 1-5, comprises the steps:
A, A layer copolymerization PETG polyester slice, the super bright PET chips of B layer PET and the super bright PET chips of C layer PET and the PET antiblocking agent masterbatch of preparation are cut into slices, send into respectively three-layer co-extruded biaxial tension equipment, wherein A layer copolymerization PETG polyester slice is sent into auxiliary extruder---double screw extruder, the super bright PET chips of B layer PET is sent into main extruder---single screw extrusion machine, and auxiliary extruder---double screw extruder is sent in the super bright PET chips of C layer PET and the section of PET antiblocking agent masterbatch;
B, ABC three strata esters sections is extruded melting at 240～280 ℃, melt generates the PET sheet material through the slab of cooling below 30 ℃;
C, the PET sheet material cast are through 80～100 ℃ of preheating longitudinal stretchings and 35 ℃ of following temperature cooling and shapings;
PET sheet material after d, the typing is again by 86～110 ℃ of preheating cross directional stretch and 180～200 ℃ of typing crystallization treatment;
But e, remove slitter edge, sided corona treatment, detection thickness and carry out again the polyester film that the single face direct heat involution that makes thickness 15um～30um is batched in rolling finally by crossing traction.
As preferably, described B layer is intermediate core layer, by main extruder---and single screw extrusion machine is extruded; The A layer is the top layer heat-sealable layer, by auxiliary extruder---double screw extruder is extruded; The C layer is anti-adhering layer, and by auxiliary extruder---double screw extruder is extruded, the A layer assists extruder, B layer main extruder, the auxiliary extruder polyester slice of C layer to extrude mass ratio and be: 10～20:65～80:10～20.
As preferably, copolymerization PETG polyester slice preparation method is in the heat-sealable layer of described A layer top layer:
A, mix after 100 parts of dimethyl terephthalate (DMT)s (DMT), 25～35 parts of ethylene glycol (EG), 1～5 part of silica (SiO2) and 20～30 parts of Isosorbide-5-Nitrae cyclohexanedimethanols (CHDM) are sent into polymeric kettle;
B, add the phosphorous acid triphen (C18H15O3P) of 2～4 parts antimony oxide (Sb2O3) and 2～4 parts as catalyst and stabilizing agent again;
C, polymeric kettle is airtight after, control polymerization temperature in the kettle and pressure carry out 0.5～1.5h ester exchange reaction with nitrogen (N2) under 170～210 ℃ of lower and 500～700pa;
D, then be warming up to 240～280 ℃ in the polymeric kettle, polymeric kettle is vacuumized, then under the effect of composite catalyst, carry out polycondensation reaction 2～4h in the high vacuum;
E, discharging, cooling, pelletizing make copolymerization PETG polyester slice.
As preferably, among the described step a, it is 20～30 part 1 with mass content at first, 4 cyclohexanedimethanols (CHDM) and mass content are that 1～5 part of silica (SiO2) joins 25～35 parts of ethylene glycol (EG), dispersed with stirring, disperse through supersonic oscillations again, so that after each composition high speed dispersion homogenizing, send into polymeric kettle; Then adding 100 parts of dimethyl terephthalate (DMT)s (DMT) mixes.
As preferably, among the described step c, carrying out ester exchange reaction after polymeric kettle is airtight replaces 3 times with nitrogen (N2), after ester exchange reaction finishes, reclaim unnecessary ethylene glycol (EG), in the steps d, composite catalyst is: the composition of titanium dioxide, silica, the compound that contains molybdenum, zinc acetate and compd A, compd A are taken from any in manganese acetate or the manganese chloride or both mixtures.Composite catalyst composition composite catalyst is the composition that contains titanium dioxide, silica, contains compound, zinc acetate and the compd A of molybdenum.Wherein the weight ratio of titanium dioxide and silica is 100: (6～9.5); Titanium dioxide is 100 with the weight ratio that contains the compound of 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 are 100: (5～115), and the weight ratio of titanium dioxide and zinc acetate and compd A total amount is 100: (50～120).The compound that contains molybdenum is taken from any in the sulfide of the oxide of molybdenum or molybdenum or both mixtures; Compd A is taken from any in manganese acetate or the manganese chloride or both mixtures.The advantage of this catalyst is that the course of reaction side reaction is few, and the polyester that obtains has better color and luster.
Of the present inventionly can directly seal existing Isosorbide-5-Nitrae cyclohexanedimethanol (CHDM) in the polyester film system, interpolation antiblocking agent (SiO2) is arranged again, then adopt the two-step method preparation can directly seal polyester film.For the PETG copolyester that contains silica (SiO2) particle, for the film blocking that prevents from producing, must in the film surface layer, add a certain amount of SiO2 particle, added the SiO2 particle, can reduce to a certain extent heat-seal strength.Can be by being that the proportioning of Isosorbide-5-Nitrae cyclohexanedimethanol (CHDM) and the ratio of SiO2 particle adjust to the 3rd monomer in the PETG preparation process, namely satisfy heat sealability and require to prevent that again the heat-sealing polyester film from producing adhesion in wrapup procedure to produce.And must adjust in production structure for the polyester film that can directly seal, we adopt three-layer co-extruded stretch processes, control film master, auxiliary extruder ratio, control thin film crystallization speed, by stretching, typing, and last handling process, suit and the rational polyester heat sealing film of SiO2 opening agent content to make heat-sealing thickness, simultaneously in order to control the production stability of film, we are to longitudinal stretching, the ratio of cross directional stretch, temperature and air quantity, the concrete technology parameters such as infrared heating power are adjusted, finally to obtain the polyester film product that can directly seal of target call.
The present invention can directly seal polyester film by preparation and compare with the conventional polyester film, except the every good characteristic that possesses the conventional polyester film, has had especially and can spend the function of heat sealing under the temperature 120.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 has saved the use waste of resource, thereby reduces the cost of whole packaging material for food.And directly use the heat-sealing polyester film can also prevent effectively that general thin is because of the existence of compound tense residual solvent, and then affect packaged food hygiene and affect people's health, therefore the direct heat sealing performance of biaxially oriented polyester film of the present invention is significant to improving people's production and living standard.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is described in further detail:
Embodiment 1
A kind of polyester film that can directly seal comprises the ABC three-decker, and described B layer is intermediate core layer, and material is the super bright PET chips of PET; The A layer is the top layer heat-sealable layer, and material is copolymerization PETG polyester slice; The C layer is anti-adhering layer, and material comprises the section of PET antiblocking agent masterbatch and the super bright PET chips of PET.
The anti-adhering layer of C layer, material has the component of following mass percent: 30%～60% the section of PET antiblocking agent masterbatch and the super bright PET chips of 40%～70%PET.
The 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, be by dimethyl terephthalate (DMT) (DMT), ethylene glycol (EG), silica (SiO2) and 1,4-CHDM (CHDM) totally four kinds of monomers with the product of ester-interchange method polycondensation.
In the anti-adhering layer of C layer, PET antiblocking agent masterbatch is cut into slices as containing silica (SiO2) polyester slice, and silica (SiO2) particle diameter is 2～3um, and content is 3000ppm.
A kind of polyester film manufacture craft that can directly seal comprises the described polyester film of claim 1-5, comprises the steps:
A, A layer copolymerization PETG polyester slice, the super bright PET chips of B layer PET and the super bright PET chips of C layer PET and the PET antiblocking agent masterbatch of preparation are cut into slices, send into respectively three-layer co-extruded biaxial tension equipment, wherein A layer copolymerization PETG polyester slice is sent into auxiliary extruder---double screw extruder, the super bright PET chips of B layer PET is sent into main extruder---single screw extrusion machine, and auxiliary extruder---double screw extruder is sent in the super bright PET chips of C layer PET and the section of PET antiblocking agent masterbatch;
B, ABC three strata esters sections is extruded melting at 240～280 ℃, melt generates the PET sheet material through the slab of cooling below 30 ℃;
C, the PET sheet material cast are through 80～100 ℃ of preheating longitudinal stretchings and 35 ℃ of following temperature cooling and shapings;
PET sheet material after d, the typing is again by 86～110 ℃ of preheating cross directional stretch and 180～200 ℃ of typing crystallization treatment;
But e, remove slitter edge, sided corona treatment, detection thickness and carry out again the polyester film that the single face direct heat involution that makes thickness 15um～30um is batched in rolling finally by crossing traction.
The B layer is intermediate core layer, by main extruder---and single screw extrusion machine is extruded; The A layer is the top layer heat-sealable layer, by auxiliary extruder---double screw extruder is extruded; The C layer is anti-adhering layer, and by auxiliary extruder---double screw extruder is extruded, the A layer assists extruder, B layer main extruder, the auxiliary extruder polyester slice of C layer to extrude mass ratio and be: 10～20:65～80:10～20.
Copolymerization PETG polyester slice preparation method is in the heat-sealable layer of A layer top layer:
A, mix after 100 parts of dimethyl terephthalate (DMT)s (DMT), 25～35 parts of ethylene glycol (EG), 1～5 part of silica (SiO2) and 20～30 parts of Isosorbide-5-Nitrae cyclohexanedimethanols (CHDM) are sent into polymeric kettle;
B, add the phosphorous acid triphen (C18H15O3P) of 2～4 parts antimony oxide (Sb2O3) and 2～4 parts as catalyst and stabilizing agent again;
C, polymeric kettle is airtight after, control polymerization temperature in the kettle and pressure carry out 0.5～1.5h ester exchange reaction with nitrogen (N2) under 170～210 ℃ of lower and 500～700pa;
D, then be warming up to 240～280 ℃ in the polymeric kettle, polymeric kettle is vacuumized, then under the effect of composite catalyst, carry out polycondensation reaction 2～4h in the high vacuum;
E, discharging, cooling, pelletizing make copolymerization PETG polyester slice.
Among the step a, it is 20～30 part 1 with mass content at first, 4 cyclohexanedimethanols (CHDM) and mass content are that 1～5 part of silica (SiO2) joins 25～35 parts of ethylene glycol (EG), dispersed with stirring, disperse through supersonic oscillations again, so that after each composition high speed dispersion homogenizing, send into polymeric kettle; Then adding 100 parts of dimethyl terephthalate (DMT)s (DMT) mixes.
Among the step c, carrying out ester exchange reaction after polymeric kettle is airtight replaces 3 times with nitrogen (N2), after ester exchange reaction finishes, reclaim unnecessary ethylene glycol (EG), in the steps d, composite catalyst is: the composition of titanium dioxide, silica, the compound that contains molybdenum, zinc acetate and compd A, compd A are taken from any in manganese acetate or the manganese chloride or both mixtures.The advantage of this catalyst is that the course of reaction side reaction is few, and the polyester that obtains has better color and luster.
Embodiment 2
A kind of preparation method of the polyester film that can directly seal, by weight: with mass content be 22 parts 1,4 cyclohexanedimethanols (CHDM) and mass content are that 3 parts silica (SiO2) joins in 23 parts the ethylene glycol (EG), dispersed with stirring, again through the high speed dispersion homogenizing, after adopting supersonic oscillations to disperse, send in the main reaction system polymeric kettle; Add 100 parts of dimethyl terephthalate (DMT)s (DMT) and mix, add again antimony oxide and the triphenyl phosphite of 2 parts (PTA weight), airtight rear with nitrogen (N2) displacement 3 times.Be under the 600Pa in the still internal pressure, be warming up to 180 ℃, esterification 0.8h, esterification reclaims unnecessary ethylene glycol (EG) after finishing; Then be warming up to 260 ℃, vacuumize polyase 13 .4h discharging, cooling, pelletizing under the condition, make copolymerization PETG polyester slice.
The copolymerization PETG polyester slice of preparation 100% is joined auxiliary double screw extruder after measuring by accurate weighing-appliance and extrudes (A layer) by mass percentage; The raw material proportioning of main extruder (B layer) is 100% to surpass bright PET chips by mass percentage, and raw material is sent into main extruder after by accurate measurement and extruded; The raw material proportioning of auxiliary double screw extruder (C layer) is 60% to surpass bright PET chips and 40% antiblocking agent masterbatch polyester slice by mass percentage, sends into extruder after raw material mixes by accurate measurement and extrudes.The mass ratio of main extruder and two auxiliary double screw extruders is 10:75:15, and 20um film A layer heat-sealable layer thickness is 2.0um, and C layer anti-sticking layer thickness is 3.0um.Polyester slice is melt extruded at 270 ℃, melt becomes sheet material through the slab of cooling below 30 ℃, the PET sheet material of casting is carried out longitudinal stretching, the longitudinal stretching preheating, draft temperature is 90 ℃, stretching ratio is 3.5 times, behind the longitudinal stretching at 35 ℃ of following temperature cooling and shapings, then carry out cross directional stretch, the cross directional stretch preheating, draft temperature is 110 ℃, stretching ratio is 3.7 times, through under 190 ℃ of temperature, carrying out the shaping film crystallization treatment respectively after the biaxial tension, under 80 ℃ and normal temperature wind, cool off again, the film that cools down is by the Traction Station flash trimming, corona, the last rollings such as detection thickness make the polyester film that can directly seal that gross thickness is 20um, and this can directly seal polyester film top layer (A layer) and be heat-sealable layer to contain 100% copolymerization PETG polyester slice; Intermediate layer (B layer) is contained and 100% is surpassed bright PET chips; Anti-stick top layer (C layer) is contained and 60% is surpassed 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 is 15:70:15, and 20um film A layer heat-sealable layer thickness is 3.0um, and 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 is 20:65:15, and 20um film A layer heat-sealable layer thickness is 4.0um, and C layer anti-sticking layer thickness is 3.0um.
The correlated performance that can directly seal polyester film that the present invention makes adopts the German MAHR model HSG-C of company heat-sealing measuring instrument according to ASTM D standard; The haze meter, the Grossmeters that adopt German BYK-Gardner GmbH company to produce carry out the measurement of mist degree and glossiness; The tensilometer that adopts company of Britain LLOYD company to produce is measured hot strength; The PX(J that adopts domestic Yancheng chemical fibre equipment factory to produce)-1 type baking oven is measured percent thermal shrinkage
Table 1: adopt the synthetic copolymerization PETG polyester slice of good cost performance to produce same thin film thickness and production technology, different heat-sealable layer thickness structures distribute to produce and can directly seal polyester film example 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), with mass content be 28 parts 1,4 cyclohexanedimethanols (CHDM) and mass content are that 3 parts silica (SiO2) joins in 32 parts the ethylene glycol (EG), dispersed with stirring, after high speed dispersion homogenizing (supersonic oscillations dispersion), send into main reaction system (polymeric kettle) again; Add 100 parts of dimethyl terephthalate (DMT)s (DMT) and mix, add again antimony oxide and the triphenyl phosphite of 2 parts (PTA weight), airtight rear with N2 displacement 3 times.Be under the 650Pa in the still internal pressure, be warming up to 190 ℃, esterification 1.5h, esterification reclaims unnecessary ethylene glycol (EG) after finishing; Then be warming up to 260 ℃, vacuumize polyase 13 .2h discharging, cooling, pelletizing under the condition, make copolymerization PETG polyester slice.
(2), the copolymerization PETG polyester slice of preparation 100% is joined auxiliary double screw extruder after measuring by accurate weighing-appliance and extrudes (A layer) by mass percentage; The raw material proportioning of main extruder (B layer) is 100% to surpass bright PET chips by mass percentage, and raw material is sent into main extruder after by accurate measurement and extruded; The raw material proportioning of auxiliary double screw extruder (C layer) is 60% to surpass bright PET chips and 40% antiblocking agent masterbatch polyester slice by mass percentage, sends into extruder after raw material mixes by accurate measurement and extrudes.The mass ratio that main extruder and two auxiliary double screw extruder materials are extruded is 15:75:15, and 18um film A layer heat-sealable layer thickness is 2.7um, and C layer anti-sticking layer thickness is 2.7um.For polyester slice is extruded melting at 240～280 ℃, melt becomes sheet material through the slab of cooling below 30 ℃, the PET sheet material of casting is carried out longitudinal stretching, the longitudinal stretching preheating, draft temperature is 100 ℃, stretching ratio is 3.5 times, behind the longitudinal stretching at 35 ℃ of following temperature cooling and shapings, then carry out cross directional stretch, the cross directional stretch preheating, draft temperature is 89 ℃, stretching ratio is 3.7 times, through under 178 ℃ of temperature, carrying out the shaping film crystallization treatment respectively after the biaxial tension, under 80 ℃ and normal temperature wind, cool off again, the film that cools down is by the Traction Station flash trimming, corona, the last rollings such as detection thickness make the polyester film that can directly seal that gross thickness is 18um, and this can directly seal polyester film top layer (A layer) and be heat-sealable layer to contain 100% copolymerization PETG polyester slice; Intermediate layer (B layer) is contained and 100% is surpassed bright PET chips; Anti-stick top layer (C layer) is contained and 60% is surpassed 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 directly seal polyester film, it is 15:75:15 that the material of main extruder and two auxiliary double screw extruders is extruded mass ratio, 18um film A layer heat-sealable layer thickness is 2.7um, and 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 directly seal polyester film, it is 15:75:15 that the material of main extruder and two auxiliary double screw extruders is extruded mass ratio, 25um film A layer heat-sealable layer thickness is 3.75um, and 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 directly seal polyester film, it is 15:75:15 that the material of main extruder and two auxiliary double screw extruders is extruded mass ratio, 30um film A layer heat-sealable layer thickness is 4.5um, and C layer anti-sticking layer thickness is 4.5um.
Table 2: adopt the synthetic copolymerization PETG polyester of good cost performance to cut production same structure mass ratio layering and same production technology, different film thicknesses are produced and can directly be sealed polyester film example 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 15:70:15, and 20um film A layer heat-sealable layer thickness is 3.0um, and C layer anti-sticking layer thickness is 3.0um.
(1), with mass content be 21 parts 1,4 cyclohexanedimethanols (CHDM) and mass content are that 1 part silica (SiO2) joins in 34 parts the ethylene glycol (EG), dispersed with stirring, after high speed dispersion homogenizing (supersonic oscillations dispersion), send into main reaction system (polymeric kettle) again; Add 100 parts of dimethyl terephthalate (DMT)s (DMT) and mix, add again antimony oxide and 4 portions of triphenyl phosphites of 4 parts (PTA weight), airtight rear with N2 displacement 3 times.Be under the 700Pa in the still internal pressure, be warming up to 176 ℃, esterification 1.2h, esterification reclaims unnecessary ethylene glycol (EG) after finishing; Then be warming up to 276 ℃, vacuumize polymerization 4h discharging, cooling, pelletizing under the condition, make copolymerization PETG polyester slice.
(2), the copolymerization PETG polyester slice of preparation 100% is joined auxiliary double screw extruder after measuring by accurate weighing-appliance and extrudes (A layer) by mass percentage; The raw material proportioning of main extruder (B layer) is 100% to surpass bright PET chips by mass percentage, and raw material is sent into main extruder after by accurate measurement and extruded; The raw material proportioning of auxiliary double screw extruder (C layer) is 60% to surpass bright PET chips and 40% antiblocking agent masterbatch polyester slice by mass percentage, sends into extruder after raw material mixes by accurate measurement and extrudes.The quality of materials of main extruder and two auxiliary double screw extruders is than being 15:70:15, and 20um film A layer heat-sealable layer thickness is 3.0um, and C layer anti-sticking layer thickness is 3.0um.The special process production process is that polyester slice is extruded melting at 220～240 ℃, melt becomes sheet material through the slab of cooling below 28 ℃, the PET sheet material of casting is carried out longitudinal stretching, the longitudinal stretching preheating, draft temperature is 60～90 ℃, stretching ratio is 3.5 times, behind the longitudinal stretching at 35 ℃ of following temperature cooling and shapings, then carry out cross directional stretch, the cross directional stretch preheating, draft temperature is 65～95 ℃, stretching ratio is 3.7 times, through under 160 ℃～180 ℃ temperature, carrying out the shaping film crystallization treatment respectively after the biaxial tension, under 60 ℃ and normal temperature wind, cool off again, the film that cools down is by the Traction Station flash trimming, corona, the last rollings such as detection thickness make the polyester film that can directly seal that gross thickness is 20um, and this can directly seal polyester film top layer (A layer) and be heat-sealable layer to contain 100% copolymerization PETG polyester slice; Intermediate layer (B layer) is contained and 100% is surpassed bright PET chips; Anti-stick top layer (C layer) is contained and 60% is surpassed bright PET chips and 40% antiblocking agent masterbatch polyester slice.
Embodiment 10
The difference of the present embodiment and embodiment 9 is: during preparation 20um film, it is 15:70:15 that the material of main extruder and two auxiliary double screw extruders is extruded mass ratio, and 20um film A layer heat-sealable layer thickness is 3.0um, and 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), with mass content be 25 parts 1,4 cyclohexanedimethanols (CHDM) and mass content are that 1 part silica (SiO2) joins in 30 parts the ethylene glycol (EG), dispersed with stirring, after high speed dispersion homogenizing (supersonic oscillations dispersion), send into main reaction system (polymeric kettle) again; Add 100 parts of dimethyl terephthalate (DMT)s (DMT) and mix, add again antimony oxide and the triphenyl phosphite of 2 parts (PTA weight), airtight rear with N2 displacement 3 times.Be under 500～700Pa in the still internal pressure, be warming up to 170～210 ℃, esterification 0.5～1.5h, esterification reclaims unnecessary ethylene glycol (EG) after finishing; Then be warming up to 240～280 ℃, vacuumize polymerization 2～4h discharging, cooling, pelletizing under the condition, make copolymerization PETG polyester slice.
(2), the copolymerization PETG polyester slice of preparation 100% is joined auxiliary double screw extruder after measuring by accurate weighing-appliance and extrudes (A layer) by mass percentage; The raw material proportioning of main extruder (B layer) is 100% to surpass bright PET chips by mass percentage, and raw material is sent into main extruder after by accurate measurement and extruded; The raw material proportioning of auxiliary double screw extruder (C layer) is 60% to surpass bright PET chips and 40% antiblocking agent masterbatch polyester slice by mass percentage, sends into extruder after raw material mixes by accurate measurement and extrudes.The mass ratio of main extruder and two auxiliary double screw extruders is 15:70:15, and 20um film A layer heat-sealable layer thickness is 3.0um, and C layer anti-sticking layer thickness is 3.0um.The special process production process is that polyester slice is extruded melting at 260～280 ℃, melt becomes sheet material through the slab of cooling below 28 ℃, the PET sheet material of casting is carried out longitudinal stretching, the longitudinal stretching preheating, draft temperature is 70～115 ℃, stretching ratio is 3.5 times, behind the longitudinal stretching at 35 ℃ of following temperature cooling and shapings, then carry out cross directional stretch, the cross directional stretch preheating, draft temperature is 86～125 ℃, stretching ratio is 3.7 times, through under 200 ℃～220 ℃ temperature, carrying out the shaping film crystallization treatment respectively after the biaxial tension, under 60 ℃ and normal temperature wind, cool off again, the film that cools down is by the Traction Station flash trimming, corona, the last rollings such as detection thickness make the polyester film that can directly seal that gross thickness is 20um, and this can directly seal polyester film top layer (A layer) and be heat-sealable layer to contain 100% copolymerization PETG polyester slice; Intermediate layer (B layer) is contained and 100% is surpassed bright PET chips; Anti-stick top layer (C layer) is contained and 60% is surpassed bright PET chips and 40% antiblocking agent masterbatch polyester slice.
The correlated performance that can directly seal polyester film that the present invention makes adopts the German MAHR model HSG-C of company heat-sealing measuring instrument according to ASTM D standard; The haze meter, the Grossmeters that adopt German BYK-Gardner GmbH company to produce carry out the measurement of mist degree and glossiness; The tensilometer that adopts company of Britain LLOYD company to produce is measured hot strength; The PX(J that adopts domestic Yancheng chemical fibre equipment factory to produce)-1 type baking oven is measured percent thermal shrinkage.
Table 3: adopt the synthetic copolymerization PETG polyester slice of good cost performance, produce same composition of raw materials and same thin film thickness, different production technologies can directly seal polyester film example comparison sheet:
Table 3
In a word, the above only is preferred embodiment of the present invention, and all equalizations of doing according to the present patent application claim change and modify, and all should belong to the covering scope of patent of the present invention.
Claims (10)
1. the polyester film that can directly seal comprises the ABC three-decker, it is characterized in that: described B layer is intermediate core layer, and material is the super bright PET chips of PET; The A layer is the top layer heat-sealable layer, and material is copolymerization PETG polyester slice; The C layer is anti-adhering layer, and material comprises the section of PET antiblocking agent masterbatch and the super bright PET chips of PET.
2. a kind of polyester film that can directly seal according to claim 1, it is characterized in that: the anti-adhering layer of described C layer, material has the component of following mass percent: 30%～60% the section of PET antiblocking agent masterbatch and the super bright PET chips of 40%～70%PET.
3. 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%.
4. a kind of polyester film that can directly seal according to claim 1, it is characterized in that: the copolymerization PETG polyester slice of described A layer top layer heat-sealable layer, be by dimethyl terephthalate (DMT) (DMT), ethylene glycol (EG), silica (SiO2) and 1,4-CHDM (CHDM) totally four kinds of monomers with the product of ester-interchange method polycondensation.
5. a kind of polyester film that can directly seal according to claim 1, it is characterized in that: in the anti-adhering layer of described C layer, the section of PET antiblocking agent masterbatch is for containing silica (SiO2) polyester slice, and silica (SiO2) particle diameter is 2～3um, and content is 3000ppm.
6. the polyester film manufacture craft that can directly seal comprises the described polyester film of claim 1-5, it is characterized in that: comprise the steps:
A, A layer copolymerization PETG polyester slice, the super bright PET chips of B layer PET and the super bright PET chips of C layer PET and the PET antiblocking agent masterbatch of preparation are cut into slices, send into respectively three-layer co-extruded biaxial tension equipment, wherein A layer copolymerization PETG polyester slice is sent into auxiliary extruder---double screw extruder, the super bright PET chips of B layer PET is sent into main extruder---single screw extrusion machine, and auxiliary extruder---double screw extruder is sent in the super bright PET chips of C layer PET and the section of PET antiblocking agent masterbatch;
B, ABC three strata esters sections is extruded melting at 240～280 ℃, melt generates the PET sheet material through the slab of cooling below 30 ℃;
C, the PET sheet material cast are through 80～100 ℃ of preheating longitudinal stretchings and 35 ℃ of following temperature cooling and shapings;
PET sheet material after d, the typing is again by 86～110 ℃ of preheating cross directional stretch and 180～200 ℃ of typing crystallization treatment;
But e, remove slitter edge, sided corona treatment, detection thickness and carry out again the polyester film that the single face direct heat involution that makes thickness 15um～30um is batched in rolling finally by crossing traction.
7. a kind of polyester film manufacture craft that can directly seal according to claim 6, it is characterized in that: described B layer is intermediate core layer, by main extruder---single screw extrusion machine is extruded; The A layer is the top layer heat-sealable layer, by auxiliary extruder---double screw extruder is extruded; The C layer is anti-adhering layer, and by auxiliary extruder---double screw extruder is extruded, the A layer assists extruder, B layer main extruder, the auxiliary extruder polyester slice of C layer to extrude mass ratio and be: 10～20:65～80:10～20.
8. a kind of polyester film manufacture craft that can directly seal according to claim 6, it is characterized in that: copolymerization PETG polyester slice preparation method is in the heat-sealable layer of described A layer top layer:
A, mix after 100 parts of dimethyl terephthalate (DMT)s (DMT), 25～35 parts of ethylene glycol (EG), 1～5 part of silica (SiO2) and 20～30 parts of Isosorbide-5-Nitrae cyclohexanedimethanols (CHDM) are sent into polymeric kettle;
B, add the phosphorous acid triphen (C18H15O3P) of 2～4 parts antimony oxide (Sb2O3) and 2～4 parts as catalyst and stabilizing agent again;
C, polymeric kettle is airtight after, control polymerization temperature in the kettle and pressure carry out 0.5～1.5h ester exchange reaction with nitrogen (N2) under 170～210 ℃ of lower and 500～700pa;
D, then be warming up to 240～280 ℃ in the polymeric kettle, polymeric kettle is vacuumized, then under the effect of composite catalyst, carry out polycondensation reaction 2～4h in the high vacuum;
E, discharging, cooling, pelletizing make copolymerization PETG polyester slice.
9. a kind of polyester film manufacture craft that can directly seal according to claim 8, it is characterized in that: among the described step a, it is 20～30 part 1 with mass content at first, 4 cyclohexanedimethanols (CHDM) and mass content are that 1～5 part of silica (SiO2) joins 25～35 parts of ethylene glycol (EG), dispersed with stirring, disperse through supersonic oscillations again, so that after each composition high speed dispersion homogenizing, send into polymeric kettle; Then adding 100 parts of dimethyl terephthalate (DMT)s (DMT) mixes.
10. a kind of polyester film manufacture craft that can directly seal according to claim 8, it is characterized in that: among the described step c, carrying out ester exchange reaction after polymeric kettle is airtight replaces 3 times with nitrogen (N2), after ester exchange reaction finishes, reclaim unnecessary ethylene glycol (EG), in the steps d, composite catalyst is: the composition of titanium dioxide, silica, the compound that contains molybdenum, zinc acetate and compd A, compd A are taken from any in manganese acetate or the manganese chloride or both mixtures.
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| CN115384160B (en) * | 2022-09-23 | 2024-02-06 | 湖南怡永丰新材料科技有限公司 | Cover film for powder-liquid double-chamber bag and preparation method and application thereof |
| CN115958866A (en) * | 2023-03-16 | 2023-04-14 | 江苏康辉新材料科技有限公司 | Flame-retardant PET film suitable for laser coding and preparation method and application thereof |
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| CN102873954B (en) | 2015-08-19 |
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Denomination of invention: A kind of polyester film that can be directly heat-sealed and preparation method thereof Effective date of registration: 20220810 Granted publication date: 20150819 Pledgee: Zhejiang Tailong Commercial Bank Co.,Ltd. Wenzhou Cangnan Qianku small and micro enterprise franchise sub branch Pledgor: Zhejiang Qiangmeng Industrial Co.,Ltd. Registration number: Y2022330001713 |
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