CN102225648A - A kind of high barrier polyester film and preparation method thereof - Google Patents
A kind of high barrier polyester film and preparation method thereof Download PDFInfo
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- CN102225648A CN102225648A CN2011100932426A CN201110093242A CN102225648A CN 102225648 A CN102225648 A CN 102225648A CN 2011100932426 A CN2011100932426 A CN 2011100932426A CN 201110093242 A CN201110093242 A CN 201110093242A CN 102225648 A CN102225648 A CN 102225648A
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- sandwich layer
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- 229920006267 polyester film Polymers 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 230000004888 barrier function Effects 0.000 title abstract description 8
- 229920000728 polyester Polymers 0.000 claims abstract description 45
- 239000003607 modifier Substances 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 33
- 150000001875 compounds Chemical class 0.000 claims description 11
- 238000010899 nucleation Methods 0.000 claims description 11
- 230000006911 nucleation Effects 0.000 claims description 11
- 238000005266 casting Methods 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 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 claims description 5
- 241001614291 Anoplistes Species 0.000 claims description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 3
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- -1 benzyl D-sorbite Chemical compound 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 229920002523 polyethylene Glycol 1000 Polymers 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical group [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 3
- 235000010234 sodium benzoate Nutrition 0.000 claims description 3
- 239000004299 sodium benzoate Substances 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 239000010410 layer Substances 0.000 abstract description 40
- 239000002131 composite material Substances 0.000 abstract description 6
- 239000012792 core layer Substances 0.000 abstract description 3
- 230000005855 radiation Effects 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract 1
- 239000002667 nucleating agent Substances 0.000 abstract 1
- 230000000704 physical effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Photovoltaic Devices (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a high-barrier polyester film, which has a three-layer composite construction, comprising a core layer, an upper cortex and a lower cortex. The core layer comprises the following components of: 60-100 wt% of PET polyester slices, 0-40 wt% of PEN polyester slices; the cortexes comprise the following components of: 92-98 wt% of PEN polyester slices, 0.2-2 wt% of a nucleating agent and 1-6 wt% of a nucleating modifier. The invention also discloses a coextruding-drawing preparation method of the above high-barrier polyester film. The invention has a simple preparation technology; in addition to excellent physical properties, the produced polyester film has better gas barrier property, heat resistance and radiation resistance performance, and can be applied in the fields of solar energy cell back-piece and the like.
Description
Technical field
The present invention relates to a kind of high-barrier polyester film and preparation method thereof, belong to the polyester film field.
Background technology
Polyester film is generally water white transparency, glossy, obdurability and elasticity good film, compare with other plastic sheetings, have that relative density is big, hot strength is high, percentage elongation is moderate, impact strength is big, good heat resistance, transparency be good, and advantage such as nontoxic is widely used in packaging material.Along with the develop rapidly of science and technology, polyester film also is being applied aspect capacitor, photosensitive material, phonotape and videotape and the solar cell owing to its good performance.As publication number is the Chinese invention patent of CN101065849A disclosed " highly adhesive polyester film and use its back protection film of solar cell "; constitute by polyester film and the resin coating that is coated on this polyester film one side; this protecting solar cell film is because its double-layer structure; complex manufacturing technology; and need to use special heat-processing equipment, manufacturing cost height.Simultaneously, because resin coating need use crosslinking agent and solvent aborning, can affect to environment.
Summary of the invention
The invention provides a kind of polyester film that steam and oxygen is had high barrier.
The present invention also provides the preparation method of above-mentioned high-barrier polyester film, and processing is simple.
A kind of high-barrier polyester film has three-layer composite structure, comprises the sandwich layer between two-layer cortex and two cortexes.
Described sandwich layer comprises following components in weight percentage: 60～100% PET polyester slice (pet resin), 0～40% PEN polyester slice (poly-2; The 6-(ethylene naphthalate)).Wherein the inherent viscosity of PET polyester slice is 0.60～0.65dl/g, and the inherent viscosity of PEN polyester slice is 0.50～0.60dl/g.
Described cortex comprises following components in weight percentage: 92～98% PEN polyester slice, 0.2～2% nucleator, 1～6% nucleation modifier.Described nucleator is Sodium Benzoate, talcum powder, nanometer grade silica, imvite, nano titanium oxide or 1; 3-2; In the benzyl D-sorbite of 4-two Asias (to methyl) one or more.Described nucleation modifier is one or more in polyethylene glycol or the triphenyl phosphite, wherein one or more among the preferred PEG-600 of polyethylene glycol, PEG-1000, PEG-2000, the PEG-5000.
The weight ratio of described sandwich layer and two-layer cortex is 3～9: 1.
Thickness 120～280 μ m of described sandwich layer, single skin thickness 5～35 μ m.
A kind of preparation method of above-mentioned high-barrier polyester film may further comprise the steps:
(1) with following components in weight percentage: 92～98% PEN polyester slice, 0.2～2% nucleator, 1～6% nucleation modifier are put into batch mixer and fully are mixed and made into cortex PEN masterbatch; The cortex PEN masterbatch that makes in vacuum drum with pre-crystallization 3～6h under 60～100 ℃ of temperature;
(2) with following components in weight percentage: 60～100% PET polyester slice, 0～40% PEN polyester slice is put into batch mixer and fully is mixed and made into the sandwich layer polyester masterbatch; The sandwich layer polyester masterbatch that makes in vacuum drum with pre-crystallization 3～6h under 60～100 ℃ of temperature;
(3) be that 3～9: 1 sandwich layer polyester masterbatch and cortex PEN masterbatch carry out drying 2～6h respectively with weight ratio under 120～170 ℃ of temperature;
(4) cortex PEN masterbatch and sandwich layer polyester masterbatch are added double screw extruder A and double screw extruder B respectively; Adjusting the main zone temperatures of extruder A is 275～300 ℃, and adjusting the main zone temperatures of extruder B is 265～300 ℃.Fused materials after filtering, the cortex PEN masterbatch of being extruded by double screw extruder A is as cortex, the sandwich layer polyester masterbatch of being extruded by double screw extruder B is made three layers of compound casting sheet (sheet) as sandwich layer through multi-layer co-extruded technology; Regulate the casting sheet that the die orifice aperture can obtain different-thickness.
Described multi-layer co-extruded technology is a kind ofly to use several extruders to supply with different fusion materials flows respectively, amounts at a compound die head internal exchange and extrudes the technology that obtains the MULTILAYER COMPOSITE sheet material.
(5) three layers of compound casting sheet preheating under 50～100 ℃ of temperature that step (4) made enter 50～100 ℃ Far-infrared Heating district, with the linear velocity longitudinal stretching of 3～5m/min; The longitudinal stretching multiplying power is 1.5～3.5, obtains diaphragm;
(6) diaphragm preheating under 90～140 ℃ of temperature that will obtain through longitudinal stretching is carried out cross directional stretch again under 100～160 ℃ of temperature; The cross directional stretch multiplying power is 1.5～3.8;
(7) will through the diaphragm of cross directional stretch under 200～240 ℃ of temperature conditions, finalize the design the back rolling.
Three layers of compound high-barrier polyester thin-pass of the present invention are crossed the preparation of co-extrusion drawing process, and its mediopellis is made up of PEN, and adds a certain amount of nucleator and nucleation accelerating agent.The chemical constitution of PEN is similar to PET, and difference is that PEN has replaced the phenyl ring among the PET by the bigger naphthalene nucleus of rigidity in the strand.Naphthalene ring makes PEN have performances such as higher physical and mechanical properties, gas barrier property, chemical stability and heat-resisting, UV resistant, radiation hardness than PET.With PEN is cortex, the gas barrier property of reinforced polyester film and weather resistance.Simultaneously, add the crystalline texture that nucleator and polyethylene glycol (PEG) nucleation accelerating agent can effectively be regulated cortex PEN, strengthen the adhesion of cortex and sandwich layer, guarantee mechanical properties in films.Compare with traditional PET polyester film, novel three layers of composite polyester film of the present invention are under the prerequisite that keeps the polyester film good physical, have better gas barrier property, heat resistance and radiation resistance, can be applicable to fields such as solar cell backing.
Description of drawings
Fig. 1 is the structural representation of film of the present invention
Description of reference numerals: 1-epithelial layer; The 2-sandwich layer; The 3-hypodermal layer.
The specific embodiment
As described in Figure 1, high-barrier polyester film of the present invention has three-layer composite structure, and the weight ratio of sandwich layer and two-layer cortex polyester masterbatch is 3～9: 1.The cortex polyester masterbatch contains following components in weight percentage: 92～98% PEN polyester slice, 0.2～2% nucleator, 1～6% nucleation modifier.Wherein nucleator is Sodium Benzoate, talcum powder, nanometer grade silica, imvite, nano titanium oxide, 1; 3-2; Wherein one or more of 4-two Asias (to methyl) benzyl D-sorbite, nucleation modifier is one or more in polyethylene glycol PEG-600, PEG-1000, PEG-2000, PEG-5000, the triphenyl phosphite (TPP).The sandwich layer polyester masterbatch contains following components in weight percentage: 60～100% PET polyester slice, 0～40% PEN polyester slice.
The preparation method of three layers of compound high-barrier polyester film of the present invention is as follows:
(1) by weight percentage, PEN polyester slice with 92～98%, 0.2～2% nucleator, 1～6% nucleation modifier are put into batch mixer and fully are mixed and made into cortex PEN masterbatch, rotating speed 〉=the 300r/min of batch mixer, the concrete percentage by weight of this cortex polyester masterbatch is as shown in table 1, in vacuum drum with pre-crystallization 3～6h under the 60-100 ℃ of temperature;
(2) by weight percentage, PET polyester slice with 60～100%, 0～40% PEN polyester slice is put into batch mixer and fully is mixed and made into the sandwich layer polyester masterbatch, rotating speed 〉=the 300r/min of batch mixer, the concrete percentage by weight of sandwich layer polyester masterbatch is as shown in table 1, in vacuum drum with pre-crystallization 3～6h under 60～100 ℃ of temperature;
(3) be that 3～9: 1 sandwich layer polyester masterbatch and cortex PEN masterbatch carry out drying 2～6h respectively again with weight ratio under 120～170 ℃ of temperature, moisture be controlled at be lower than 30ppm;
(4) dried cortex PEN masterbatch and sandwich layer polyester masterbatch are added double screw extruder A and B respectively, adjusting the main zone temperatures of extruder A is 275～300 ℃, and adjusting the main zone temperatures of extruder B is 265～300 ℃.Fused materials carries out extrusion composite technology after filtering and makes three layers of compound casting sheet, the cortex PEN masterbatch of being extruded by double screw extruder A is as cortex, the sandwich layer polyester masterbatch of being extruded by double screw extruder B is as sandwich layer, lamination (compound) becomes the three-decker of skin/core/cortex in three layers of mouth mould of die head, extrudes, cools off and make three layers of compound casting sheet (sheet) through die orifice; Regulate the casting sheet that the die orifice aperture can obtain different-thickness.
(5) sheet preheating under 50～100 ℃ of temperature enters 100 ℃～50 ℃ Far-infrared Heating district, carries out longitudinal stretching with the linear velocity of 3～5m/min, and the longitudinal stretching multiplying power is 1.5～3.5;
(6), will under 100～160 ℃ of temperature, carry out cross directional stretch again through diaphragm preheating under 90～140 ℃ of temperature of longitudinal stretching, the cross directional stretch multiplying power is 1.5～3.8;
(7) rolling after diaphragm is finalized the design under 200～240 ℃ of temperature conditions.
Adopt the cortex and the core layer prepared high-barrier polyester film of different content component as shown in table 1.
Table 1
Each embodiment in the his-and-hers watches 1 carries out performance test respectively, the results are shown in Table 2, table 3.
Table 2
Table 3
From table 1,2,3 as can be seen, and three layers of compound high-barrier polyester film of the present invention have good barrier performance, physical and mechanical property, can be applied to barrier property is had the field such as packaging material, insulating materials, solar cell backing of high request.
Claims (7)
1. high-barrier polyester film, it is characterized in that: comprise the sandwich layer between two-layer cortex and two cortexes, described sandwich layer comprises following components in weight percentage: 60～100% PET polyester slice, 0～40% PEN polyester slice, described cortex comprises following components in weight percentage: 92～98% PEN polyester slice, 0.2～2% nucleator, 1～6% nucleation modifier; The weight ratio of described sandwich layer and two-layer cortex is 3～9: 1.
2. high-barrier polyester film as claimed in claim 1 is characterized in that: thickness 120～280 μ m of described sandwich layer, single skin thickness 5～35 μ m.
3. high-barrier polyester film as claimed in claim 1 is characterized in that: the inherent viscosity of described PET polyester slice is 0.60～0.65dl/g, and the inherent viscosity of described PEN polyester slice is 0.50～0.60dl/g.
4. high-barrier polyester film according to claim 1, it is characterized in that: described nucleator is Sodium Benzoate, talcum powder, nanometer grade silica, imvite, nano titanium oxide, 1,3-2, wherein one or more of 4-two Asias (to methyl) benzyl D-sorbite.
5. high-barrier polyester film according to claim 1 is characterized in that: described nucleation modifier is one or more in polyethylene glycol and the triphenyl phosphite.
6. high-barrier polyester film according to claim 5 is characterized in that: described polyethylene glycol is one or more among PEG-600, PEG-1000, PEG-2000, the PEG-5000.
7. the preparation method of a high-barrier polyester film as claimed in claim 1 is characterized in that, may further comprise the steps:
(1) by weight percentage, 92～98% PEN polyester slice, 0.2～2% nucleator, 1～6% nucleation modifier are put into batch mixer and fully be mixed and made into cortex PEN masterbatch; The cortex PEN masterbatch that makes in vacuum drum with pre-crystallization 3～6h under 60～100 ℃ of temperature;
(2) by weight percentage, the PET polyester slice with 60～100%, 0～40% PEN polyester slice is put into batch mixer and fully is mixed and made into the sandwich layer polyester masterbatch; The sandwich layer polyester masterbatch that makes in vacuum drum with pre-crystallization 3～6h under 60～100 ℃ of temperature;
(3) be that 3～9: 1 sandwich layer polyester masterbatch and cortex PEN masterbatch carry out drying 2～6h respectively with weight ratio under 120～170 ℃ of temperature;
(4) dried cortex PEN masterbatch and sandwich layer polyester masterbatch are added double screw extruder A and double screw extruder B respectively; Adjusting the main zone temperatures of extruder A is 275～300 ℃, and adjusting the main zone temperatures of extruder B is 265～300 ℃; Fused materials after filtering, the cortex PEN masterbatch of being extruded by double screw extruder A is as cortex, the sandwich layer polyester masterbatch of being extruded by double screw extruder B is made three layers of compound casting sheet as sandwich layer through squeezing multi-layer co-extruded technology; Regulate the casting sheet that the die orifice aperture can obtain different-thickness;
(5) with three layers of compound casting sheet preheating under 50～100 ℃ of temperature, enter 50 ℃～100 ℃ Far-infrared Heating district, with the linear velocity longitudinal stretching of 3～5m/min, the longitudinal stretching multiplying power is 1.5～3.5, obtains diaphragm;
(6) diaphragm preheating under 90～140 ℃ of temperature that will obtain through longitudinal stretching is carried out cross directional stretch again under 100～160 ℃ of temperature; The cross directional stretch multiplying power is 1.5～3.8;
(7) rolling after the diaphragm behind the cross directional stretch is finalized the design under 200～240 ℃ of temperature conditions.
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| CN201110093242.6A CN102225648B (en) | 2011-04-14 | 2011-04-14 | High-barrier polyester film and its preparation method |
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| CN201110093242.6A CN102225648B (en) | 2011-04-14 | 2011-04-14 | High-barrier polyester film and its preparation method |
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| CN102225648B CN102225648B (en) | 2014-07-09 |
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Cited By (23)
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| CN103057232A (en) * | 2013-01-08 | 2013-04-24 | 常州百佳薄膜科技有限公司 | High-barrier PET (polyethylene terephthalate) film and making method thereof |
| CN103407257A (en) * | 2013-08-16 | 2013-11-27 | 汕头可逸塑胶有限公司 | High-barrier-property BOPET (biaxially-oriented polyethylene terephthalate) packaging film and production method thereof |
| CN103483782A (en) * | 2013-09-03 | 2014-01-01 | 陈曦 | Multipurpose polyester film and preparation method thereof |
| CN103692748A (en) * | 2013-12-13 | 2014-04-02 | 合肥乐凯科技产业有限公司 | Optical polyester thin film |
| CN104263273A (en) * | 2014-09-28 | 2015-01-07 | 上海济仕新材料科技有限公司 | High-barrier polyester film as well as preparation method and applications thereof |
| CN104842608A (en) * | 2015-02-12 | 2015-08-19 | 广东树业环保科技股份有限公司 | Uvioresistant polyester film for window film and preparation method therefor |
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Cited By (35)
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