CN114231203A - High-unwinding, no-precipitation and high-haze self-adhesive polyethylene protective film and preparation method thereof - Google Patents

High-unwinding, no-precipitation and high-haze self-adhesive polyethylene protective film and preparation method thereof Download PDF

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CN114231203A
CN114231203A CN202111484330.9A CN202111484330A CN114231203A CN 114231203 A CN114231203 A CN 114231203A CN 202111484330 A CN202111484330 A CN 202111484330A CN 114231203 A CN114231203 A CN 114231203A
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temperature
zone
protective film
haze
film
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CN114231203B (en
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文斌森
魏洪媚
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Jiangmen Hualong Membrane Materials Co ltd
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Jiangmen Hualong Membrane Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/29—Laminated material
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04—Homopolymers or copolymers of ethene
    • C09J123/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/16—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer
    • C09J2301/162—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer the carrier being a laminate constituted by plastic layers only
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2423/00—Presence of polyolefin
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2423/00—Presence of polyolefin
    • C09J2423/04—Presence of homo or copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2423/00—Presence of polyolefin
    • C09J2423/04—Presence of homo or copolymers of ethene
    • C09J2423/046—Presence of homo or copolymers of ethene in the substrate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to the technical field of optical protective films, and provides a self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze and a preparation method thereof. According to the invention, through the selection and matching of the raw materials, the surface of the film material is regularly and densely distributed in convex-concave points, and when the film material is uncoiled and peeled, the bonding surface of the adhesive layer and the back layer of the film material cannot generate microscopic vacuum negative pressure, so that the purposes of easy uncoiling and adhesion prevention are achieved; in addition, silicone master batches are not added into the protective film, so that the precipitation phenomenon cannot occur in use; the inner layer of the protective film is made of high-haze high-pressure low-density polyethylene, so that the protective film has high haze and shows a good matte effect. The invention also provides a preparation method of the self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze, which is characterized in that the air temperature of the cooling film bubble is controlled to be 20-25 ℃, and the cooling speed of the film bubble is reduced by increasing the air temperature, so that the protective film achieves the required haze.

Description

High-unwinding, no-precipitation and high-haze self-adhesive polyethylene protective film and preparation method thereof
Technical Field
The invention relates to the technical field of optical protective films, in particular to a self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze and a preparation method thereof.
Background
The polarizer is widely used in the fields of photoelectric display, sunglasses, anti-glare goggles, filters of photographic equipment, polarizing microscopes, 3D glasses, special medical glasses, etc., wherein the application is the largest in market scale and production value of photoelectric display.
In order to prevent contamination or damage of the surface of the polarizer during the manufacturing and transportation of the polarizer, a protective film is attached to the surface of the polarizer. The protective film is generally formed by three layers integrally, and comprises an adhesive layer, a core layer and a back adhesive layer, when in actual production, the protective film is usually rolled into a cylinder, and under a larger rolling pressure, a combined surface of the adhesive layer and the back adhesive layer is tightly pressed, so that the protective film is not easy to unwind after being rolled, and the film is easy to stretch and deform when in use.
The patent CN112430436A discloses a high easy unwinding self-adhesion protection film, and this protection film includes adhesive linkage, intermediate level and antiseized layer, and the adhesive linkage raw materials include thermoplastic elastomer material and tackifying resin, and the intermediate level raw materials include polypropylene random copolymer resin, and antiseized layer raw materials include high density polyethylene, low density polyethylene and antiseized masterbatch, and antiseized masterbatch is the silicone masterbatch. The protective film has good unwinding property, but when the film is applied at the later stage due to the addition of the silicone master batch, low molecular compounds can be separated out or air bubbles can be generated in the film material due to high temperature of a butt-jointed object or long film pasting time, and residues are left on the surface of the protective object after the protective film is removed to form ghost.
Disclosure of Invention
In view of the above, the invention provides a self-adhesive polyethylene protective film with high unwinding, no precipitation and high haze and a preparation method thereof. The self-adhesive polyethylene protective film provided by the invention is not added with silicone master batch, the obtained protective film has no precipitation phenomenon, is easy to unwind, and has a better matte effect (namely high haze).
In order to achieve the above object, the present invention provides the following technical solutions:
a self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze is prepared by co-extruding and blowing the outer layer, the middle layer and the inner layer;
the outer layer is prepared from metallocene low-density polyethylene and polyolefin plastomer; the mass ratio of the metallocene low-density polyethylene to the polyolefin plastomer is 6-17: 4-15;
the preparation raw material of the middle layer is first high-pressure low-density polyethylene; the melt index of the first high-pressure low-density polyethylene is 0.5-1.5 g/10 min; the density is 0.920-0.930 g/cm 3;
the inner layer is prepared from a second high-pressure low-density polyethylene; the second high pressure low density polyethylene is high haze high pressure low density polyethylene; the melt index of the high-haze high-pressure low-density polyethylene is 1.0-2.0 g/10min, and the density is 0.920-0.930 g/cm 3.
Preferably, in the raw materials for preparing the outer layer, the melt index of the metallocene low-density polyethylene is 0.8-1.5 g/10min, and the density is 0.910-0.915 g/cm 3;
in the preparation raw materials of the outer layer, the melt index of the polyolefin plastomer is 2.5-4 g/10min, and the density is 0.870-0.900 g/cm 3.
Preferably, the mass ratio of the outer layer to the middle layer to the inner layer is 10-15: 30-50: 40-70.
Preferably, the haze of the protective film is more than or equal to 18%.
Preferably, the method comprises the following steps:
respectively feeding the outer layer preparation raw material, the middle layer preparation raw material and the inner layer preparation raw material into an outer layer extruder, a middle layer extruder and an inner layer extruder for melting and plasticizing, filtering the obtained molten gel, conveying the filtered molten gel to a die head, extruding and blowing a film, forming film bubbles, blowing out the film bubbles from the die head, and cooling the blown film bubbles through an automatic air ring at the die head to obtain the self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze; the air temperature of the automatic air ring is 20-25 ℃.
Preferably, the outer layer extruder, the middle layer extruder and the inner layer extruder are all provided with 6 heating zones, and the heating zones are sequentially marked as a first zone to a sixth zone according to the passing sequence of raw materials; the die head is provided with 4 heating zones which are sequentially marked as a first zone to a fourth zone according to the passing sequence of the raw materials;
the temperature of the first zone of the outer layer extruder is 170-175 ℃, the temperature of the second zone is 175-180 ℃, the temperature of the third zone is 175-180 ℃, the temperature of the fourth zone is 175-180 ℃, the temperature of the fifth zone is 175-180 ℃, and the temperature of the sixth zone is 175-180 ℃;
the temperature of the first zone of the middle layer extruder is 160-165 ℃, the temperature of the second zone is 165-170 ℃, the temperature of the third zone is 165-170 ℃, the temperature of the fourth zone is 165-170 ℃, the temperature of the fifth zone is 160-165 ℃ and the temperature of the sixth zone is 160-165 ℃;
the temperature of the inner layer extruder in the first area is 155-160 ℃, the temperature of the second area is 160-165 ℃, the temperature of the third area is 160-165 ℃, the temperature of the fourth area is 160-165 ℃, the temperature of the fifth area is 160-165 ℃ and the temperature of the sixth area is 160-165 ℃;
the temperature of the first area of the die head is 170-175 ℃, the temperature of the second area is 175-180 ℃, the temperature of the third area is 175-180 ℃, and the temperature of the fourth area is 175-180 ℃.
Preferably, the extrusion pressure of the outer layer extruder, the middle layer extruder and the inner layer extruder is 15-40 MPa independently.
The preparation method of claim 5, wherein after the bubble is cooled, the steps of bubble stabilization, thickness measurement, traction, flaw detection, edge cutting, static electricity removal and winding are sequentially carried out.
The invention provides a self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze, which is prepared by co-extruding and blowing films of an outer layer, a middle layer and an inner layer; the outer layer is prepared from metallocene low-density polyethylene and polyolefin plastomer; the mass ratio of the metallocene low-density polyethylene to the polyolefin plastomer is 6-17: 4-15; the preparation raw material of the middle layer is first high-pressure low-density polyethylene; the melt index of the first high-pressure low-density polyethylene is 0.5-1.5 g/10 min; the density is 0.920-0.930 g/cm3(ii) a The inner layer is prepared from a second high-pressure low-density polyethylene; the second high pressure low density polyethylene is high haze high pressure low density polyethylene; the melt index of the high-haze high-pressure low-density polyethylene is 1.0-2.0 g/10min, and the density is 0.920-0.930 g/cm3. The invention forms regular and dense convex-concave point arrangement on the surface of the membrane material by selecting and matching the preparation raw materials of the outer layer, the inner layer and the middle layer, and the adhesive layer and the back layer of the membrane material are arranged when the membrane material is uncoiled and peeledThe bonding surface can not generate microscopic vacuum negative pressure, thereby achieving the purposes of easy uncoiling and adhesion prevention; in addition, silicone master batches are not added into the protective film, so that the precipitation phenomenon cannot occur in use; in addition, the high-haze high-pressure low-density polyethylene is selected as the inner layer of the protective film, so that the protective film has high haze and shows a good matte effect.
The invention also provides a preparation method of the self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze, and in the preparation of the traditional protective film, in order to ensure the productivity, the cooling temperature of the film bubble is generally below 15 ℃, while the air temperature for cooling the film bubble is controlled to be 20-25 ℃, and the cooling speed of the film bubble is reduced by increasing the air temperature, so that the protective film achieves the required haze.
The example result shows that the high-unwinding, non-precipitation and high-haze polyethylene protective film provided by the invention has good unwinding performance, no precipitation phenomenon and haze of more than 19%.
Drawings
Fig. 1 is a microscopic view of the polyethylene protective film prepared in example 1.
Detailed Description
The invention provides a self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze, which is characterized by being prepared by co-extruding and blowing films of an outer layer, a middle layer and an inner layer.
In the invention, the raw materials for preparing the outer layer are metallocene low-density polyethylene and polyolefin plastomer; the mass ratio of the metallocene low-density polyethylene to the polyolefin plastomer is 6-17: 4-15,
the preparation raw material of the middle layer is first high-pressure low-density polyethylene; the melt index of the first high-pressure low-density polyethylene is 0.5-1.5 g/10 min; the density is 0.920-0.930 g/cm independently3；
The inner layer is prepared from a second high-pressure low-density polyethylene; the second high pressure low density polyethylene is high haze high pressure low density polyethylene; the melt index of the high-haze high-pressure low-density polyethylene is 1.0-2.0 g/10min, and the density is 0.920-0.930 g/cm3。
In the invention, the outer layer is a self-adhesive layer; the preparation raw materials of the outer layer are as follows: the mass ratio of the metallocene low-density polyethylene to the polyolefin plastomer is 6-17: 4-15, preferably 8-15: 5-12; the melt index of the metallocene low-density polyethylene is preferably 0.8-1.5 g/10min, more preferably 0.9-1.2 g/10min, and the density is preferably 0.910-0.915 g/cm3More preferably 0.912 to 0.913g/cm3In a specific embodiment of the invention, the metallocene low density polyethylene is preferably Sauter based 8112 brand metallocene low density polyethylene (melt index of 1.1/10min, density of 0.912 g/cm)3). In the invention, the melt index of the polyolefin plastomer (POP) is preferably 2.5-4 g/10min, more preferably 2.6-3.5 g/10min, and the density is preferably 0.870-0.900 g/cm3More preferably 0.880 to 0.890g/cm3. In the specific embodiment of the invention, the POP is preferably a Saudi base brand 8380 POP (melt index of 3.0g/10min, density of 0.880 g/cm)3). In the invention, the POP has high self-adhesion, and the melt index and the density of the POP are preferably controlled within the range, so that the self-adhesion of the outer layer can be improved.
In the invention, the preparation raw material of the middle layer is first high-pressure low-density polyethylene (LDPE); the melt index of the first high-pressure low-density polyethylene is 0.5-1.5 g/10min, preferably; the density is 0.920-0.930 g/cm3Preferably 0.9203-0.925 g/cm3In a particular embodiment of the invention, the LDPE is preferably a Saudi base grade HP0722NN LDPE (melt index of 0.75g/10min, density of 0.922 g/cm)3) (ii) a The first high-pressure low-density polyethylene selected by the invention has the characteristics of low crystal point and easiness in processing.
In the invention, the preparation raw material of the inner layer is second high-pressure low-density polyethylene; the second high pressure low density polyethylene is high haze high pressure low density polyethylene; the melt index of the high-haze high-pressure low-density polyethylene is 1.0-2.0 g/10min, preferably 1.3-1.5 g/10min, and the density is 0.920-0.930 g/cm3Preferably 0.923 to 0.925g/cm3In particular embodiments of the present invention, the high haze high pressure lowThe density polyethylene is preferably high haze high pressure low density polyethylene (melt index of 1.5g/10min, density of 0.924 g/cm) of Japanese Sumitomo brand F213-P3) Or high haze high pressure low density polyethylene (melt index 5g/10min, density 0.918 g/cm) of LB5000, LG chemical3). According to the invention, through selection and matching of the preparation raw materials of the outer layer, the middle layer and the inner layer, regular and dense convex-concave point arrangement is formed on the surface of the membrane material, and when the membrane material is uncoiled and peeled, microscopic vacuum negative pressure cannot be generated on the bonding surface of the adhesive layer and the back layer of the membrane material, so that the purposes of easy uncoiling and adhesion prevention are achieved.
In the invention, the mass ratio of the outer layer, the middle layer and the inner layer is preferably 10-15: 30-50: 40-70, and more preferably 12-13: 35-45: 45-65.
In the invention, the haze of the self-adhesive pure polyethylene protective film is preferably more than or equal to 18%, and more preferably 18.6-21.2%.
The invention also provides a preparation method of the self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze, which comprises the following steps:
respectively feeding the outer layer preparation raw material, the middle layer preparation raw material and the inner layer preparation raw material into an outer layer extruder, a middle layer extruder and an inner layer extruder for melting and plasticizing, filtering the obtained molten gel, conveying the filtered molten gel to a die head, extruding and blowing a film, forming film bubbles, blowing out the film bubbles from the die head, and cooling the blown film bubbles through an automatic air ring at the die head to obtain the self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze; the air temperature of the automatic air ring is 20-25 ℃.
In the invention, the outer layer extruder, the middle layer extruder and the inner layer extruder are preferably provided with 6 heating zones which are sequentially marked as a first zone to a sixth zone according to the passing sequence of raw materials; the die head is provided with 4 heating zones which are sequentially marked as a first zone to a fourth zone according to the passing sequence of the raw materials.
In the invention, the temperature of the first zone of the outer layer extruder is preferably 170-175 ℃, and more preferably 172-173 ℃; the temperature of the second zone is preferably 175-180 ℃, and more preferably 176-178 ℃; the temperature of the three zones is preferably 175-180 ℃, and more preferably 176-178 ℃; the temperature of the fourth zone is preferably 175-180 ℃, and more preferably 176-178 ℃; the temperature of the fifth area is preferably 175-180 ℃, and more preferably 176-178 ℃; the temperature of the sixth zone is preferably 175-180 ℃, and more preferably 176-178 ℃.
In the invention, the temperature of the first zone of the middle layer extruder is preferably 160-165 ℃, and more preferably 162-163 ℃; the temperature of the second zone is preferably 165-170 ℃, and more preferably 166-168 ℃; the temperature in the three zones is preferably 165-170 ℃, and more preferably 166-168 ℃; the temperature of the fourth zone is preferably 165-170 ℃, and more preferably 166-168 ℃; the temperature of the fifth area is preferably 160-165 ℃, and more preferably 162-163 ℃; the temperature of the sixth zone is preferably 160-165 ℃, and more preferably 162-163 ℃;
in the invention, the temperature of the first zone of the inner layer extruder is preferably 155-160 ℃, and more preferably 156-158 ℃; the temperature of the second zone is preferably 160-165 ℃, and more preferably 162-163 ℃; the temperature of the three zones is preferably 160-165 ℃, and more preferably 162-163 ℃; the temperature of the fourth zone is preferably 160-165 ℃, and more preferably 162-163 ℃; the temperature of the fifth area is preferably 160-165 ℃, and more preferably 162-163 ℃; the temperature of the six zones is preferably 160-165 ℃, and more preferably 162-163 ℃.
In the invention, the temperature of the first area of the die head is preferably 170-175 ℃, and more preferably 172-173 ℃; the temperature of the second zone is preferably 175-180 ℃, and more preferably 176-178 ℃; the temperature of the three zones is preferably 175-180 ℃, and more preferably 176-178 ℃; the temperature of the fourth zone is preferably 175-180 ℃, and more preferably 176-178 ℃.
In the invention, the extrusion pressure of the outer layer extruder, the middle layer extruder and the inner layer extruder is preferably 15-40 MPa, and more preferably 30-35 MPa independently.
In the invention, the preparation raw materials of the outer layer, the middle layer and the inner layer are melted and plasticized in an extruder, a melt enters a die head, is converged at a die core in the die head and is extruded from a die opening to form a film bubble, the film bubble is cooled by an automatic air ring at the die opening after being blown out, and the air temperature of the automatic air ring is 20-25 ℃, preferably 22-23 ℃. In the invention, the air flow has a cooling effect on the film bubble, when the air temperature is lower than 20 ℃, the cooling speed of the film bubble is high, but the haze of the product is reduced, the larger the air temperature is adjusted, the higher the haze is, but the cooling speed of the film bubble is low, the productivity is reduced, the air temperature is controlled to be 20-25 ℃, the protective film with the required haze can be obtained, and the higher productivity can be ensured.
In the invention, after the bubble is cooled, the bubble stabilizing, thickness measuring, drawing, flaw detection, edge cutting, static electricity removing and winding are preferably carried out in sequence.
In a specific embodiment of the invention, the multilayer co-extrusion equipment is preferably provided with a raw material dust removal device, an automatic batching device, an extruder (comprising an outer layer extruder, a middle layer extruder and an inner layer extruder), a filtering device, an automatic wind ring online thickness measuring device, a herringbone row, an upper traction rotating device, an online defect detection device, a static electricity removal device and a central winding device, and further comprises a guide roller and a traction clamping roller which are used for drawing the movement of a film. In the extrusion process, raw materials are dedusted by a raw material dedusting device, and then are respectively batched by an automatic batching device to obtain an outer layer material, a middle layer material and an inner layer material; the obtained outer layer material, the middle layer material and the inner layer material respectively enter an outer layer extruder, a middle layer extruder and an inner layer extruder for melting and plasticizing, the obtained molten rubber enters a filtering device for filtering and then is conveyed to a die head, film blowing is carried out in an extrusion mode, film bubbles are formed and blown out from a die opening, and the control mode of the cooling temperature of the extruder, the die head and the air ring in the extrusion process is not repeated here.
After the cooled film bubble is stabilized, the thickness distribution of the whole film bubble is measured by an online thickness gauge in a rotating mode at 360 ℃, information is fed back to an automatic air ring, and the thickness uniformity of the film bubble is improved by the automatic air ring through the adjustment of air temperature; the film bubble is clamped into a flat cylindrical film by the herringbone row and then enters an upper traction rotating device, and the film is flattened and then sequentially enters a guide roller for further cooling; and the cooled film enters a flaw detection device to detect the appearance and crystal points of the film, is cut by an auxiliary traction clamping roller, is separated into single pieces, enters a static electricity removal device, and is finally wound by a winding device to obtain the protective film.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
The self-adhesive polyethylene protective film with high unwinding, no precipitation and high haze prepared by the embodiment has three layers of structures, namely an outer layer, a middle layer and an inner layer, wherein the weight ratio of the three layers of materials is 10:35: 55; the raw materials of each layer are as follows:
outer layer: the polyethylene comprises, by mass, metallocene low-density polyethylene 8112 and POP8380, wherein the mass ratio of the metallocene low-density polyethylene to the POP is 6.5: 13.2;
middle layer: high pressure low density polyethylene HP0722 NN;
inner layer: high haze high pressure low density polyethylene F213-P;
the method is produced in a ten-thousand-level dust-free purification workshop, and the adopted film blowing equipment is provided with a raw material dust removal device, an automatic batching device, an extruder, a filtering device, an automatic air ring online thickness measuring device, an upper traction rotating device, a corona treatment device, an online flaw detection device, a static electricity removal device and a central winding device, wherein the extruder comprises an outer layer extruder, a middle layer extruder and an inner layer extruder, and outlets of the three extruders are connected with a die head; the specific preparation process is as follows:
the outer layer, the middle layer and the inner layer raw materials are dedusted by a dedusting device and then are respectively added into an automatic batching device to be mixed according to a set proportion, the mixture is melted and plasticized into a melt by an extruder, and the melt is filtered by impurities through a filter to reach a die head when being extruded by the extruder; extruding and blowing a film, air-cooling (the air temperature is 20-25 ℃), stabilizing film bubbles by a stabilizing ring, detecting the thickness by an online thickness measuring device, entering an inverted V-shaped plate for bubble formation, entering an upper traction rotating device for flattening the film, cooling by a guide roller, entering a crystal point flaw detector for detecting the appearance and crystal points of the film, cutting edges, entering a front and rear winding device by a lower traction clamping roller, removing static electricity, and then winding in front and rear directions to obtain the self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze.
Wherein the temperature and pressure of the extruder and die are shown in table 1:
TABLE 1 extruder temperature and pressure
Figure BDA0003396877910000081
Example 2
The extrusion mass ratio of the outer layer, the middle layer and the inner layer is changed to 12:48:40, and the mass ratio of the metallocene low-density polyethylene to POP in the outer layer is changed to 7.8: 14.3; the other conditions were the same as in example 1, and the preparation method was the same as in example 1.
Example 3
The extrusion mass ratio of the outer layer, the middle layer and the inner layer is changed to 12:40:48, and the mass ratio of the metallocene low-density polyethylene to POP in the outer layer is changed to 8.5: 12.6; the other conditions were the same as in example 1, and the preparation method was the same as in example 1.
Example 4
The extrusion mass ratio of the outer layer, the middle layer and the inner layer is changed to 13:42:45, and the mass ratio of the metallocene low-density polyethylene to POP in the outer layer is changed to 16.3: 8.8; the other conditions were the same as in example 1, and the preparation method was the same as in example 1.
Example 5
The extrusion mass ratio of the outer layer, the middle layer and the inner layer is changed to 10:30:60, and the mass ratio of the metallocene low-density polyethylene to POP in the outer layer is changed to 14.5: 7.6; the other conditions were the same as in example 1, and the preparation method was the same as in example 1.
Example 6
The extrusion mass ratio of the outer layer, the middle layer and the inner layer is changed to 15:40:45, the mass ratio of the metallocene low-density polyethylene to POP in the outer layer is changed to 12.3:5.6, and the high-haze high-pressure low-density polyethylene in the inner layer is replaced by LB 5000; the other conditions were the same as in example 1, and the preparation method was the same as in example 1.
Comparative example 1
The self-adhesive protection film with the matte surface has a three-layer structure comprising an outer layer, a middle layer and an inner layer, wherein the raw materials adopted by each layer are as follows:
the outer layer is made of JPE POP brand KF370, the melt index is 3.5g/10min, and the density is 0.905g/cm3(ii) a The middle layer, middle layer and inner layer of high pressure low density polyethylene are of the brand 2420H of Maoming petrochemical, the melt index is 2.0g/10min, and the density is 0.924g/cm3(ii) a Linear selecting bat with majen name in middle layerThe melt index of the bimodal linear low-density polyethylene FB2230 is 0.2g/10min, and the density is 0.922g/cm3The inner layer of the mother granules was made of Shanghai bicrystal PEAB-10BMFP with a melt index of 2.5.0g/10min and a density of 1.05g/cm3。
The proportions of the raw materials in each layer and the extrusion proportions of the outer layer, the middle layer and the inner layer are shown in table 2;
TABLE 2 proportions of raw materials in the respective layers and extrusion proportions of outer, middle and inner layers
Figure BDA0003396877910000091
The preparation method comprises the following steps:
the method comprises the following steps of mixing the raw materials of the outer layer, the middle layer and the inner layer in proportion through an automatic batching system, feeding the raw materials into an extruder of the outer layer, the middle layer and the inner layer respectively for fusion and plasticization, feeding the raw materials into a die head for extrusion and film forming through a die orifice, cooling the raw materials through an air ring, feeding the raw materials into an upper traction clamping roller through a stabilizing ring and a herringbone row for clamping and flattening a film bubble, feeding the flattened film into an upper traction roller for traction and rotation, cooling and trimming the film through a guide roller, feeding the flattened film into a lower traction device, and winding the film before and after separation to obtain the fog-surface self-adhesive protective film.
The extruder for each layer was heated in 5 zones and the temperature and pressure measurements for the control extruder and die were as shown in table 3:
TABLE 3 temperature and pressure of extruder and die
Condition 1 region/. degree.C 2 region/. degree.C Zone 3/. degree.C Zone 4/. degree.C Zone 5/. degree.C Pressure (Mpa)
Outer layer 160 165 170 165 160 23
Middle layer 165 172 178 168 165 32
Inner layer 195 202 205 200 200 42
Die head 203 208 213 210
The formulation of comparative example 1 used bimodal linear low density polyethylene FB2230, which has poor bubble stability, difficult control of thickness and more crystalline points during processing due to high processing temperature of the raw material and large temperature difference with other polyethylene materials; and the formula in the comparative example 1 is added with the unwinding master batch, so that the phenomenon of separation of the blocking net is easy to occur.
Comparative example 2
The utility model provides a high temperature resistant autohension protection film, has three layer construction, is skin, middle level and inlayer respectively, and the raw materials that each layer adopted are as follows:
the outer layer is POP of JPE brand KF370, the melt index is 3.5g/10min, and the density is 0.905g/cm3(ii) a The high-pressure low-density polyethylene of the middle layer, the middle layer and the inner layer is a product with a brand name of 2420H of petrochemical, the melt index is 2.0g/10min, and the density is 0.924g/cm3(ii) a The inner layer of the fogging concentrate is W9019 of Foshan Daoxing, the melt index is 8.5.0g/10min, and the density is 1.2g/cm3。
The proportions of the raw materials in each layer and the extrusion proportions of the outer layer, the middle layer and the inner layer are shown in table 4;
TABLE 4 proportions of raw materials in the respective layers and extrusion proportions of outer, middle and inner layers
Figure BDA0003396877910000101
The preparation method comprises the following steps: the method comprises the following steps of mixing the raw materials of the outer layer, the middle layer and the inner layer in proportion through an automatic batching system, feeding the raw materials into an extruder of the outer layer, the middle layer and the inner layer respectively for fusion and plasticization, feeding the raw materials into a die head for extrusion and film forming through a die orifice, cooling the raw materials through an air ring, feeding the raw materials into an upper traction clamping roller through a stabilizing ring and a herringbone row for clamping and flattening a film bubble, feeding the flattened film into an upper traction roller for traction and rotation, cooling and trimming the film through a guide roller, feeding the flattened film into a lower traction device, and winding the film before and after separation to obtain the fog-surface self-adhesive protective film.
The extruder for each layer was heated in 5 zones and the temperature and pressure measurements for the control extruder and die were as shown in table 5:
TABLE 5 temperature and pressure of extruder and die
Figure BDA0003396877910000102
The fogging master batches are added in the comparative example 2, so that the net is easily blocked, the net changing times are increased, and the waste is increased and separated out in the production process.
And (3) testing performance parameters:
fig. 1 is a microscopic view of the polyvinyl alcohol protective film prepared in example 1, and it can be seen from fig. 1 that the surface of the polyvinyl alcohol protective film prepared by the present invention has a regular and dense arrangement of convex-concave points, and this special structure shows that when the film is unwound and peeled, the bonding surface of the adhesive layer and the back layer of the film material will not generate a microscopic vacuum negative pressure, so as to achieve the purpose of easy unwinding and anti-adhesion.
Microscopic observation is carried out on the polyethylene protective films prepared in the embodiments 2-6, and the results show that the surfaces of the polyethylene protective films are all in similar concave-convex point arrangement.
The thickness, mechanical properties, haze, and friction coefficient of the protective films prepared in examples 1 to 6 and comparative examples 1 to 2 were measured, and the presence or absence of precipitates was observed, and the results are shown in table 6:
TABLE 6 results of testing the Performance parameters of the protective films obtained in examples 1 to 6 and comparative examples 1 to 2
Figure BDA0003396877910000111
According to the data in table 6, it can be seen that the polyvinyl alcohol protective film prepared by the invention has good mechanical properties, good unwinding property, high haze and no precipitation, and the inner layer of the protective film in the comparison documents 1-2 has a slightly large friction coefficient, poor unwinding property, small haze and precipitation.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (8)

1. The self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze is characterized by being prepared by co-extruding and blowing films of an outer layer, a middle layer and an inner layer;
the outer layer is prepared from metallocene low-density polyethylene and polyolefin plastomer; the mass ratio of the metallocene low-density polyethylene to the polyolefin plastomer is 6-17: 4-15;
the preparation raw material of the middle layer is first high-pressure low-density polyethylene; the melt index of the first high-pressure low-density polyethylene is 0.5-1.5 g/10 min; the density is 0.920-0.930 g/cm3；
The inner layer is prepared from a second high-pressure low-density polyethylene; the second high pressure low density polyethylene is high haze high pressure low density polyethylene; the melt index of the high-haze high-pressure low-density polyethylene is 1.0-2.0 g/10min, and the density is 0.920-0.930 g/cm3。
2. The self-adhesive polyethylene protective film with high unwinding, no precipitation and high haze according to claim 1, wherein the melt index of the metallocene low-density polyethylene in the raw materials for preparing the outer layer is 0.8-1.5 g/10min, and the density is 0.910-0.915 g/cm3；
In the preparation raw materials of the outer layer, the melt index of the polyolefin plastomer is 2.5-4 g/10min, and the density is 0.870-0.900 g/cm3。
3. The self-adhesive pure polyethylene protective film with high unwinding, no precipitation and high haze as claimed in claim 1, wherein the mass ratio of the outer layer, the middle layer and the inner layer is 10-15: 30-50: 40-70.
4. The self-adhesive pure polyethylene protective film with high unwinding, no precipitation and high haze as claimed in any one of claims 1 to 3, wherein the haze of the protective film is not less than 18%.
5. The preparation method of the self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze according to any one of claims 1 to 4 is characterized by comprising the following steps:
respectively feeding the outer layer preparation raw material, the middle layer preparation raw material and the inner layer preparation raw material into an outer layer extruder, a middle layer extruder and an inner layer extruder for melting and plasticizing, filtering the obtained molten gel, conveying the filtered molten gel to a die head, extruding and blowing a film, forming film bubbles, blowing out the film bubbles from the die head, and cooling the blown film bubbles through an automatic air ring at the die head to obtain the self-adhesive polyethylene protective film with high uncoiling, no precipitation and high haze; the air temperature of the automatic air ring is 20-25 ℃.
6. The preparation method of claim 5, wherein the outer layer extruder, the middle layer extruder and the inner layer extruder are all provided with 6 heating zones, and the heating zones are sequentially marked as a first zone to a sixth zone according to the raw material passing sequence; the die head is provided with 4 heating zones which are sequentially marked as a first zone to a fourth zone according to the passing sequence of the raw materials;
the temperature of the first zone of the outer layer extruder is 170-175 ℃, the temperature of the second zone is 175-180 ℃, the temperature of the third zone is 175-180 ℃, the temperature of the fourth zone is 175-180 ℃, the temperature of the fifth zone is 175-180 ℃, and the temperature of the sixth zone is 175-180 ℃;
the temperature of the first zone of the middle layer extruder is 160-165 ℃, the temperature of the second zone is 165-170 ℃, the temperature of the third zone is 165-170 ℃, the temperature of the fourth zone is 165-170 ℃, the temperature of the fifth zone is 160-165 ℃ and the temperature of the sixth zone is 160-165 ℃;
the temperature of the inner layer extruder in the first area is 155-160 ℃, the temperature of the second area is 160-165 ℃, the temperature of the third area is 160-165 ℃, the temperature of the fourth area is 160-165 ℃, the temperature of the fifth area is 160-165 ℃ and the temperature of the sixth area is 160-165 ℃;
the temperature of the first area of the die head is 170-175 ℃, the temperature of the second area is 175-180 ℃, the temperature of the third area is 175-180 ℃, and the temperature of the fourth area is 175-180 ℃.
7. The production method according to claim 6, wherein the extrusion pressure of the outer layer extruder, the middle layer extruder and the inner layer extruder is independently 15 to 40 MPa.
8. The preparation method of claim 5, wherein after the bubble is cooled, the steps of bubble stabilization, thickness measurement, traction, flaw detection, edge cutting, static electricity removal and winding are sequentially carried out.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012106025A1 (en) * 2011-01-31 2012-08-09 Exxonmobil Chemical Patents Inc. Coextruded films and processes for making such films
CN111806023A (en) * 2020-06-23 2020-10-23 江门市华龙膜材股份有限公司 Polyethylene protective film for photosensitive dry film and preparation method thereof
CN113635636A (en) * 2021-08-13 2021-11-12 茂名联塑建材有限公司 High-performance PE film and preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012106025A1 (en) * 2011-01-31 2012-08-09 Exxonmobil Chemical Patents Inc. Coextruded films and processes for making such films
CN111806023A (en) * 2020-06-23 2020-10-23 江门市华龙膜材股份有限公司 Polyethylene protective film for photosensitive dry film and preparation method thereof
CN113635636A (en) * 2021-08-13 2021-11-12 茂名联塑建材有限公司 High-performance PE film and preparation method and application thereof

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