CN112226076A - Ultra-high smooth polyamide master batch, polyamide film and preparation method thereof - Google Patents

Ultra-high smooth polyamide master batch, polyamide film and preparation method thereof Download PDF

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CN112226076A
CN112226076A CN202010947425.9A CN202010947425A CN112226076A CN 112226076 A CN112226076 A CN 112226076A CN 202010947425 A CN202010947425 A CN 202010947425A CN 112226076 A CN112226076 A CN 112226076A
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polyamide
ultra
master batch
high smooth
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刘运锦
贾露
李智尧
林新土
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Xiamen Changsu Industrial Co Ltd
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    • C08J2443/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium or a metal; Derivatives of such polymers
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Abstract

The invention discloses an ultrahigh smooth polyamide master batch, a polyamide film and a preparation method thereof, wherein the ultrahigh smooth polyamide film is sequentially provided with an upper surface layer, a core layer and a lower surface layer from top to bottom; the upper surface layer and the lower surface layer comprise 3-6 parts of ultra-high smooth polyamide master batch and 94-97 parts of polyamide resin by mass part; the core layer is composed of polyamide resin; wherein the ultra-high smooth polyamide master batch comprises, by mass, 0.5-10 parts of silicon-acrylic acid microspheres formed by copolymerizing organic silicon and acrylic acid, 0-10 parts of an opening agent and 80-99.5 parts of polyamide resin. The polyamide master batch and the polyamide film have lower friction coefficient, overcome the problem that the common slipping agent is easy to migrate, expand the application field of the polyamide film and have wide application prospect.

Description

Ultra-high smooth polyamide master batch, polyamide film and preparation method thereof
Technical Field
The invention belongs to the technical field of flexible packaging materials, and particularly relates to ultra-high smooth polyamide master batches, a polyamide film and a preparation method thereof.
Background
Biaxially oriented polyamide films (BOPA) are obtained from various nylon raw materials through a biaxial orientation process, have the advantages of excellent mechanical strength, barrier property, puncture resistance, transparency, oil resistance, chemical solvent resistance, no toxicity and the like, and are widely applied to the fields of food packaging, lithium battery flexible packaging, medicine bags and the like. Biaxially oriented polyamide films are rarely used alone in practice and are usually combined with other films by glue. For example, in the field of food packaging, a composite film with a PA/PE structure can be adopted, and the excellent puncture resistance of a BOPA film and the heat sealing performance of PE are utilized to be used for meat freezing packaging, so that the packaging bag can be prevented from being punctured by sharp bones; the composite film with a PA/PET/PE structure can also be adopted, and the excellent mechanical properties of BOPA and BOPET and the heat sealing property of PE are utilized, so that the composite film can be used for packaging heavy objects such as rice, washing powder and the like; the composite film with the structure of PA// PET// AL// PE can also be used for products with special requirements on barrier property, such as sauce packaging and the like. In the field of lithium battery flexible packaging and medicine packaging, a composite film with a PA// AL// CPP structure is generally adopted, and the composite film is endowed with deeper 'pit punching depth' by utilizing the excellent flexibility characteristic of BOPA.
Because the film has self-adhesion, in the BOPA production process, a three-layer co-extrusion technology is usually adopted, and master batch is added into two outer surface layers to prevent the film from being continuously broken. But in the actual application process, the problem that the composite film is difficult to page in the code spraying process can be solved due to the lower friction coefficient; in the field of lithium battery flexible packages and medicine packages, the lower friction coefficient has deeper 'punching depth'. In order to reduce the friction coefficient, small molecule type slipping agents can be added, and the small molecule slipping agents can be transferred to the printing surface of the film under the influence of the environment (particularly high-temperature weather) during the transportation and storage of the film, so that the surface tension is reduced, and the printing and compounding effects are influenced. Crosslinked microspheres such as organic silicon can also be added, but the surface of the single crosslinked microspheres is too smooth and can fall off and transfer under the action of external force such as friction, so that the product quality is influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides the ultra-high smooth polyamide master batch, the polyamide film and the preparation method thereof, and solves the problems in the background art.
One of the technical schemes adopted by the invention for solving the technical problems is as follows: provides an ultra-high smooth polyamide master batch, which comprises 0.5 to 10 parts of silicon-acrylic acid microspheres, 0 to 10 parts of opening agent and 80 to 99.5 parts of polyamide resin by weight; the silicon-acrylic acid microspheres are copolymer particles of organic silicon and acrylic acid, the average particle size D50 is 2-5 mu m, and the average particle size D50 of the opening agent is 2-5 mu m.
The preparation method of the ultra-high smooth polyamide master batch comprises the following steps: mixing silicon-acrylic acid microspheres, a shedding agent and polyamide resin, adding the mixture into an extruder with the temperature of 185-285 ℃ for melting, and then splitting through a porous die head; then cooling in a water tank with the water temperature of 30-55 ℃ and granulating by a granulator; and finally, sucking the mixture into a drying oven at the temperature of 60-90 ℃ for drying and packaging to prepare the ultra-high smooth polyamide master batch.
The technical scheme adopted by the invention for solving the technical problems is as follows: the ultra-high smooth polyamide film is provided with an upper surface layer, a core layer and a lower surface layer from top to bottom in sequence;
the upper surface layer comprises 3-6 parts of ultra-high smooth polyamide master batch and 94-97 parts of polyamide resin in parts by mass;
the core layer is composed of polyamide resin;
the lower surface layer comprises 3-6 parts of ultra-high smooth polyamide master batch and 94-97 parts of polyamide resin by mass;
wherein the ultra-high smooth polyamide master batch comprises, by mass, 0.5-10 parts of silicon-acrylic acid microspheres, 0-10 parts of an opening agent and 80-99.5 parts of polyamide resin; the silicon-acrylic acid microspheres are copolymer particles of organic silicon and acrylic acid, the average particle size D50 is 2-5 mu m, and the average particle size D50 of the opening agent is 2-5 mu m.
In a preferred embodiment of the present invention, an ultra-high slip polyamide film has a thickness of 15-30 μm.
The preparation method of the ultra-high smooth polyamide film comprises the following steps:
step one, respectively melting polyamide resin and ultrahigh smooth polyamide master batch on an upper surface layer, polyamide resin on a core layer, polyamide resin and ultrahigh smooth polyamide master batch on a lower surface layer by respective extruders in a feeding scale supply mode at the temperature of 220-285 ℃, uniformly flowing out through a T-shaped die head, and cooling on a quenching roller at the temperature of 25-55 ℃ to form an unstretched sheet;
step two, cleaning and plasticizing the unstretched sheet, and synchronously stretching the unstretched sheet at the temperature of 190 ℃ and 250 ℃ by using a linear motor track;
and step three, performing heat setting on the film stretched in the step two at the temperature of 190-260 ℃ to obtain the ultra-high smooth polyamide film.
Compared with the background technology, the technical scheme has the following advantages:
1. the friction coefficient COF of the ultra-high smooth polyamide film is less than or equal to 0.2, the ultra-high smooth polyamide film is particularly suitable for being applied in special fields, such as southwest areas (high-temperature and high-humidity environments), and the problem that the composite film is difficult to page in the code spraying process can be solved; as applied to the fields of lithium battery flexible packages and medicine packages, the lower friction coefficient has deeper 'pit punching depth';
2. the silicon-acrylic acid microspheres are copolymer particles of organic silicon and acrylic acid, the average particle size D50 is 2-5 mu m, and good compatibility between the acrylic acid and polyamide is utilized, so that the film is endowed with smooth characteristic and the microspheres are prevented from being rubbed and falling off; the problem that the single organic silicon crosslinked microspheres fall off due to external friction force is solved, and the problem that the corona surface corona is reduced due to the migration of the micromolecule slipping agent under the high-temperature condition is also solved;
3. according to the scheme, the silicon-acrylic acid microspheres are matched with other opening agents such as silicon dioxide and the like, so that the adhesion force of the film can be reduced, and the film is prevented from being adhered and broken; the friction coefficient is adjusted within a certain range by adjusting the proportion of the two components, and the application field of the friction coefficient is expanded.
Drawings
FIG. 1 is a layer structure diagram of the ultra-high-slip polyamide films of examples 1 to 4.
Wherein, 10-upper surface layer, 20-core layer, 30-lower surface layer.
Detailed Description
The terms "upper" and "lower" are used in an orientation or positional relationship shown in the drawings only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
The silicon-acrylic acid microspheres in the ultra-high smooth polyamide master batch are copolymer particles of organic silicon and acrylic acid, wherein the molar ratio of the organic silicon to the acrylic acid monomers is 50: 70-50: 30, can be prepared by emulsion polymerization, hydrosilylation, free radical copolymerization and other methods, such as polysiloxane graft modified polyacrylate polymer emulsion, and then the microspheres are formed by liquid spray drying; commercially available silicon-acrylic copolymer resins meeting the compounding ratio requirements can also be purchased and ball milled to obtain the desired size, and for example, the silicon-acrylic microspheres used in the examples are CHALINE R170S from Ningyue chemical industries, Inc., which has an organosilicon content of 70% and an average particle diameter of 30 μm and is ball milled to 3 μm.
The opening agent is one or more of silicon dioxide, calcium carbonate, talcum powder, magnesium oxide, zinc oxide, phosphogypsum powder and crosslinked PMMA micro powder.
In the following examples or comparative examples, the preparation method of each functional master batch (including ultra-high smooth polyamide master batch and anti-sticking master batch) is as follows:
the raw materials are melted by a double-screw extruder according to the component ratio in a feeding scale feeding mode, are subjected to splitting by a porous die head, are cooled in a water tank, are cut into granules by a granulator, are sucked into an oven, and are packaged after being dried. Wherein the temperature of the extruder is 185-285 ℃, the rotating speed of the extruder is 400-550 r/min, the water temperature of the water tank is 30-55 ℃, the temperature of the oven is 60-90 ℃, and the moisture of the master batch is less than or equal to 1500 ppm.
In the following examples or comparative examples, the polyamide films (including ultra-high slip polyamide films, polyamide films) were prepared by the following method:
the method comprises the following steps: melting the components in the upper surface layer, the core layer and the lower surface layer in a feeding scale supply mode according to a proportion at 220-285 ℃, uniformly flowing out through a T-shaped die head, and cooling on a quenching roller at 25-55 ℃ to form an unstretched sheet, wherein the thickness of the unstretched sheet is preferably 150-500 mu m;
step two: and after the unstretched sheet is washed by water and plasticized, synchronously stretching the unstretched sheet at the temperature of 190-250 ℃ by using a linear motor track, wherein the stretching multiplying power is preferably 3.0-3.5.
Step three: and (3) performing heat setting on the film stretched in the step two at the temperature of 190-260 ℃ to finally obtain the nylon film, wherein the heat setting time is preferably 40-120s, and the film thickness is preferably 15-30 μm.
Examples 1 to 4
The ultra-high slip polyamide films of examples 1-4 were of a three-layer structure comprising an upper skin layer 10, a core layer 20 and a lower skin layer 30. The concrete components are as follows:
TABLE 1 EXAMPLES 1-4 ULTRA-HIGH SLIDING POLYAMIDE FILM AND MASTER BATCH
Figure BDA0002675780940000051
Comparative example 1
A biaxially oriented nylon 6 film having a thickness of 15 μm was commercially available.
Comparative examples 2 to 7
The polyamide films of comparative examples 2-7, again of three-layer construction, comprised an upper skin layer, a core layer and a lower skin layer. The concrete components are as follows:
TABLE 2 COMPARATIVE EXAMPLES 2-7 POLYAMIDE FILM AND MASTER BATTERY
Figure BDA0002675780940000061
The polyamide films of examples 1-4 and comparative examples 1-7 were tested by:
coefficient of friction: testing according to GB10006-88 standard;
adhesion force: testing the adhesion force of the non-corona surface and the non-corona surface according to the ASTM D3354 standard;
light transmittance and haze: testing according to GBT 2410-2008 standard;
and (3) testing the depth of a punched hole: the PA/AL/CPP composite film is prepared by the polyamide films of the examples and the comparative examples, a pit punching mold used in a lithium ion battery aluminum-plastic packaging film factory is used for clamping the PA/AL/CPP composite film, and pit punching heads with different depths are used for testing the film until the film is broken.
Pit transfer test: the polyamide films of examples and comparative examples were clamped by using a punching die used in a lithium ion battery aluminum plastic packaging film factory, and the film was tested by using a punching head of the same depth, and the film was repeated 1000 times to observe whether or not the die had a transferred matter, and if so, the film was marked with a "Δ", and if not, the film was marked with a "o".
Corona attenuation: a sample of A4 size film was taken 20 sheets and dried in an oven environment at 60 ℃ for 10 days and the difference between the initial and final surface tension values of the corona side of the film was recorded.
The test results are shown in the following table:
table 3 examples 1-4 performance test tables
Item Example 1 Example 2 Example 3 Example 4
Average thickness/μm 15 15 15 15
Coefficient of friction 0.18 0.15 0.14 0.09
Adhesion force/N 1.4 1.3 1.3 1.7
Haze/% 2.0 2.2 2.5 1.4
Transmittance (a) 92.3 92.3 92.3 92.3
Depth of pit/mm 5.6 5.6 5.7 5.9
Pit transfer ○ ○ ○ ○
Corona decay/dyn 4 4 4 4
TABLE 4 TEST TABLE FOR COMPARATIVE EXAMPLES 1-7
Item Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5 Comparative example 6 Comparative example 7
Average thickness/μm 15 15 15 15 15 15 15
Coefficient of friction 0.46 0.45 0.46 0.45 0.24 0.26 0.42
Adhesion force/N 1.6 1.7 1.5 1.8 1.3 1.2 1.6
Haze/% 3.0 2.9 3.1 2.8 3.2 2.7 3.0
Transmittance (a) 92.3 92.3 92.3 92.3 92.3 92.3 92.3
Depth of pit/mm 5.0 5.1 5.0 4.9 5.6 5.5 4.9
Pit transfer ○ ○ ○ ○ ○ △ △
Corona decay/dyn 10 10 11 8 14 4 4
As can be seen from the above table, the friction coefficients of the polyamide films of examples 1-4 were less than COF ≦ 0.2, and the friction coefficients decreased as the content of the silicon-acrylic microspheres increased. From examples 1-4 and comparative examples 1-7, it can be seen that the pits of examples 1-4 are deeper, the corona attenuation is reduced, and no powder is transferred after pit punching is repeated; from comparative example 5, it was found that changing the structure of the migrating slipping agent can lower the friction coefficient, but the corona decay becomes severe; from comparative example 6, it was found that the untreated silicone particles were transferred by repeated cratering and external force such as friction; from comparative example 7, it is understood that when the particle size of the opening agent is much larger than that of the silicon-acrylic microspheres, the friction coefficient becomes large.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. The ultra-high smooth polyamide master batch is characterized in that: according to the mass portion, the coating comprises 0.5-10 portions of silicon-acrylic acid microspheres, 0-10 portions of opening agent and 80-99.5 portions of polyamide resin; the silicon-acrylic acid microspheres are copolymer particles of organic silicon and acrylic acid, the average particle size D50 is 2-5 mu m, and the average particle size D50 of the opening agent is 2-5 mu m.
2. The ultra-high smooth polyamide masterbatch of claim 1, characterized in that: the opening agent is one or more of silicon dioxide, calcium carbonate, talcum powder, magnesium oxide, zinc oxide, phosphogypsum powder and crosslinked PMMA micro powder.
3. The method for preparing an ultra-high smooth polyamide masterbatch as claimed in any one of claims 1-2, wherein: mixing silicon-acrylic acid microspheres, a shedding agent and polyamide resin, adding the mixture into an extruder with the temperature of 185-285 ℃ for melting, and then splitting through a porous die head; then cooling in a water tank with the water temperature of 30-55 ℃ and granulating by a granulator; and finally, sucking the mixture into a drying oven at the temperature of 60-90 ℃ for drying and packaging to prepare the ultra-high smooth polyamide master batch.
4. An ultra-high smooth polyamide film characterized by: an upper surface layer, a core layer and a lower surface layer are sequentially arranged from top to bottom;
the upper surface layer comprises 3-6 parts of ultra-high smooth polyamide master batch and 94-97 parts of polyamide resin in parts by mass;
the core layer is composed of polyamide resin;
the lower surface layer comprises 3-6 parts of ultra-high smooth polyamide master batch and 94-97 parts of polyamide resin by mass;
wherein the ultra-high smooth polyamide master batch comprises, by mass, 0.5-10 parts of silicon-acrylic acid microspheres, 0-10 parts of an opening agent and 80-99.5 parts of polyamide resin; the silicon-acrylic acid microspheres are copolymer particles of organic silicon and acrylic acid, the average particle size D50 is 2-5 mu m, and the average particle size D50 of the opening agent is 2-5 mu m.
5. The ultra-high slip polyamide film as claimed in claim 4, wherein: the opening agent is one or more of silicon dioxide, calcium carbonate, talcum powder, magnesium oxide, zinc oxide, phosphogypsum powder and crosslinked PMMA micro powder.
6. The ultra-high slip polyamide film as claimed in claim 4, wherein: the ultra-high smooth polyamide film is 15-30 mu m.
7. The process for producing an ultra-high smooth polyamide film as claimed in any one of claims 4 to 6, wherein: the method comprises the following steps:
step one, respectively melting polyamide resin and ultrahigh smooth polyamide master batch on an upper surface layer, polyamide resin on a core layer, polyamide resin and ultrahigh smooth polyamide master batch on a lower surface layer by respective extruders in a feeding scale supply mode at the temperature of 220-285 ℃, uniformly flowing out through a T-shaped die head, and cooling on a quenching roller at the temperature of 25-55 ℃ to form an unstretched sheet;
step two, cleaning and plasticizing the unstretched sheet, and synchronously stretching the unstretched sheet at the temperature of 190 ℃ and 250 ℃ by using a linear motor track;
and step three, performing heat setting on the film stretched in the step two at the temperature of 190-260 ℃ to obtain the ultra-high smooth polyamide film.
8. The method for preparing an ultra-high smooth polyamide film according to claim 7, wherein: in the first step, the thickness of the prepared unstretched sheet is 150-500 μm.
9. The method for preparing an ultra-high smooth polyamide film according to claim 7, wherein: in the second step, the drawing ratio is 3.0 × 3.0 to 3.5 × 3.5.
10. The method for preparing an ultra-high smooth polyamide film according to claim 7, wherein: in the third step, the heat setting time is 40-120 s.
CN202010947425.9A 2020-09-10 2020-09-10 Ultra-high smooth polyamide master batch, polyamide film and preparation method thereof Pending CN112226076A (en)

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