CN115716930B - Ultraviolet cross-linked POF heat-shrinkable film and preparation method thereof - Google Patents
Ultraviolet cross-linked POF heat-shrinkable film and preparation method thereof Download PDFInfo
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- 229920006257 Heat-shrinkable film Polymers 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003999 initiator Substances 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 11
- 150000003254 radicals Chemical class 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 11
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 11
- 229920005606 polypropylene copolymer Polymers 0.000 claims description 9
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical group C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 8
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 claims description 2
- QKTWWGYCVXCKOJ-UHFFFAOYSA-N 2-methoxy-1-(2-methoxyphenyl)-2-phenylethanone Chemical compound C=1C=CC=CC=1C(OC)C(=O)C1=CC=CC=C1OC QKTWWGYCVXCKOJ-UHFFFAOYSA-N 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 abstract description 13
- 229920000642 polymer Polymers 0.000 abstract description 4
- 230000003993 interaction Effects 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 46
- 238000007605 air drying Methods 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 239000012965 benzophenone Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241000218378 Magnolia Species 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000071 blow moulding Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229920003020 cross-linked polyethylene Polymers 0.000 description 1
- 239000004703 cross-linked polyethylene Substances 0.000 description 1
- CUJPJTIBYGTKKC-UHFFFAOYSA-N cyclohexanol;diphenylmethanone Chemical compound OC1CCCCC1.C=1C=CC=CC=1C(=O)C1=CC=CC=C1 CUJPJTIBYGTKKC-UHFFFAOYSA-N 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012949 free radical photoinitiator Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Abstract
The invention discloses an ultraviolet cross-linked POF heat-shrinkable film and a preparation method thereof, wherein the preparation method comprises the following steps: soaking the washed and dried POF base film and a certain amount of photoinitiator or free radical initiator in a solvent until the solvent is completely absorbed by the POF film, then placing the POF base film under ultraviolet light at a certain ambient temperature for irradiation, washing off the residual initiator on the surface of the film after the irradiation is finished, and drying to obtain the ultraviolet cross-linked POF heat-shrinkable film. The invention selects ultraviolet light with simple equipment and easily controllable energy as a crosslinking driving force, and utilizes the interaction between different photoinitiators and polymers to obviously improve the crosslinking efficiency of the POF heat-shrinkable film under the condition of low initiator addition, so that the traditional POF heat-shrinkable film has higher heat stability and heat shrinkage rate, and the processing and application range of the POF heat-shrinkable film is obviously widened.
Description
Technical Field
The invention relates to the technical field of heat-shrinkable films, in particular to an ultraviolet cross-linked POF heat-shrinkable film and a preparation method thereof.
Background
The polyolefin material is a polymer material with the greatest demand and the greatest application, and one of the applications is to prepare a plastic film for the field of heat shrinkage materials. The most widely used polyolefin films are POF films, the thermal stability and thermal shrinkage properties of which are closely related to the degree of crosslinking thereof.
The traditional POF heat-shrinkable film is generally prepared by taking ternary polymerization polypropylene as an inner layer and an outer layer and linear low-density polyethylene as an intermediate layer through processes such as three-layer coextrusion blow molding, and the like, and the multilayer structure endows the film with the advantages of high transparency, high strength, good toughness and the like, and meanwhile, the film also has the problems of incompatibility among layers, poor heat stability, narrow heat shrinkage window range, improved low-temperature heat-shrinkable performance and the like, and influences the application of the film to a certain extent. The cross-linking modification can improve the defects of the POF heat-shrinkable film, introduce covalent bonds to connect molecular chains between layers, improve compatibility, and improve temperature resistance and low-temperature heat-shrinkable performance. The existing film crosslinking modification method mainly improves the crosslinking density by introducing an initiator to be combined with irradiation. The 201410747785.9 is characterized in that firstly, the photoinitiator is blended with the polyethylene master batch to prepare the master batch, and then the cross-linked polyethylene film is prepared through three-layer coextrusion blow molding, ultraviolet irradiation and other processes, so that the heat shrinkage rate of the film is effectively improved. However, the kind of the initiator has a remarkable influence on the effect of ultraviolet crosslinking, and most of the initiator can cause degradation of the polymer while forming a crosslinked structure, thereby influencing the effect of crosslinking modification. In addition, the introduction of the initiator prior to the extrusion process can cause problems such as the initiator being susceptible to degradation, deactivation, and the like. The initiator can be prevented from being degraded in the processing process by directly adopting low-energy electron irradiation crosslinking, but the process is high in difficulty and high in energy consumption, and is not beneficial to popularization and application.
Disclosure of Invention
In order to solve the problems, the invention provides an ultraviolet cross-linked POF heat-shrinkable film and a preparation method thereof, so as to provide the cross-linked POF heat-shrinkable film with the advantages of higher heat stability and heat shrinkage rate, high production efficiency, low equipment cost and the like.
The specific technical scheme is as follows:
a first aspect of the present invention is to provide a method for producing an ultraviolet crosslinked POF heat shrinkable film, having such a feature that it comprises the steps of: soaking the washed and dried POF base film and a certain amount of photoinitiator or free radical initiator in a solvent until the solvent is completely absorbed by the POF film, then placing the POF base film under ultraviolet light at a certain ambient temperature for irradiation, washing off the residual initiator on the surface of the film after the irradiation is finished, and drying to obtain the ultraviolet cross-linked POF heat-shrinkable film.
The preparation method is characterized in that the part ratio of the POF base film to the photoinitiator is 100: (0.2-1.0).
The preparation method also has the characteristic that the photoinitiator is Benzophenone (BP) 、 One of 2,2' -dimethoxy-2-phenyl acetophenone (Irgacure 651) and hydroxycyclohexane-phenyl ketone (Irgacure 184).
The preparation method is characterized in that the part ratio of the POF base film to the free radical photoinitiator is 100: (2-10).
The above preparation method is also characterized in that the radical initiator is one of dibenzoyl peroxide (BPO), di-t-butyl peroxide (DTBP), azobisisobutyronitrile (AIBN) and Azobisisoheptonitrile (ABVN).
The above preparation method also has such characteristic that the ambient temperature is 50-70 ℃.
The preparation method also has the characteristics that the ultraviolet wavelength is 365nm and the irradiation time is 2-5min.
The above preparation method also has such a feature that the thickness of the POF base film is 0.015 to 0.025mm.
The above preparation method is also characterized in that the intermediate layer of the POF base film is linear low density polyethylene, and the inner and outer layers of the POF base film are copolymer polypropylene.
The second aspect of the present invention is to provide an ultraviolet crosslinked POF heat-shrinkable film produced according to the above production method.
The beneficial effect of above-mentioned scheme is:
1) The invention uses ultraviolet light as driving force to crosslink and modify the existing POF film, has simple equipment and convenient operation, can rapidly obtain ultraviolet crosslinked POF heat-shrinkable films with different thicknesses, has good heat stability and heat-shrinkable performance, and remarkably expands the processing and application range of the existing heat-shrinkable films;
2) The invention utilizes the interaction between different photoinitiation and polymers to obviously improve the crosslinking efficiency of the POF heat-shrinkable film under the condition of low initiator addition
3) The method utilizes the solvent soaking method to effectively introduce the initiator into the POF membrane system, and improves the loading efficiency of the initiator, thereby improving the crosslinking efficiency.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention will be further illustrated, but is not limited, by the following examples.
Example 1
Cutting POF base film (thickness 0.017mm, linear low density polyethylene as middle layer, polypropylene copolymer as inner and outer layers, and large package material Co., ltd.) to about 15cm×15cm, washing with distilled water and acetone, air drying, and weighing; immersing the treated POF base film and BP (sigma Aldrich trade Co., ltd.) accounting for 0.4% of the film mass in acetone until the solvent is completely absorbed by the POF film; and then the film is irradiated for 2min under the irradiation of ultraviolet light with the wavelength of 365nm at the temperature of 60 ℃, and after the irradiation is finished, the residual initiator on the surface of the film is washed off by acetone, and the film is dried to obtain the ultraviolet cross-linked POF heat-shrinkable film.
Example 2
Cutting POF base film (thickness 0.017mm, linear low density polyethylene as middle layer, polypropylene copolymer as inner and outer layers, and large package material Co., ltd.) to about 15cm×15cm, washing with distilled water and acetone, air drying, and weighing; immersing the treated POF base film and BP (sigma Aldrich trade Co., ltd.) accounting for 0.5% of the film mass in acetone until the solvent is completely absorbed by the POF film; and then the film is irradiated for 2min under the irradiation of ultraviolet light with the wavelength of 365nm at the temperature of 60 ℃, and after the irradiation is finished, the residual initiator on the surface of the film is washed off by acetone, and the film is dried to obtain the ultraviolet cross-linked POF heat-shrinkable film.
Example 3
Cutting POF base film (thickness 0.017mm, linear low density polyethylene as middle layer, polypropylene copolymer as inner and outer layers, and large package material Co., ltd.) to about 15cm×15cm, washing with distilled water and acetone, air drying, and weighing; immersing the treated POF base film and BP (sigma Aldrich trade Co., ltd.) accounting for 0.6% of the film mass in acetone until the solvent is completely absorbed by the POF film; and then the film is irradiated for 2min under the irradiation of ultraviolet light with the wavelength of 365nm at the temperature of 60 ℃, and after the irradiation is finished, the residual initiator on the surface of the film is washed off by acetone, and the film is dried to obtain the ultraviolet cross-linked POF heat-shrinkable film.
Example 4
Cutting POF base film (thickness 0.017mm, linear low density polyethylene as middle layer, polypropylene copolymer as inner and outer layers, and large package material Co., ltd.) to about 15cm×15cm, washing with distilled water and acetone, air drying, and weighing; immersing the treated POF base film and BP (sigma Aldrich trade Co., ltd.) accounting for 0.7% of the film mass in acetone until the solvent is completely absorbed by the POF film; and then the film is irradiated for 2min under the irradiation of ultraviolet light with the wavelength of 365nm at the temperature of 60 ℃, and after the irradiation is finished, the residual initiator on the surface of the film is washed off by acetone, and the film is dried to obtain the ultraviolet cross-linked POF heat-shrinkable film.
Example 5
Cutting POF base film (thickness 0.017mm, linear low density polyethylene as middle layer, polypropylene copolymer as inner and outer layers, and large package material Co., ltd.) to about 15cm×15cm, washing with distilled water and acetone, air drying, and weighing; soaking the treated POF base film and BP accounting for 0.4% of the film mass in ethanol until the solvent is completely absorbed by the POF film; and then the film is irradiated for 2min under the irradiation of ultraviolet light with the wavelength of 365nm at the temperature of 60 ℃, and after the irradiation is finished, the residual initiator on the surface of the film is washed off by acetone, and the film is dried to obtain the ultraviolet cross-linked POF heat-shrinkable film.
Example 6
Cutting POF base film (thickness 0.017mm, linear low density polyethylene as middle layer, polypropylene copolymer as inner and outer layers, and large package material Co., ltd.) to about 15cm×15cm, washing with distilled water and acetone, air drying, and weighing; soaking the treated POF base film and BPO (Shanghai Michelia Biochemical technology Co., ltd.) accounting for 4% of the film mass in acetone until the solvent is completely absorbed by the POF film; and then the film is irradiated for 2min under the irradiation of ultraviolet light with the wavelength of 365nm at the temperature of 60 ℃, and after the irradiation is finished, the residual initiator on the surface of the film is washed off by acetone, and the film is dried to obtain the ultraviolet cross-linked POF heat-shrinkable film.
Example 7
Cutting POF base film (thickness 0.017mm, linear low density polyethylene as middle layer, polypropylene copolymer as inner and outer layers, and large package material Co., ltd.) to about 15cm×15cm, washing with distilled water and acetone, air drying, and weighing; soaking the treated POF base film and BPO (Shanghai Michelia Biochemical technology Co., ltd.) accounting for 7% of the film mass in acetone until the solvent is completely absorbed by the POF film; then the film is irradiated for 2min under the ultraviolet radiation with the wavelength of 365nm at the temperature of 60 ℃, after the irradiation is finished, the residual initiator on the surface of the film is washed off by acetone, and the film is dried to obtain the ultraviolet cross-linked POF heat-shrinkable film
Comparative example 1
Cutting POF base film (thickness 0.017mm, linear low density polyethylene as middle layer, polypropylene copolymer as inner and outer layers, and large package material Co., ltd.) to about 15cm×15cm, washing with distilled water and acetone, air drying, and weighing; soaking the treated POF base film in acetone until the solvent is completely absorbed by the POF film; and then the film is irradiated for 2min under the irradiation of ultraviolet light with the wavelength of 365nm at the temperature of 60 ℃, and is washed clean by acetone after the irradiation is finished, and is dried to obtain the ultraviolet cross-linked POF heat-shrinkable film.
The heat-shrinkable films provided in examples 1 to 7 and comparative examples were tested according to the methods related to ISO10147 and GB/T10003-2008 in the present invention, and the tests are shown in the following table:
as shown in the table above, when no photoinitiator or free radical initiator is added, the base film is basically not crosslinked, the thermal shrinkage rate of the POF thermal shrinkage film is low, the crosslinking degree of the POF thermal shrinkage film is obviously increased after the photoinitiator or free radical initiator is added and is irradiated under ultraviolet light, the thermal stability and the thermal shrinkage rate are obviously improved, and the processing and application range of the traditional POF thermal shrinkage film are obviously expanded.
Compared with the initiator directly introduced into the three-layer co-extrusion engineering, the invention avoids the degradation and inactivation of the initiator in the processing process and improves the initiator efficiency.
According to the invention, the conventional POF base film is directly subjected to crosslinking modification, and the POF heat-shrinkable films with different thicknesses can be obtained by selecting the base films with different thicknesses, so that the influence of the introduction of an initiator on the flowability of a polymer and further on an extrusion process is avoided.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, and it will be appreciated by those skilled in the art that equivalent substitutions and obvious variations may be made using the teachings of the present invention, which are intended to be included within the scope of the invention.
Claims (6)
1. The preparation method of the ultraviolet cross-linked POF heat-shrinkable film is characterized by comprising the following steps: soaking the washed and dried POF base film and a certain amount of photoinitiator or free radical initiator in a solvent until the solvent is completely absorbed by the POF film, then placing the POF base film under ultraviolet light at a certain ambient temperature for irradiation, washing off the residual initiator on the surface of the film after the irradiation is finished, and drying to obtain the ultraviolet cross-linked POF heat-shrinkable film;
wherein, the part ratio of the POF base film to the photoinitiator is 100: (0.2-1.0);
the photoinitiator is diphenyl ketone 、 One of 2,2' -dimethoxy-2-phenyl acetophenone and hydroxycyclohexane-yl phenyl ketone; the part ratio of the POF base film to the free radical initiator is 100: (2-10), wherein the free radical initiator is one of dibenzoyl peroxide, di-tert-butyl peroxide, azobisisobutyronitrile and azobisisoheptonitrile.
2. The method of claim 1, wherein the ambient temperature is 50-70 ℃.
3. The method according to claim 1, wherein the ultraviolet light has a wavelength of 365nm and the irradiation time is 2 to 5 minutes.
4. A method according to any one of claims 1 to 3, wherein the POF base film thickness is 0.015 to 0.025mm.
5. The method according to claim 4, wherein the intermediate layer of the POF base film is linear low density polyethylene, and the inner and outer layers of the POF base film are polypropylene copolymers.
6. An ultraviolet crosslinked POF heat-shrinkable film, characterized by being produced according to the production method of any one of claims 1 to 5.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006175799A (en) * | 2004-12-24 | 2006-07-06 | Asahi Kasei Chemicals Corp | Thermal shrinkable film |
| CN104385734A (en) * | 2014-12-09 | 2015-03-04 | 黑龙江省润特科技有限公司 | Ultraviolet crosslinked polyethylene heat shrinkage package film and preparation method thereof |
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| AU2019346436A1 (en) * | 2018-09-25 | 2021-03-18 | Evoqua Water Technologies Llc | Ion exchange membrane through UV initiated polymerization |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006175799A (en) * | 2004-12-24 | 2006-07-06 | Asahi Kasei Chemicals Corp | Thermal shrinkable film |
| CN104385734A (en) * | 2014-12-09 | 2015-03-04 | 黑龙江省润特科技有限公司 | Ultraviolet crosslinked polyethylene heat shrinkage package film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 紫外光辐照交联对超高相对分子质量聚乙烯纤维结构和性能的影响;陈自力等;高分子材料科学与工程;第17卷(第03期);62-65、70 * |
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