CN1733397A - Biaxial tension co-extrusion high-obstruct base material membrane and process for preparing the same - Google Patents
Biaxial tension co-extrusion high-obstruct base material membrane and process for preparing the same Download PDFInfo
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Abstract
This invention provides biaxial tension coextrude resistive base material membrane and preparation method. Wherein, the membrane comprises at least a resistive layer that is at least one of PA, PVA, PVDC and MAD6, a splice layer belonged to EAA, EEA, ethylenemethacrylic acid copolymerized resin or polyolefin and neolyn resin that can combine the other tow layers, and a heat-sealing layer that is at least one of the polyolefin resin, EVA and PET; besides, there is nano inorganic material in resistive layer and or heat-sealing layer to improve performance. The product fits to package for all kinds goods.
Description
Technical field
The present invention relates to a kind of plastic shaping material, especially a kind of biaxial tension co-extrusion high-obstruct base material membrane and preparation method thereof.
Background technology
The packaging material that the plastic flexible package film is the contour shelf-life of food, medicine, high commodity on shelf is commonly used.Mainly contain the thin polymer film of biaxial tension, as BOPP (Biaially oriented polypropylene), BOPET (biaxial orientation polyethylene glycol terephthalate), BOPA (Biaxially orientated polyamide), BOPS mono-material films such as (biaxial orientation styrene), or film, plating silicon fiml are bored in platings such as PP, PE, PET; And PP, LDPE, EVA, PVDC, thin-film materials such as PA, PVC.Early stage these products have been brought into play enormous function in people's life.In order to improve the performance of product, in recent years, developed again adopt BOPP/ aluminium platinum/PET/LDPE, BOPP/CPP that the dry type composite algorithm produces or/LLDPE, composite packing films such as BOPET/PA/CPP satisfy ever-increasing packing demand.Described dry type composite algorithm production technology is: after the mono-material film processing film forming, as required that several layers is compound.
Though the packaging material intensity height of individual layer material preparation, its shelf-life is short, can not satisfy the demand of people to packaging material; PP TYPE can overcome the deficiency of monolayer material to a certain extent, but its intensity is lower than biaxial stretching film, and membrane product is thick partially and waste material and resource have improved cost simultaneously; In addition, traditional processing technology also exists complex process, defect of high cost.
At present, the external composite membrane that multi-layer co-extruded and biaxial tension have occurred, but all be confined to resin of the same race or similar, as the employing of multilayer BOPP film is the composite membrane of homopolymerization or copolymerization PP resin, what multilayer BOPA film adopted is the homopolymerization of PA6, PA6/66, the combination of copolymer, and film, plating silicon fiml are bored in platings such as PP, PE, PET; And PP, LDPE, EVA, PVDC, PA, the PVC etc. of blow moulding production are of the same race or the laminated film of similar resin.This mainly is because because incompatible between polar resin and the non-polar resin, during directly that polarity is different two kinds of resin co-extrusions, is difficult to compoundly, bonding between layer and the layer, and may produce and peels off, and is difficult to obtain well behaved film.Therefore, adopt at present mostly adhesives together with the resin bonding of opposed polarity.
Though CN1252348A discloses Japanese Wu Yu company " multilayer film casing of stretching and preparation method thereof ", it does the shrink film of membrane layer this multilayer film casing for polyamide.Adopt many extruders to extrude, through melting adhered each layer of annular die and coextrusion preparation, this film manufacturing cost height.
Along with the enhancing of people's environmental protection consciousness, saving and resource conservation, cut the waste, reducing cost becomes the target of scientist and engineers and technicians' unremitting effort.Therefore, the thin-film material that development technology is simple, cost is low, quality is good, performance is high is very significant.
Summary of the invention
The purpose of this invention is to provide a kind of biaxial tension co-extrusion high-obstruct base material membrane, this base material film is the composite membrane of similar polymers not, have high gas barrier, high strength, high transparent, heat-sealable, impressionability, reduce the material usage of prior art composite package film, reduce packing cost, the quality height of membrane product can be made the packing articles that is suitable for various article packings simultaneously, satisfies different needs.
Another object of the present invention provides a kind of preparation method of biaxial tension co-extrusion high-obstruct base material membrane.This method is combined as high-obstruct base material membrane with multilayer, many materials raw material by multi-layer co-extruded one step of technology, owing to adopt the one-shot forming of biaxial tension method, has effectively improved the quality of membrane product simultaneously.
The object of the present invention is achieved like this: a kind of biaxial tension co-extrusion high-obstruct base material membrane, at least comprise a barrier layer, an adhesive linkage and a hot sealing layer, described barrier layer is a kind of of PA (polyamide), PVA (polyvinyl alcohol), PVDC (polyvinylidene chloride), EVOH (ethene one EVOH), described hot sealing layer is a kind of among vistanex, EVA, PET, PLA (PLA) or the PS, the adhering resin of described adhesive linkage for barrier layer and hot sealing layer being combined.
High-obstruct base material membrane of the present invention also comprises one second adhesive linkage and second hot sealing layer, and barrier layer is positioned at the centre of base material film, and is mutually bonding with hot sealing layer through adhesive linkage.
Also can also comprise the one second and/or the 3rd barrier layer, second adhesive linkage and second hot sealing layer by high-obstruct base material membrane of the present invention, barrier layer is positioned at the centre of base material film, and is mutually bonding with hot sealing layer through adhesive linkage.
The polymer of second adhesive linkage wherein, second barrier layer, second hot sealing layer and corresponding ground floor is identical or different.
Barrier layer wherein can place the outermost or the centre of base material film, preferably places in the middle of the base material film.
PA wherein comprises nylon 6 and nylon 66, also can be nylon 11, nylon 12, and NYLON610, nylon 612, and nylon 1010, nylon 46, nylon 7, nylon 9, nylon 13, new varieties have nylon 6I, nylon 9 T and special nylon-barrier resin MXD6.Among the present invention, preferred nylon 6 and nylon 66, MXD6, PVA and EVOH.
In the barrier layer and/or hot sealing layer of base material film of the present invention, also comprise nano inorganic material,, reach the effect of getting twice the result with half the effort to improve gas barrier property, heat distortion temperature and the mechanical property of barrier layer.Above-mentioned nano inorganic material can carry out polymerization behind the monomer and obtains nanometer polymer for inorganic nano material is embedded, or with inorganic nano material and the direct blending of polymer, these methods and the polymer that obtains are fully open in the prior art, referring to US4739007, US5385776, US5091462, US5102948, US5552469, and in the Adv.Mater. in 1996 8,29 disclosed silicate nano-composition layering polymer; PlasticsTechnology 1998,1, nano-complex of disclosed clay filled etc. in 21.Among the present invention, preferably adopt the mode of blend to prepare the nano modification polymer.Wherein nano inorganic material is nano imvite or clay, SiO
2, TiO
2, CaCO
3Deng.The content of nano inorganic material in polymer is 1～10wt%.
The adhering resin of adhesive linkage of the present invention for barrier layer of the present invention and hot sealing layer being combined, include but not limited to ethylene-propylene acid resin (EAA), ethylene-propylene acetoacetic ester copolymer resins (EEA), ethylene-methyl methacrylate copolymer resins or polyolefin and maleic anhydride modified resin etc.
Barrier layer of the present invention, adhesive linkage or hot sealing layer etc. can for of the same race or not similar polymers be meant in the base material film of the present invention, during functional layer more than containing one deck, the polymer of same functional layer is identical or different, for example in a scheme of the present invention, comprise three layers of barrier layer, these three layers of barrier layers can all be PA6, can first barrier layer be PA6 also, second barrier layer is MXD6, the 3rd barrier layer is PA6, and perhaps these three layers of barrier layers are: the unsymmetric structure of MXD6-PA6-EVOH; Same two-layer hot sealing layer can be all LLDPE, also can be respectively the unsymmetric structure of LLDPE and EVA or PET.Such combination can be satisfied different packing needs.
When the compatibility between different types of resin is relatively poor, can also in the resin of barrier layer and/or hot sealing layer, add the compatible resin of corresponding resin, preferred compatible resin is adhering resin, silanes coupling agent etc.The consumption of compatible resin is the 1-10wt% of the resin of barrier layer and/or hot sealing layer.
The invention still further relates to a kind of biaxial tension co-extrusion high-obstruct base material membrane, for comprising the layer structure of three layers of barrier layer at least, one deck barrier layer wherein is PA, and in addition two-layer is selected from one or more the combination of PVA, PVDC, EVOH.
The layer structure of typical base material film of the present invention is:
As required, can the further compound BOPP that is used to print on the base material film of the present invention, BOPE or polyolefin film, if necessary, and can also be multiple again with aluminizer, so that the packing of suitable different needs enlarges purposes.
The optimal cross section thickness of base material film of the present invention is 15-100 μ m, preferred 20-60 μ m.Wherein, barrier layer accounts for the 5-60% of film gross thickness, and adhesive linkage accounts for the 5-30% of film gross thickness, and hot sealing layer accounts for the 20-45% of film gross thickness, preferred barrier layer thickness is less than 40% of film gross thickness, and the mechanics of its product, combination property reach or be higher than the current packaging product.And in the prior art; the thickness of general identical function, purposes packaging film is 80 μ m; only this item just can be saved 50% material, and the user saves the packing cost of 10-30%, this shows that this is the quality product of economical with materials, resource conservation, minimizing environmental pollution.
The preparation method of biaxial tension co-extrusion high-obstruct base material membrane of the present invention comprises the steps:
1) the used high molecular polymer material of each layer adds respectively in the different plasticizing machines and plastifies;
2) be extruded as the sheet material of multilayer by co-extrusion die head;
3) stretch through bi-directional synchronization, or carry out the vertical and horizontal stretching respectively;
4) obtain finished product through thermal finalization and cooling.
Wherein said preparation technology's concrete technological parameter is determined according to barrier material.
In the above-mentioned particularly preparation process, the temperature that co-extrusion is got to know is less than 250 ℃, preferred 230-250 ℃, the temperature of biaxial tension film body is 60-120 ℃, and heat setting temperature is 60-160 ℃, for heat shrink films, heat setting temperature is 60-100 ℃, and the heat setting temperature of non-heat shrink films is 110-160 ℃; Draw ratio is less than 18 times, and generally the longitudinal stretching multiplying power is 2.5-5 times, and the cross directional stretch multiplying power is 3-7 times, and preferred longitudinal stretching multiplying power is 2.5-4.5 times, and the cross directional stretch multiplying power is 3-6 times.
In the preparation process of the present invention, be material of main part or backing material with the material of barrier layer, and set concrete technological parameter according to the material of barrier layer.
Hot strength 〉=the 50Mpa of base material film of the present invention, elongation at break 〉=60%, gas permeation amount≤30cm
3/ m
224H 0.1mpa, rate of perviousness≤20g/m
224H.Heat seal strength 〉=15N is at full light light transmittance 〉=90%.
Adopt technical scheme of the present invention, can production high-barrier boiling film, high-barrier non high temperature boiling film and medical package material.
The present invention compared with prior art has following beneficial effect: every kind of raw material have its unique advantage, also its weakness are arranged respectively, and coextrusion processes the raw-material advantage of various differences can be merged to together, make colory laminated film, the present invention gropes and provides technical parameter and technology multi-layer co-extruded and biaxial tension high-barrier biaxial tension base material film and production by a large amount of experiments.The present invention adopts double bubble process, a step process to make the high-barrier multilayer complex films, the goods of producing detect its obstruct through relevant department and substantially exceed the co-extrusion film, intensity is higher than the mechanical property of mono-material, and satisfy design idea of the present invention, have good heat sealability, barrier, the transparency, try out through many enterprises and can satisfy dry type compound every quality, index fully.Thus, economical with materials greatly under condition of equivalent as can be seen, thus for resource conservation, reduce to pollute, reduce cost, played positive role.The food of base material film packing of the present invention, shelf-life can prolong greatly.
Describe the present invention in detail below in conjunction with the drawings and specific embodiments, described embodiment is used for understanding and describing the present invention, rather than restriction the present invention.
Description of drawings
Fig. 1 is Biaxially stretched multilayered co-extrusion high-obstruct base material membrane preparation method of the present invention and craft block-diagram,
Fig. 2 is the distribution and the match materials schematic diagram of five-layer structure sectional view of the present invention.
Fig. 3 is the distribution and the match materials schematic diagram of seven-layer structure sectional view of the present invention.
Fig. 4 is the present invention three distribution and match materials schematic diagram of structural section figure layer by layer.
The specific embodiment
Embodiment one
Fig. 1 is Biaxially stretched multilayered co-extrusion high-obstruct base material membrane preparation method of the present invention and craft block-diagram, generally by three above extruders to several not to resin extrude, enter head and carry out composite co-extruding, carry out vertical, horizontal stretching, thermal finalization respectively or simultaneously again, obtain Biaxially stretched multilayered co-extrusion high-obstruct base material membrane of the present invention.
Referring to Fig. 2 left side label, five-layer structure sectional view of the present invention, two skins (A layer) are hot sealing layer, selecting Exxon Neftegas Limited's trade mark for use is the LLDPE resin of 1018CA, barrier layer C selects nylon PA6/66 resin for use, producing the trade mark by BASF Aktiengesellschaft is C35EN, or the 5034FDX40 of Ube, and the trade mark that two-layer bonded resin bed B adopts Mitsui ﹠ Co., Ltd. to produce is the ethylene-propylene acid resin (EAA) of 528H.Preparation technology is referring to Fig. 1, and each layer material joined the plasticizing extruder of each layer respectively, produces through co-extrusion die head biaxial tension heat setting process.Intercepting the base material film structure is symmetrical structure A/B/C/B/A, layers of material ratio 10-25wt%/5-10wt%/5-45wt%/5-10wt%/10-25wt%.
In order to improve the compatibility between the resin, A layer, C layer add the compatilizer of 1-10% respectively.Compatilizer can be the adhering resin 528H of B layer or silane coupler etc.
In the preparation process, the longitudinal stretching multiplying power is 1: 2.8-4.5, and the cross directional stretch multiplying power is 1: 2.8-4.5, biaxial tension temperature and control temperature see table:
| Longitudinal stretching temperature ℃ | Cross directional stretch temperature ℃ | Heat setting temperature ℃ | |
| 60-120 ℃ of film body temperature | 60-120 ℃ of film body temperature | Heat shrink films | Non-heat shrink films |
| 60-100 ℃ of film body temperature | 100-160 ℃ of film body temperature | ||
The plasticizing extrusion temperature of each layer is decided according to the processability of resin, but the highlyest should not surpass 250 ℃, co-extrusion die head temperature 〉=230 ℃≤250 ℃.
In addition, in the present embodiment, can also in the raw material of A and/or B layer, add the nano imvite of 4wt%.
Embodiment two
Be all 5 layers of structure, base material film of the present invention also can be unsymmetric structure, referring to Fig. 2 right side label, the A layer is first hot sealing layer, it is the PP resin of HF400 that resin is selected the Korea S Samsung trade mark for use, but barrier layer C selects German BASF C35FN or the Japan EVOH of Leli company resin for use, trade mark G156B, the binding resin that binding resin selects for use Mitsui ﹠ Co., Ltd. to produce, it is the LDPE of FN810 that the second hot sealing layer E selects the Korea S Samsung trade mark for use, intercepting the base material film structure is asymmetrical A/B/C/D/E layer structure, B wherein, the material system of D is identical, just according to the structure film forming of material PP-HF400/571/G156B (or C35FN)/571/N810LDPE, various material ratios are 10-25wt%/5-10wt%/5-45wt%/5-10wt%/10-25wt%, and this ratio also can be a thickness.Draft temperature and multiplying power and preparation technology are referring to embodiment 1.
In the present embodiment, the trade mark that also can adopt Mitsui ﹠ Co., Ltd. to produce of the second binding resin layer D is the ethylene-propylene acid resin (EAA) of 528H.
Embodiment three
Choice of Resin is with example 1 or example 2, and structure is three layers of barrier layer PA6/66/ adhesive linkage ethylene-propylene acetoacetic ester copolymer resins/hot sealing layer LLDPE, and each stratum proportion is 20-60%/5-15%/20-60%.As shown in Figure 4.Other are with embodiment 1.
Embodiment four
Pressing the material of embodiment 1 selects.Press following structure proportion production high-barrier biaxial stretching film: PA/ adhesive/LDPE/ adhesive/PA; Adhesive wherein is: E.I.Du Pont Company's commodity are called Fusaboud
Maleic anhydride modified polymer like this, barrier layer is positioned at the outside of base material film, ratio 25%/5-10%/20-40%/5-10%/25%, stretching ratio and working process parameter are with embodiment 1.The PA adhesive
Embodiment five
With reference to the high-barrier biaxial stretching film of the present invention of embodiment 1 preparation seven-layer structure, structure is A/B/C/D/C/B/A, and referring to Fig. 3, the raw material of each layer is referring to table 3.
Each stratum proportion: 10-20%/5-15%/15-25%/10-20%/15-25%/5-15%/10-20%
Other embodiment
Base material film of the present invention can be three layers, five layers or seven-layer structure, and when the layer tree of barrier layer, adhesive linkage and hot sealing layer surpassed one deck, its material can be identical or different, produces the combination of various structures relatively, specifically referring to table 1-4.Wherein/be or.
Five layers of symmetrical structure A/B/C/B/A of table 1
| The preface example | Match materials 1 | Match materials 2 | Match materials 3 |
| A | PP/PE | PP/PE | PP/PE |
| B | Adhesive | Adhesive | Adhesive |
| C | PA/PVDC/PVA/MXD6 | ||
| B | Adhesive | Adhesive | Adhesive |
| A | PP/PE | PP/PE | PP/PE |
Five layers of unsymmetric structure A/B/C/D/E of table 2
| The preface example | Match materials 1 | Match materials 2 |
| A | PET | PA/PLA/PS |
| B | Adhesive | Adhesive |
| C | PA or PVDC, PVA or MXD6 | |
| D | Adhesive | Adhesive |
| E | Polyolefin | Polyolefin |
Seven layers of symmetry of table 3 and unsymmetric structure A/B/C/D/C/B/A, and A/B/C/D/E/F/G
| The preface example | Match materials 1 | Match materials 2 | Match materials 3 |
| A.A | PP/PE/EVA | PET | PP |
| B.B | Adhesive | Adhesive | Adhesive |
| C.C | PA | PA | PA |
| D.D | PVA/EVA adhesive/EVOH/PVDC/PA/MXD6 | ||
| C.E | PA | PA | PA |
| B.F | Adhesive | Adhesive | Adhesive |
| A.G | PP/PE/EVA | PP/PE/EVA | PE |
Three layers of unsymmetric structure A/B/C of table 4
| The preface example | Matching materials | ||
| A | PA | EVOH | MXD6/PLA |
| B | Adhesive | PVA | Adhesive |
| C | Polyolefin is as PE | PA | Polyolefin is as PP |
Comparative example
The five-layer co-squeezing film without biaxial tension of product performance index of the present invention and prior art compares
| Project | Unit | Embodiment 1 (five layers of stretching) | Embodiment 2 (five layers of stretching) | The five-layer co-squeezing film |
| Film thickness | um | 35 | 35 | 80 |
| Hot strength | Vertical/horizontal Mpa | ≥50 | ≥50 | 28 |
| Disconnect elongation | Vertical/horizontal % | ≥60 | ≥60 | ≥100 |
| Tear edge | Vertical/horizontal N | ≥10 | ≥10 | ≤5 |
| Heat seal strength | N20(UM) | ≥15 | ≥15 | ≥15 |
| Peeling force | N | ≥5 | ≥5 | ≥5 |
| The oxygen transit dose | Cm 3/m 2. 24H.0.1Mpa | ≤20 | ≤10 | ≤30 |
| Steam penetrating capacity | G/m24H | ≤15 | ≤5 | ≤10 |
| 100 ℃ of hot water shrinkages | 100％ | ≤5 | ≤5 | ≤5 |
| Transparency | 90％ | 90％ | 90％ |
As seen from the above table, properties of product of the present invention are much higher than prior art products, and film thickness is then lower, has saved raw material, not only can reduce cost of goods manufactured greatly and can enlarge packaging field again.
Claims (10)
1. biaxial tension co-extrusion high-obstruct base material membrane, at least the layer structure that comprises a barrier layer, an adhesive linkage and a hot sealing layer, described barrier layer is one or more the combination of PA, PVA, PVDC, EVOH, and described hot sealing layer is a kind of among vistanex, EVA resin, PLA, PET, PLA or the PS; The adhering resin of described adhesive linkage for barrier layer and hot sealing layer are combined.
2. a kind of high-obstruct base material membrane according to claim 1 also comprises one second adhesive linkage and second hot sealing layer, and barrier layer is positioned at the centre of base material film, and is mutually bonding with hot sealing layer through adhesive linkage.
3. a kind of high-obstruct base material membrane according to claim 1 also comprises the one second and/or the 3rd barrier layer, second adhesive linkage and second hot sealing layer, and barrier layer is positioned at the centre of base material film, and is mutually bonding with hot sealing layer through adhesive linkage.
4. according to claim 2 or 3 described a kind of high-obstruct base material membranes, second adhesive linkage wherein, second barrier layer, second hot sealing layer are identical or different with the polymer of one deck accordingly.
5. according to claim 1 or 2 or 3 described a kind of high-obstruct base material membranes, the PA in the barrier layer comprises nylon 6, nylon 66, nylon 11, nylon 12, NYLON610, nylon 612, nylon 1010, nylon 46, nylon 7, nylon 9, nylon 13, nylon 6I, nylon 9 T or MXD6; Preferred nylon 6 and nylon 66 and MXD6; Adhesive linkage is ethylene-propylene acid resin, ethylene-propylene acetoacetic ester copolymer resins, ethylene-methyl methacrylate copolymer resins or polyolefin and maleic anhydride modified resin.
6. according to claim 1 or 2 or 3 described a kind of high-obstruct base material membranes, in wherein the barrier layer and/or hot sealing layer, also comprise nano inorganic material, wherein nano inorganic material is nano imvite or clay, SiO
2, TiO
2, CaCO
3Deng.
7. according to claim 1 or 2 or 3 described a kind of high-obstruct base material membranes, also comprise compatible resin in the barrier layer wherein and/or the resin of hot sealing layer, described compatible resin is adhering resin or silanes coupling agent, and the consumption of compatible resin is the 1-10% of corresponding resin.
8. biaxial tension co-extrusion high-obstruct base material membrane, for comprising the layer structure of three layers of barrier layer at least, one deck barrier layer wherein is PA, in addition two-layer is selected from one or more the combination of PVA, PVDC, EVOH.
9. the preparation method of a biaxial tension co-extrusion high-obstruct base material membrane comprises the steps:
1) the used high molecular polymer material of each layer added respectively in the different plasticizing machines plastifies;
2) sheet material or the three bubble method blowings that are extruded as multilayer by co-extrusion die head stretch;
3) stretch through bi-directional synchronization, or carry out the vertical and horizontal stretching respectively;
4) obtain finished product through thermal finalization and cooling;
Wherein said preparation technology's concrete technological parameter is determined according to barrier material.
10. a kind of high-obstruct base material membrane according to claim 9, wherein draw ratio is less than 18 times, and generally the longitudinal stretching multiplying power is 2.5-5 times, and the cross directional stretch multiplying power is 3-7 times, and preferred longitudinal stretching multiplying power is 2.5-4.5 times, the cross directional stretch multiplying power is 3-6 times.
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2005
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