CN116080114B - Preparation method of biaxially oriented PDCPD film - Google Patents
Preparation method of biaxially oriented PDCPD film Download PDFInfo
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- 229920001153 Polydicyclopentadiene Polymers 0.000 title claims abstract description 111
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000011347 resin Substances 0.000 claims abstract description 38
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 238000001125 extrusion Methods 0.000 claims abstract description 36
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 238000005096 rolling process Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 11
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- 238000010438 heat treatment Methods 0.000 claims description 9
- 229940014569 pentam Drugs 0.000 claims description 5
- YBVNFKZSMZGRAD-UHFFFAOYSA-N pentamidine isethionate Chemical compound OCCS(O)(=O)=O.OCCS(O)(=O)=O.C1=CC(C(=N)N)=CC=C1OCCCCCOC1=CC=C(C(N)=N)C=C1 YBVNFKZSMZGRAD-UHFFFAOYSA-N 0.000 claims description 5
- 229920000636 poly(norbornene) polymer Polymers 0.000 claims description 4
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- 239000011810 insulating material Substances 0.000 abstract description 3
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- 239000010408 film Substances 0.000 description 69
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- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a preparation method of a biaxially oriented PDCPD film, which is characterized by comprising the following steps: after being dried, PDCPD resin is added into a single screw extruder for melt extrusion, wherein the screw diameter of the single screw extruder is 30mm, and the length-diameter ratio of the screw is not higher than 35:1, the extrusion temperature is 230-260 ℃; the extruded melt is longitudinally pressed twice to form a unidirectional sheet; then the unidirectional sheet enters a transverse pulling box to be transversely pulled twice; and cooling and rolling the biaxially oriented film obtained after transverse drawing to obtain the biaxially oriented PDCPD film. The biaxially oriented PDCPD film prepared by the invention has the characteristics of low density, high mechanical strength, uniform thickness, low dielectric constant, low dielectric loss and the like, and can be widely applied to the fields of insulating materials, solar cell back plates, plastic suction boxes, electronic consumption packaging materials, rigid copper-clad plates, hard or grooved plates and the like.
Description
Technical Field
The invention belongs to the preparation of films, and relates to a preparation method of a biaxially oriented PDCPD film. The biaxially oriented PDCPD film prepared by the invention can be widely applied to the fields of insulating materials, solar cell back plates, plastic suction boxes, electronic consumption packaging materials, rigid copper-clad plates, hard or grooved plates and the like.
Background
PDCPD (short for polydicyclopentadiene) is a polymer with a three-dimensional network structure formed by a reaction injection molding process of dicyclopentadiene. PDCPD has the advantages of low density, good dimensional stability, acid and alkali resistance, high rigidity, good creep resistance and good electrical insulation property, and is applied to surfboards, automobile bumpers, sleigh vehicles, water pipes, helmets and the like. Because PDCPD is a polyolefin material with low dielectric constant and dielectric loss, it has been applied to 5G radomes.
With the growing demand for high strength boards and structures, there is a wide market for higher strength materials in sports equipment and automotive parts. The PDCPD is used as a high-strength polyolefin material, the strength is far higher than that of the traditional polypropylene (PP for short) and polyethylene (PE for short) materials, even higher than that of poly-1-methyl-4-pentene, and the temperature resistance is better. CN112961279a discloses a method for preparing a copolymer of polydicyclopentadiene and polydicyclopentadiene, which makes the copolymer have higher strength and wider application range. The preparation of self-skinning polydicyclopentadiene foam [ J ] by chemical foaming method is disclosed in document (Chen Guowei, he Yuxin, li Xuyang, liu Qiuju, zhang Yuqing) in the scientific and engineering of high molecular materials, 2015, 31 (05): 149-153), which is characterized by low foam density, good mechanical strength and thermal stability.
PDCPD is formed by reaction injection molding at present due to the characteristic of semi-thermosetting materials, but a screw extrusion mode is not reported for forming a plate or a sheet. Meanwhile, the mode of preparing the film by biaxially stretching the formed sheet is not reported.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a biaxially oriented PDCPD film. Aiming at the defects that the existing PDCPD preparation can only be subjected to reaction injection molding, film preparation is not realized and the like, the PDCPD is extruded to form a uniform sheet by adopting a special screw design, and then the sheet is subjected to secondary longitudinal compression and secondary transverse drawing to prepare the biaxially oriented PDCPD film with uniform thickness. Therefore, the preparation method of the biaxially oriented PDCPD film has the advantages of continuous production, high mechanical strength, difficult tearing, good creep resistance, small dielectric constant and dielectric loss and the like.
The invention comprises the following steps: a preparation method of a biaxially oriented PDCPD film is characterized by comprising the following steps:
a. and (3) drying: adding the (pure) PDCPD resin into a vacuum drying tank, heating and drying to obtain dried PDCPD resin;
b. melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is not higher than (or equal to or not higher than) 35:1, the extrusion temperature is 230-260 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure (roller) is 140-200 ℃, the pressure is 0.3-0.6 MPa, the temperature of the second longitudinal pressure (roller) is 180-230 ℃, the pressure is 0.7-1.2 MPa, and the longitudinal stretching multiple is 1.3-1.9;
d. And (3) transverse pulling twice: the cooled unidirectional sheet (directly) enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 170-180 ℃, the first transverse drawing multiple is 1.2-1.4 times, the temperature of the second transverse drawing is 200-210 ℃, and the second transverse drawing multiple is 1.05-1.25 times;
e. Post-treatment: and cooling the biaxially oriented film, measuring the thickness, and then rolling to obtain the biaxially oriented PDCPD film.
In the content of the invention: the drying temperature of the heating and drying in the step a is preferably 80 ℃ and the drying time is 4 hours.
In the content of the invention: the PDCPD resin in the step a can be one or more than two of PARMAX-VARIM (Parmex), pentam 1400 (Japanese rayleigh), metton TM (U.S. Metton) and Telene TM (U.S. CYMETECH LLC).
In the content of the invention: in the step e, the speed of the winding is preferably 5-20 m/min, and the thickness of the prepared biaxially oriented PDCPD film is preferably 0.02-0.045 mm.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
(1) The method adopts a secondary longitudinal pressure mode to melt the PDCPD resin to form a unidirectional stretching sheet, and then transversely stretches the unidirectional sheet to form an isotropic bidirectional stretching film through secondary transverse stretching, so that the prepared bidirectional stretching PDCPD film has the advantages of being good in performance, low in density, high in tensile strength, uniform in thickness, good in toughness, good in corrosion resistance and the like, and can be used as a surface modification layer of a part of high-strength structural members;
(2) According to the method, the PDCPD with semi-thermosetting property is subjected to hot pressing treatment, the PDCPD melt is converted into the sheet through the first longitudinal pressing, the longitudinal stretching of the PDCPD is realized through the second longitudinal pressing, the thickness of the sheet is more uniform, and meanwhile, the molecular chains are longitudinally arranged, so that the longitudinal ductility is improved;
(3) In the method, the PDCDP unidirectional sheets are sequentially and transversely stretched in a secondary transverse stretching mode, and as the transverse molecular chains in the unidirectional sheets are not obviously oriented, the first transverse stretching multiple is relatively high, and the second transverse stretching multiple is smaller on the basis of one transverse stretching, mainly the molecular chains are fixed, so that the molecular chains are more uniformly arranged;
(4) The method realizes the thin-film production of PDCPD, has simple preparation process and strong equipment operability, can realize continuous production, and is beneficial to large-scale industrial production;
(5) The biaxially oriented PDCPD film obtained by the method has low dielectric constant and dielectric loss, has good insulating property, can be used as a rigid copper-clad plate material, and can be used as a rigid plate thinning material;
(6) The method of the invention opens up a new forming process of the PDCPD material, so that the application field of PDCPD is greatly developed, and PDCPD can be used as a high-performance film or sheet for application exploration;
(7) The preparation process is simple, the working procedure is simple and easy to operate, and the prepared biaxially oriented PDCPD film has the characteristics of low density, high mechanical strength, uniform thickness, low dielectric constant, low dielectric loss and the like, can be widely applied to the fields of insulating materials, solar cell back plates, plastic suction boxes, electronic consumption packaging materials, rigid copper-clad plates, hard or grooved plates and the like, and has strong practicability.
Drawings
FIG. 1 is a flow chart of the production process of the present invention and embodiments;
FIG. 2 is a diagram showing a process for preparing a biaxially oriented PDCPD film according to the embodiment of the present invention;
FIG. 3 is a schematic view of the die head of FIG. 2;
fig. 4 is a schematic view of the track structure of the drop box of fig. 2.
Detailed Description
The following examples are intended to further illustrate the present invention but are not to be construed as limiting its scope, as many insubstantial modifications and adaptations of the invention that are within the scope of the invention as described above would be within the skill of the art.
Example 1:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. And (3) drying: adding (pure) PDCPD resin (Telene TM) into a vacuum drying tank, and drying at 80 ℃ for 4 hours to obtain dried PDCPD resin;
b. melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 28:1, the extrusion temperature is 260 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure is 190 ℃, the pressure is 0.56MPa, the temperature of the second longitudinal pressure is 230 ℃, the pressure is 1.15MPa, and the longitudinal stretching multiple is 1.6;
d. And (3) transverse pulling twice: the cooled unidirectional sheet enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 172 ℃, the first transverse drawing multiple is 1.32 times, the temperature of the second transverse drawing is 200 ℃, and the second transverse drawing multiple is 1.12 times;
e. Post-treatment: and cooling the biaxially oriented film, and winding after measuring the thickness, wherein the winding speed is 18m/min, so that the biaxially oriented PDCPD film is prepared, and the thickness of the prepared biaxially oriented PDCPD film is 0.02mm.
Example 2:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. and (3) drying: adding pure PDCPD resin (Pentam, 1400) into a vacuum drying tank, and drying at 80 ℃ for 4 hours to obtain dried PDCPD resin;
b. melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 25:1, the extrusion temperature is 240 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure is 200 ℃, the pressure is 0.5MPa, the temperature of the second longitudinal pressure is 190 ℃, the pressure is 0.94MPa, and the longitudinal stretching multiple is 1.4;
d. and (3) transverse pulling twice: the cooled unidirectional sheet enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 180 ℃, the first transverse drawing multiple is 1.25 times, the temperature of the second transverse drawing is 205 ℃, and the second transverse drawing multiple is 1.2 times;
e. post-treatment: and cooling the biaxially oriented film, and winding after measuring the thickness, wherein the winding speed is 8m/min, so that the biaxially oriented PDCPD film is prepared, and the thickness of the prepared biaxially oriented PDCPD film is 0.04mm.
Example 3:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. and (3) drying: adding PDCPD resin (Pentam, 1400 and Metton TM in a mixing ratio of 1:1) into a vacuum drying tank, and drying at 80 ℃ for 4 hours to obtain dried PDCPD resin;
b. melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 28:1, the extrusion temperature is 230 ℃;
c. twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure is 140 ℃, the pressure is 0.6MPa, the temperature of the second longitudinal pressure is 180 ℃, the pressure is 1.2MPa, and the longitudinal stretching multiple is 1.3;
d. and (3) transverse pulling twice: the cooled unidirectional sheet enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 170 ℃, the first transverse drawing multiple is 1.4 times, the temperature of the second transverse drawing is 210 ℃, and the second transverse drawing multiple is 1.05 times;
e. Post-treatment: and cooling the biaxially oriented film, and winding after measuring the thickness, wherein the winding speed is 5m/min, so that the biaxially oriented PDCPD film is prepared, and the thickness of the prepared biaxially oriented PDCPD film is 0.045mm.
Example 4:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. And (3) drying: adding pure PDCPD resin (PARMAX-VARIM) into a vacuum drying tank, and drying at 80 ℃ for 4 hours to obtain dried PDCPD resin;
b. melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 28:1, the extrusion temperature is 260 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure is 180 ℃, the pressure is 0.3MPa, the temperature of the second longitudinal pressure is 220 ℃, the pressure is 0.7MPa, and the longitudinal stretching multiple is 1.7;
d. And (3) transverse pulling twice: the cooled unidirectional sheet enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 180 ℃, the first transverse drawing multiple is 1.3 times, the temperature of the second transverse drawing is 205 ℃, and the second transverse drawing multiple is 1.1 times;
e. Post-treatment: and cooling the biaxially oriented film, and winding after measuring the thickness, wherein the winding speed is 14m/min, so that the biaxially oriented PDCPD film is prepared, and the thickness of the prepared biaxially oriented PDCPD film is 0.025mm.
The performance index of the PDCPD films prepared in examples 1 to 4 is shown in Table 1 below.
Table 1: PDCPD film Performance index Table prepared in examples 1 to 4:
as can be seen from the data shown in Table 1, the biaxially oriented PDCPD film provided by the invention has the characteristics of mass production, high mechanical strength, low density, good toughness, low dielectric constant and dielectric loss and the like. Meanwhile, the combination of the secondary longitudinal pressure and the secondary transverse pulling mode can enable the semi-thermosetting material PDCPD to realize film forming processing, and expand the application field of the PDCPD material.
Example 5:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. And (3) drying: adding the (pure) PDCPD resin into a vacuum drying tank, heating and drying to obtain dried PDCPD resin, wherein the drying temperature is 80 ℃ and the drying time is 4 hours;
b. Melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 35:1, the extrusion temperature is 260 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure (roller) is 200 ℃, the pressure is 0.6MPa, the temperature of the second longitudinal pressure (roller) is 230 ℃, the pressure is 1.2MPa, and the longitudinal stretching multiple is 1.9;
d. And (3) transverse pulling twice: the cooled unidirectional sheet (directly) enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 180 ℃, the first transverse drawing multiple is 1.4 times, the temperature of the second transverse drawing is 210 ℃, and the second transverse drawing multiple is 1.25 times;
e. Post-treatment: and cooling the biaxially oriented film, measuring the thickness, and then rolling to obtain the biaxially oriented PDCPD film, wherein the thickness of the biaxially oriented PDCPD film is 0.045mm.
Example 6:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. And (3) drying: adding the (pure) PDCPD resin into a vacuum drying tank, heating and drying to obtain dried PDCPD resin, wherein the drying temperature is 80 ℃ and the drying time is 4 hours;
b. melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 25:1, the extrusion temperature is 230 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure (roller) is 140 ℃, the pressure is 0.3MPa, the temperature of the second longitudinal pressure (roller) is 180 ℃, the pressure is 0.7MPa, and the longitudinal stretching multiple is 1.3;
d. And (3) transverse pulling twice: the cooled unidirectional sheet (directly) enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 170 ℃, the first transverse drawing multiple is 1.2 times, the temperature of the second transverse drawing is 200 ℃, and the second transverse drawing multiple is 1.05 times;
e. Post-treatment: and cooling the biaxially oriented film, measuring the thickness, and then rolling to obtain the biaxially oriented PDCPD film, wherein the thickness of the biaxially oriented PDCPD film is preferably 0.02mm.
Example 7:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. And (3) drying: adding the (pure) PDCPD resin into a vacuum drying tank, heating and drying to obtain dried PDCPD resin, wherein the drying temperature is 80 ℃ and the drying time is 4 hours;
b. Melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 30:1, the extrusion temperature is 245 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure (roller) is 170 ℃, the pressure is 0.45MPa, the temperature of the second longitudinal pressure (roller) is 205 ℃, the pressure is 0.95MPa, and the longitudinal stretching multiple is 1.6;
d. And (3) transverse pulling twice: the cooled unidirectional sheet (directly) enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 175 ℃, the first transverse drawing multiple is 1.3 times, the temperature of the second transverse drawing is 205 ℃, and the second transverse drawing multiple is 1.15 times;
e. Post-treatment: and cooling the biaxially oriented film, measuring the thickness, and then rolling to obtain the biaxially oriented PDCPD film, wherein the thickness of the biaxially oriented PDCPD film is preferably 0.032mm.
Example 8:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. And (3) drying: adding the (pure) PDCPD resin into a vacuum drying tank, heating and drying to obtain dried PDCPD resin, wherein the drying temperature is 80 ℃ and the drying time is 4 hours;
b. melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 27:1, the extrusion temperature is 238 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure (roller) is 155 ℃, the pressure is 0.4MPa, the temperature of the second longitudinal pressure (roller) is 195 ℃, the pressure is 0.8MPa, and the longitudinal stretching multiple is 1.4;
d. And (3) transverse pulling twice: the cooled unidirectional sheet (directly) enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 172 ℃, the first transverse drawing multiple is 1.25 times, the temperature of the second transverse drawing is 203 ℃, and the second transverse drawing multiple is 1.1 times;
e. post-treatment: and cooling the biaxially oriented film, measuring the thickness, and then rolling to obtain the biaxially oriented PDCPD film, wherein the thickness of the biaxially oriented PDCPD film is preferably 0.028mm.
Example 9:
the preparation method of the biaxially oriented PDCPD film comprises the following steps:
a. And (3) drying: adding the (pure) PDCPD resin into a vacuum drying tank, heating and drying to obtain dried PDCPD resin, wherein the drying temperature is 80 ℃ and the drying time is 4 hours;
b. Melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is 32:1, the extrusion temperature is 252 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure (roller) is 185 ℃, the pressure is 0.5MPa, the temperature of the second longitudinal pressure (roller) is 220 ℃, the pressure is 1.1MPa, and the longitudinal stretching multiple is 1.8;
d. And (3) transverse pulling twice: the cooled unidirectional sheet (directly) enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 178 ℃, the first transverse drawing multiple is 1.35 times, the temperature of the second transverse drawing is 208 ℃, and the second transverse drawing multiple is 1.22 times;
e. Post-treatment: and cooling the biaxially oriented film, measuring the thickness, and then rolling to obtain the biaxially oriented PDCPD film, wherein the thickness of the biaxially oriented PDCPD film is preferably 0.04mm.
In examples 5-9 above: the PDCPD resin in the step a is one or more than two of PARMAX-VARIM (Parmex), pentam 1400 (Japanese rayleigh), metton TM (U.S. Metton) and Telene TM (U.S. CYMETECH LLC).
In examples 5-9 above: and e, the speed of the winding in the step can be any speed of 5-20 m/min.
In the above embodiment: the process parameters (temperature, time, pressure, vehicle speed, etc.) and the amount of each component in each step are in the range, and any point is applicable.
The technical contents of the invention and the technical contents not specifically described in the above embodiments are the same as the prior art, and the raw materials are all commercial products.
The present invention is not limited to the above-described embodiments, and the present invention can be implemented with the above-described advantageous effects.
Claims (4)
1. A preparation method of a biaxially oriented PDCPD film is characterized by comprising the following steps:
a. And (3) drying: adding the PDCPD resin into a vacuum drying tank, heating and drying to obtain dried PDCPD resin;
b. Melt extrusion: adding the dried PDCPD resin into a single-screw extruder for melt extrusion to obtain an extruded melt, wherein the screw diameter of the single-screw extruder is 30mm, and the length-diameter ratio of the screw is not higher than 35:1, the extrusion temperature is 230-260 ℃;
c. Twice longitudinal pressure: forming a unidirectional sheet from the extruded melt through two longitudinal pressures, and cooling to obtain a cooled unidirectional sheet, wherein the temperature of the first longitudinal pressure is 140-200 ℃, the pressure is 0.3-0.6 MPa, the temperature of the second longitudinal pressure is 180-230 ℃, the pressure is 0.7-1.2 MPa, and the longitudinal stretching multiple is 1.3-1.9;
d. And (3) transverse pulling twice: the cooled unidirectional sheet enters a transverse drawing box and is subjected to transverse drawing twice to obtain a biaxially oriented film, wherein the temperature of the first transverse drawing is 170-180 ℃, the first transverse drawing multiple is 1.2-1.4 times, the temperature of the second transverse drawing is 200-210 ℃, and the second transverse drawing multiple is 1.05-1.25 times;
e. Post-treatment: and cooling the biaxially oriented film, measuring the thickness, and then rolling to obtain the biaxially oriented PDCPD film.
2. The method for preparing the biaxially oriented PDCPD film according to claim 1, which is characterized in that: the drying temperature of the heating and drying in the step a is 80 ℃ and the drying time is 4 hours.
3. The method for preparing the biaxially oriented PDCPD film according to claim 1 or 2, which is characterized in that: the PDCPD resin in the step a is one or a mixture of more than two of PARMAX-VARIM, pentam 1400, metton TM and Telene TM.
4. The method for preparing the biaxially oriented PDCPD film according to claim 1 or 2, which is characterized in that: and e, the speed of the winding is 5-20 m/min, and the thickness of the prepared biaxially oriented PDCPD film is 0.02-0.045 mm.
Priority Applications (1)
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CN101564653A (en) * | 2009-06-05 | 2009-10-28 | 李鑫 | Method for preparing polyolefin micro-porous membrane |
CN105358307A (en) * | 2013-07-01 | 2016-02-24 | 日本瑞翁株式会社 | Method for producing stretched film |
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