CN101722700A - Low-haze multi-layer co-extrusion two-way stretching polyamide film and preparation method - Google Patents
Low-haze multi-layer co-extrusion two-way stretching polyamide film and preparation method Download PDFInfo
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Abstract
The invention provides a low-haze multi-layer co-extrusion two-way stretching polyamide film and a preparation method. The two-way stretching polyamide film comprises at least three co-extrusion structures, namely a surface layer A, a surface layer C and a middle layer B, wherein the surface layer A and the surface layer C contain antiblocking agents. The invention also discloses a preparation method of the two-way stretching polyamide film, comprising the following steps of: preparing polyamide raw materials, extruding, casting pieces, thermoforming, slacking, drawing, winding, and the like. The two-way stretching polyamide film has the advantages of low haze, high gloss and high transparency and can be widely applied to the field of the packaging industry.
Description
Technical field
The present invention relates to packet industry, particularly a kind of low haze, high gloss, good two-way stretching polyamide film and the preparation method of processing characteristics.
Background technology
Polyamide film also claims nylon film, and it has good mechanical performance, dimensional stability, hear resistance, oil resistivity, solvent resistance, paracentesis resistance and gas barrier property, therefore is widely used in packet industry.
But polyamide is a kind of polymer of very easily crystallization, exists stronger hydrogen bond action between its molecule, so that the viscosity of polyamide film and plasticity are very responsive for variations in temperature.Therefore, be drawn in the process of film polyamide being cast sheet, if on the big molecular level of polyamide, produced too much crystallization bulky grain because temperature control is improper, will be in follow-up drawing process, cause production accidents such as film stretching difficulty, rupture of membranes, film fracture, thereby greatly increase the production cost of enterprise, and the factor of merit of product is reduced, manufacturing enterprise is on a sticky wicket in market competition.
In order to enlarge the elasticity of biaxial tension operation, reduce the operation easier of biaxial tension, industry has also been made some effort, and the most frequently used is the roughness that improves film surface by the adding additive.For example the file of Chinese patent 96105765.3 discloses a kind of polyamide-based film of biaxial stretching, be to adopt 20%～70% polyolefin to join in 100% the aliphatic polyamide raw material to form copolymer mixture, be used for improving the performance of stretch process, so that make more smooth, the better film of elongation strain performance.
Yet these additives that are used at present, when having improved film take-up and having cut performance, also may cause the film mist degree to raise (mist degree is meant the unintelligible or muddy degree of film, is owing to film surface produces scattering of light with inner), cause transparency to descend.On the other hand, packaging industry has very big demand to low haze, high polyamide film transparent, high gloss for a long time, and this kind film can make surface of package have more attraction, thereby stimulates consumer to the desire to purchase of this packaging product.Therefore, be badly in need of a kind of more two-way stretching polyamide film of low haze, better transparency that has at present, to adapt to the urgent demand of packaging Industry Market.
Summary of the invention
The multi-layer co-extrusion two-way stretching polyamide film that the purpose of this invention is to provide a kind of low haze is to solve the high problem of existing polyamide film mist degree.
Another object of the present invention provides a kind of preparation method of multi-layer co-extrusion two-way stretching polyamide film of low haze, to solve the high problem of polyamide film mist degree that prior preparation method produces.
The present invention proposes a kind of multi-layer co-extrusion two-way stretching polyamide film of low haze, it comprises top layer A, top layer C and the intermediate layer B that is made of polyamide raw materials, described top layer A and described top layer C lay respectively at the both sides of intermediate layer B, and intermediate layer B, top layer A and top layer C form coextruded structure jointly, described top layer A, top layer C and intermediate layer B include a kind of additive, and described additive comprises the silica of a kind of glue or chain at least.
According to the multi-layer co-extrusion two-way stretching polyamide film of the described low haze of preferred embodiment of the present invention, the silica in the described additive can be nanometer grade silica, and its size is less than 100 nanometers.
Comprise nanometer grade silica and micron silica according to the silica in the described additive of multi-layer co-extrusion two-way stretching polyamide film of the described low haze of preferred embodiment of the present invention, the size of described nanometer grade silica is less than 100 nanometers, and the size of described micron silica is at the 0.5-5.0 micron.
According to the multi-layer co-extrusion two-way stretching polyamide film of the described low haze of preferred embodiment of the present invention, the thickness of described top layer A and described top layer C is in the 0.2-2.5 micrometer range.
According to the multi-layer co-extrusion two-way stretching polyamide film of the described low haze of preferred embodiment of the present invention, the total thickness of intermediate layer B, top layer A and top layer C is in the 6-40 micrometer range, and the thickness of described intermediate layer B accounts for the 50%-90% of gross thickness.
The present invention proposes a kind of preparation method of multi-layer co-extrusion two-way stretching polyamide film of low haze in addition, it may further comprise the steps: (1) extrudes operation: add a kind of additive in polyamide raw materials, in extruder, extrude a polyamide diaphragm by a co-extrusion die head after the fusion then, described polyamide diaphragm comprises a top layer A, a top layer C and an intermediate layer B, and described additive comprises the silica of a kind of glue or chain at least.(2) casting sheet operation: the polyamide diaphragm is cooled to below 50 ℃.(3) longitudinal stretching operation: the polyamide diaphragm is controlled in 45-80 ℃ the temperature range and carries out longitudinal stretching.(4) cross directional stretch operation: the polyamide diaphragm is controlled in 90-160 ℃ the temperature range and carries out cross directional stretch, and form polyamide film.(5) heat-setting process: polyamide film is controlled in 150-250 ℃ the scope and finalizes the design.
Preparation method according to the multi-layer co-extrusion two-way stretching polyamide film of the described low haze of preferred embodiment of the present invention, it also comprises drying process: the polyamide raw materials that will add additive is carried out vacuum drying, and moisture content is controlled in the 500-1500ppm scope.
Preparation method according to the multi-layer co-extrusion two-way stretching polyamide film of the described low haze of preferred embodiment of the present invention, after to the biaxial tension of polyamide diaphragm, also further comprise step: the polyamide film after stretching is carried out sided corona treatment, the surface tension of film is reached more than the 52mN/m.
According to the preparation method of the multi-layer co-extrusion two-way stretching polyamide film of the described low haze of preferred embodiment of the present invention, the silica in the described additive comprises the nanometer grade silica of size less than 100 nanometers.
With respect to prior art, the invention has the beneficial effects as follows:
1, the present invention is by adding the additive that contains silica in polyamide raw materials, significantly reduced the gap that exists on the polyamide diaphragm, thereby make polyamide film can possess the good optical performance, for example very low mist degree, very high glossiness and transparency etc.
2, in the additive of the present invention, both contain nano level silica, can contain micron-sized silica again, thereby made polyamide film on the basis of low haze, possessed good processing properties again, particularly the splitting winding performance.
3, the present invention can also carry out sided corona treatment to film after to the polyamide film biaxial tension, makes film surface have stronger tension force, helps improving the production yield of polyamide film, and improves the toughness in the film use.
Certainly, implement arbitrary product of the present invention and might not need to reach simultaneously above-described all advantages.
Description of drawings
Fig. 1 is a kind of embodiment flow chart of the multi-layer co-extrusion two-way stretching polyamide film preparation method of low haze of the present invention.
The specific embodiment
Main thought of the present invention is to add to contain the additive of silica in polyamide raw materials, because good caking property is arranged between silica and the polyamide, therefore can make the space on the film less after the polyamide diaphragm stretches.And, make that therefore the polyamide film that is added with silica can possess the good optical performance, for example very low mist degree, very high glossiness and transparency etc. because the space is the main cause that causes the film mist degree to increase.And the silica dioxide granule that is adopted is more little, can make the space on the film few more, and then mist degree is then low more.
The multi-layer co-extrusion two-way stretching polyamide film of low haze of the present invention, it includes three-decker: top layer A, intermediate layer B and top layer C.Top layer A and top layer C lay respectively at the both sides of intermediate layer B, and the thickness of top layer A and top layer C can be identical, also can be different, and generally greater than 0.1 μ m, usually in the 0.2-2.5 mu m range, more fortunately in the 0.5-1.8 mu m range.The thickness of whole three-layer co-extruded two-way stretching polyamide film is generally in the 6-40 mu m range, more fortunately in the 10-25 mu m range.The thickness of intermediate layer B accounts for the 50%-90% of all thickness.And intermediate layer B, top layer A and top layer C form coextruded structure jointly.Here said coextruded structure is meant that the polymer of top layer A, intermediate layer B and top layer C extrudes through three screw extruders respectively, by entering operations such as casting sheet, stretching, thermal finalization behind the co-extrusion die head, finally forms multi-layer co-extruded polyamide film then.Wherein, the raw material of top layer A and top layer C can be different with intermediate layer B layer, but preferably use the polyamide raw materials identical with the B layer.
The present invention is used to produce the raw material of two-way stretching polyamide film, can be polyamide 6 (PA6 or title Nylon6), polyamide 66 (PA66 or title Nylon66) and copolyamide thereof etc., preferably PA6.The inherent viscosity RV of used polyamide 6 is generally 2.5-3.5, is preferably 2.8-3.0.The polyamide raw materials inherent viscosity that is used for top layer and intermediate layer can not differ greatly, in order to avoid produce flowing instability in the production process, makes film that striped be arranged.
In order to make polyamide film have better performance, additive used in the present invention can include but not limited to stabilizing agent, antistatic additive, lubricant, antioxidant, UV absorbers, antiblocking agent etc.These additives can adopt the method for female section, promptly add additive in polymerization process, also can adopt polymer-extruded melt blending to get method.
Wherein, antiblocking agent is divided into organic additive and inorganic additive, includes but not limited to calcium carbonate, silica, talcum powder, magnesium carbonate, brium carbonate, calcium phosphate, aluminium oxide, titanium dioxide, carbon black, kaolin, cross linked acrylic etc.The selected antiblocking agent of the present invention can adopt the above-mentioned additive of identical chemical composition, variable grain size, also can adopt the additive of two or more different chemical composition.These additives can adopt diverse ways, add in each layer of two-way stretching polyamide film with different concentration.The concentration of antiblocking agent is generally 0.01%-0.4% (percentage by weight) among top layer A and the top layer C, is preferably 0.04%-0.2%.The concentration of antiblocking agent is generally 0.001%-0.1% among the B of intermediate layer, is preferably 0.001%-0.02%.The content of whole film antiblocking agent is generally less than 0.2%, preferably less than 0.16%.
It should be noted that emphasis of the present invention just is all to have added the additive that contains silica among top layer A, intermediate layer B and the top layer C, can reduce the mist degree of polyamide film greatly, improve the transparency of film.And this silica can be glue or chain, and in order to improve the adhesion between additive and the polyamide, and reduce space on the stretched film, the used silica of the present invention can be a kind of nanometer grade silica, its size is generally less than 100nm, more fortunately in the 20-50nm scope.Simultaneously for to make made two-way stretching polyamide film that good processing properties be arranged, splitting winding performance particularly, the present invention also can adopt micron silica, and its size is generally at 0.5-5.0 μ m, more fortunately in the 1.0-2.5 mu m range.Among the present invention, nano level silica mainly can be applied among top layer A and the top layer C, and micron silica can be applied in each layer.
The present invention has proposed the preparation method of the multi-layer co-extrusion two-way stretching polyamide film of above-mentioned low haze in addition, sees also Fig. 1, and it may further comprise the steps:
S11, extrude operation: in polyamide raw materials, add a kind of additive, in extruder, extrude a polyamide diaphragm by a co-extrusion die head after the fusion then, described polyamide diaphragm comprises a top layer A, a top layer C and an intermediate layer B, and described additive comprises the silica of a kind of glue or chain at least.Used silica can be a kind of nanometer grade silica, and its size is generally less than 100nm, more fortunately in the 20-50nm scope.For to make made two-way stretching polyamide film that good processing properties be arranged, particularly the splitting winding performance also can adopt micron silica simultaneously, and its size is generally at 0.5-5.0 μ m, more fortunately in the 1.0-2.5 mu m range.Among the present invention, nano level silica mainly can be applied among top layer A and the top layer C, and micron silica can be applied in each layer.
In addition, polyamide raw materials can be carried out the vacuum drying operation before extruding, its moisture is remained in the 500-1500ppm scope, is preferably in the 800-1000ppm scope.
S12, casting sheet operation: the polyamide diaphragm is cooled to below 50 ℃, preferably less than 20 ℃.In order to obtain good casting sheet effect, can adopt static auxiliary casting sheet or the auxiliary casting of air-flow sheet, be preferably the auxiliary casting of static sheet.
S13, longitudinal stretching operation: the polyamide diaphragm is controlled in 45-80 ℃ the temperature range and carries out longitudinal stretching, can stretch by predefined different stretch multiplying power with the roller of two friction speeds, indulge and draw multiplying power to be generally 2.5: 1-5.0: 1, be preferably 3.0: 1-4.0: 1.Longitudinal stretching can one section carries out, and also can be divided into two sections and carry out.
S14, the cross directional stretch operation: the polyamide diaphragm is controlled in 90-160 ℃ the temperature range and carries out cross directional stretch, and form polyamide film, this process can be carried out in the baking oven of Band clamp.The multiplying power of cross directional stretch is generally 3.0: 1-5.0: 1, be preferably 3.5: 1-4.5: 1.
Especially, the sequencing of above-mentioned longitudinal stretching operation and cross directional stretch operation can be adjusted according to actual needs.And the longitudinal stretching that present embodiment adopts was a kind of preferred implementation before cross directional stretch, and its reason is an orientation of being convenient to the polyamide strand.
S15, heat-setting process: polyamide film is controlled in 150-250 ℃ the scope and finalizes the design, the time is generally 1-15 second.
Not only has the good optical performance by the prepared two-way stretching polyamide film of above-mentioned preparation method, for example very high glossiness and transparency, very low mist degree, and has a good machinability, particularly rolling is cut functional, see also table 1, it is for producing the parameter of polyamide film various features index:
Table 1
In order more in depth to understand the present invention, the inventor is by great deal of experiment data and experimental result, produce the parameter of the required the best of polyamide film of the present invention in order to proof, and disclose outstanding optical property that polyamide film of the present invention possesses and good machinability.
Following table 2 is polyamide raw materials that the inventor is adopted when testing.Wherein, contain silicon S350 (particle diameter is 1.8 μ m) 10% among female section 1 (viscosity RV=2.8), contain silicon OX-50 (particle diameter is 50nm) 1000ppm in female section 2.Above-mentioned female section all is to adopt polyamide 6 section and silica to extrude melt blending to make.
| Numbering | Raw material | Characteristic |
| ??V | Polyamide 6 section | ??RV＝3.0 |
| ??MB1 | Female section 1 | Contain silica (particle diameter is 1.8 μ m) 10% RV=2.8 |
| ??MB2 | Female section 2 | Contain silica (particle diameter is 50nm) 1000ppm RV=2.8 |
Table 2
Following E1-E4 is the experimental data that co-extrusion polyamide film of the present invention changes different material and parameter.
E1：
The three-layer co-extruded structure of ABC, wherein B layer in intermediate layer is raw materials used is 100% section V, top layer A layer and top layer C are raw materials used all to be the section MB1 of the section V and 1% (weight ratio) of 99% (weight ratio).Raw material melt extrudes through extruder through after the vacuum drying, three layers of raw material pass through co-extrusion die head, Electrostatic Absorption is at cold bulging direct casting sheet, sheet is made the polyamide film that thickness is 15 μ m through longitudinal stretching, cross directional stretch, thermal finalization, lax, traction, rolling, and wherein A layer and C layer thickness are 2 μ m.Film has very low mist degree, very high glossiness, but processing characteristics is bad, and the big film of rolling place is rolled up apparent a little longitudinal stripe that has.
E2：
The three-layer co-extruded structure of ABC, wherein B layer in intermediate layer is raw materials used is 100% section V, top layer A layer and table C are raw materials used all to be the section MB1 of the section V and 1.5% (weight ratio) of 98.5% (weight ratio).Raw material melt extrudes through extruder through after the vacuum drying, three layers of raw material pass through co-extrusion die head, Electrostatic Absorption is at cold bulging direct casting sheet, sheet is made the polyamide film that thickness is 15 μ m through longitudinal stretching, cross directional stretch, thermal finalization, lax, traction, rolling, and wherein A layer and C layer thickness are 2 μ m.Film has lower mist degree, higher glossiness, processing characteristics still can, rolling is normal substantially.
E3：
The three-layer co-extruded structure of ABC, wherein B layer in intermediate layer is raw materials used is the MB 1 of 99.84% section V and 0.16%, top layer A layer and C layer are raw materials used all to be the section V of 59.4% (weight ratio), the section MB2 of the section MB1 and 40% (weight ratio) of 0.6% (weight ratio).Raw material melt extrudes through extruder through after the vacuum drying, three layers of raw material pass through co-extrusion die head, Electrostatic Absorption is at cold bulging direct casting sheet, sheet is made the polyamide film that thickness is 15 μ m through longitudinal stretching, cross directional stretch, thermal finalization, lax, traction, rolling, and wherein A layer and C layer thickness are 2 μ m.Film has very low mist degree, very high glossiness, and processing characteristics is very good.
E4：
The three-layer co-extruded structure of ABC, wherein the raw material of intermediate layer B layer is 100% section V.Top layer A layer and C layer are raw materials used all to be the section V of 59.4% (weight ratio), the section MB2 of the section MB1 and 40% (weight ratio) of 0.6% (weight ratio).Raw material melt extrudes through extruder through after the vacuum drying, three layers of raw material pass through co-extrusion die head, Electrostatic Absorption is at cold bulging direct casting sheet, sheet is made the polyamide film that thickness is 25 μ m through longitudinal stretching, cross directional stretch, thermal finalization, lax, traction, rolling, and wherein A layer and C layer thickness are 3.5 μ m.Film has very low mist degree, very high glossiness, and processing characteristics is very good.
E5：
The three-layer co-extruded structure of ABC, wherein the raw material of intermediate layer B layer is by being that 99.84% section V and 0.16%MB1 forms.Top layer A layer and C layer are raw materials used all to be the section V of 72.47% (weight ratio), the section MB2 of the section MB1 and 27.0% (weight ratio) of 0.53% (weight ratio).Raw material melt extrudes through extruder through after the vacuum drying, three layers of raw material pass through co-extrusion die head, Electrostatic Absorption is at cold bulging direct casting sheet, sheet is made the polyamide film that thickness is 10 μ m through longitudinal stretching, cross directional stretch, thermal finalization, lax, traction, rolling, and wherein A layer and C layer thickness are 1 μ m.Film has very low mist degree, very high glossiness, and processing characteristics is very good.
Following table 3 is membrane structure parameters of embodiment E 1-E5.Table 4 is the film performance contrast of embodiment E 1-E5.
Table 3
| Numbering | Mist degree/% | Glossiness (60 °) | Coefficient of friction (moving) | The rolling performance | Cut performance |
| ??E1 | ??2.0 | ??185 | ??0.48 | ??× | ??× |
| ??E2 | ??2.5 | ??180 | ??0.45 | ??△ | ??△ |
| ??E3 | ??1.6 | ??191 | ??0.43 | ??◎ | ??◎ |
| Numbering | Mist degree/% | Glossiness (60 °) | Coefficient of friction (moving) | The rolling performance | Cut performance |
| ??E4 | ??1.7 | ??189 | ??0.43 | ??◎ | ??◎ |
| ??E5 | ??1.8 | ??195 | ??0.40 | ??◎ | ??◎ |
Table 4
Annotate:
◎: expression can roll banding, and rolling can be clamminess, and does not have longitudinal stripe, extraordinary processing characteristics.
Zero: expression can roll banding, and rolling can be clamminess, and does not have longitudinal stripe, good processing properties.
△: expression can roll banding, and rolling can be clamminess, and does not have longitudinal stripe, and processing characteristics still can.
*: expression can roll banding, and rolling can be clamminess, and a little longitudinal stripe is arranged, and processing characteristics is bad.
The present invention is by adding the additive that contains silica in polyamide raw materials, significantly reduced the gap that exists on the polyamide diaphragm, thereby make polyamide film can possess the good optical performance, for example very low mist degree, very high glossiness and transparency etc.
More than disclosed only be several specific embodiment of the present invention, but the present invention is not limited thereto, any those skilled in the art can think variation, all should drop in protection scope of the present invention.
Claims (9)
1. the multi-layer co-extrusion two-way stretching polyamide film of a low haze, it is characterized in that, comprise a top layer A, a top layer C and an intermediate layer B who constitutes by polyamide raw materials, described top layer A and described top layer C lay respectively at the both sides of intermediate layer B, and intermediate layer B, top layer A and top layer C form coextruded structure jointly, described top layer A, top layer C and intermediate layer B include a kind of additive, and described additive comprises the silica of a kind of glue or chain at least.
2. the multi-layer co-extrusion two-way stretching polyamide film of low haze as claimed in claim 1 is characterized in that, the silica in the described additive is nanometer grade silica, and its size is less than 100 nanometers.
3. the multi-layer co-extrusion two-way stretching polyamide film of low haze as claimed in claim 1, it is characterized in that, silica in the described additive comprises nanometer grade silica and micron silica, the size of described nanometer grade silica is less than 100 nanometers, and the size of described micron silica is at the 0.5-5.0 micron.
4. the multi-layer co-extrusion two-way stretching polyamide film of low haze as claimed in claim 1 is characterized in that, the thickness of described top layer A and described top layer C is in the 0.2-2.5 micrometer range.
5. the multi-layer co-extrusion two-way stretching polyamide film of low haze as claimed in claim 1 is characterized in that, the total thickness of intermediate layer B, top layer A and top layer C is in the 6-40 micrometer range, and the thickness of described intermediate layer B accounts for the 50%-90% of gross thickness.
6. the preparation method of the multi-layer co-extrusion two-way stretching polyamide film of a low haze is characterized in that, may further comprise the steps:
(1) extrudes operation: in polyamide raw materials, add a kind of additive, in extruder, extrude a polyamide diaphragm by a co-extrusion die head after the fusion then, described polyamide diaphragm comprises a top layer A, a top layer C and an intermediate layer B, and described additive comprises the silica of a kind of glue or chain at least;
(2) casting sheet operation: the polyamide diaphragm is cooled to below 50 ℃;
(3) longitudinal stretching operation: the polyamide diaphragm is controlled in 45-80 ℃ the temperature range and carries out longitudinal stretching;
(4) cross directional stretch operation: the polyamide diaphragm is controlled in 90-160 ℃ the temperature range and carries out cross directional stretch, and form polyamide film;
(5) heat-setting process: polyamide film is controlled in 150-250 ℃ the scope and finalizes the design.
7. the preparation method of the multi-layer co-extrusion two-way stretching polyamide film of low haze as claimed in claim 6, it is characterized in that, it also comprises drying process: the polyamide raw materials that will add additive is carried out vacuum drying, and moisture content is controlled in the 500-1500ppm scope.
8. the preparation method of the multi-layer co-extrusion two-way stretching polyamide film of low haze as claimed in claim 6, it is characterized in that, after to the biaxial tension of polyamide diaphragm, also further comprise step: the polyamide film after stretching is carried out sided corona treatment, the surface tension of film is reached more than the 52mN/m.
9. the preparation method of the multi-layer co-extrusion two-way stretching polyamide film of low haze as claimed in claim 6 is characterized in that, the silica in the described additive comprises the nanometer grade silica of size less than 100 nanometers.
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| CN108059824A (en) * | 2017-12-20 | 2018-05-22 | 贵州省材料产业技术研究院 | A kind of transparent flame-retarding high-temperature nylon and preparation method thereof |
| CN109666292A (en) * | 2018-12-14 | 2019-04-23 | 德州东鸿制膜科技有限公司 | BOPA film and preparation method thereof with high barrier and straight line easy-to-rupture |
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