CN116023695A - Release film and preparation method thereof - Google Patents
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- CN116023695A CN116023695A CN202310049814.3A CN202310049814A CN116023695A CN 116023695 A CN116023695 A CN 116023695A CN 202310049814 A CN202310049814 A CN 202310049814A CN 116023695 A CN116023695 A CN 116023695A
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- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 238000001125 extrusion Methods 0.000 claims abstract description 14
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 229920001707 polybutylene terephthalate Polymers 0.000 claims abstract description 13
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000000155 melt Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 238000009998 heat setting Methods 0.000 claims abstract description 5
- 239000000314 lubricant Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000005096 rolling process Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 16
- 239000000178 monomer Substances 0.000 claims description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 9
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- FDKXTQMXEQVLRF-ZHACJKMWSA-N (E)-dacarbazine Chemical compound CN(C)\N=N\c1[nH]cnc1C(N)=O FDKXTQMXEQVLRF-ZHACJKMWSA-N 0.000 claims description 6
- 238000007792 addition Methods 0.000 claims description 6
- SMNDYUVBFMFKNZ-UHFFFAOYSA-N 2-furoic acid Chemical compound OC(=O)C1=CC=CO1 SMNDYUVBFMFKNZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000012044 organic layer Substances 0.000 claims description 4
- 230000004224 protection Effects 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 239000004611 light stabiliser Substances 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- TXQVDVNAKHFQPP-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(CO)(CO)CO TXQVDVNAKHFQPP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 2
- 229940124543 ultraviolet light absorber Drugs 0.000 claims 3
- 239000003957 anion exchange resin Substances 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 229920000139 polyethylene terephthalate Polymers 0.000 abstract description 58
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 206010051246 Photodermatosis Diseases 0.000 abstract description 4
- 230000003373 anti-fouling effect Effects 0.000 abstract description 4
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- 230000008845 photoaging Effects 0.000 abstract description 4
- 230000002045 lasting effect Effects 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 2
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- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
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- 150000002500 ions Chemical class 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical group C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
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- 230000003068 static effect Effects 0.000 description 2
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- BDNKZNFMNDZQMI-UHFFFAOYSA-N 1,3-diisopropylcarbodiimide Chemical compound CC(C)N=C=NC(C)C BDNKZNFMNDZQMI-UHFFFAOYSA-N 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
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- 125000003158 alcohol group Chemical group 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 238000007112 amidation reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
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- 230000002950 deficient Effects 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a release film and a preparation method thereof, which belong to the technical field of release films and comprise a PET (polyethylene terephthalate) substrate, wherein an organosilicon release agent is coated on one side of the PET substrate, and the PET substrate comprises the following raw materials: modified PET resin, polybutylene terephthalate, ultraviolet absorber and lubricant; weighing the raw materials in the PET substrate according to a proportion, fully and uniformly mixing, heating and drying, adding into a melt extrusion device for extrusion, stretching, heat setting, cooling and rolling to obtain the PET substrate, and coating an organosilicon release agent on one side of the PET substrate to obtain the release film. The PET substrate adopted by the invention has good toughness and photo-aging resistance after modification, and has lasting antistatic performance and antibacterial property, in addition, the PET substrate can also generate synergistic promotion effect with an organosilicon release agent, and the amphiphobic performance, the antifouling capability and the chemical corrosion resistance of the release agent are improved.
Description
Technical Field
The invention belongs to the technical field of release films, and particularly relates to a release film and a preparation method thereof.
Background
In general, a release film is used as an adhesive surface protective film for an adhesive, a pressure-sensitive adhesive, drops, or the like, or as a carrier sheet for forming a resin sheet, specifically, as a ceramic sheet, an electrode sheet, or the like. Recently, with the diversification of the uses and varieties of optical products, the production yield has been increased, and the like, and the adhesives, binders, and the like have tended to change from a liquid state to a sheet state for the purpose of improving productivity, and the like. Such sheet-like release films temporarily protect the tacky adhesive surface of the adhesive product, for example, prior to use of the label, to become contaminated with dust, debris, moisture and other contaminants. Typically, the release film is separated from the adhesive surface prior to use of the adhesive product. Thus, a coating layer is formed on the release film so as to impart adhesion to the product while imparting peelability to the surface of the product.
In the prior art, because the organosilicon release agent has low cost and wide application range, PET (polyester film) is mostly adopted as a base material, and the surface of the base material is coated with the organosilicon release agent to form a release film. Such a release film coated with silicon has a problem that the surface of the film is easily charged when rubbed because the surface has a very high inherent resistance. At this time, foreign matter such as dust adheres to the film surface due to static electricity, and an electric shock occurs, which causes defective products. In order to improve such a defect caused by static electricity, a silicon release film is required to have antistatic properties.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a release film and a preparation method thereof.
The PET substrate adopted by the release film disclosed by the invention has good toughness and photo-aging resistance after being modified, has lasting antistatic performance and antibacterial property, and can be used for generating a synergistic promotion effect with an organosilicon release agent to improve the amphiphobic performance, the antifouling capability and the chemical corrosion resistance of the release agent, so that the obtained release film has extremely high application value.
The aim of the invention can be achieved by the following technical scheme:
a release film comprises a PET substrate, wherein one side of the PET substrate is coated with an organosilicon release agent.
Further, the organosilicon release agent is a Dow Corning organosilicon release agent, specifically, a Sly-off SL9106 release agent, a Sly-off SL7558 release agent and a Sly-off SL7920 release agent.
Further, the PET substrate comprises the following raw materials in parts by weight: 50-60 parts of modified PET resin, 20-30 parts of polybutylene terephthalate, 0.8-1 part of ultraviolet absorber and 3-4 parts of lubricant;
the mechanical property of the polybutylene terephthalate (PBT) is superior to that of PET, and the polybutylene terephthalate (PBT) has good toughness and good compatibility with PET, so that the toughness of a PET substrate can be remarkably improved by blending the polybutylene terephthalate (PBT) and the PET;
weighing the raw materials according to a proportion, fully and uniformly mixing, heating and drying, adding into a melt extrusion device for extrusion, and obtaining the PET substrate through stretching, heat setting, cooling and rolling.
Further, the ultraviolet absorber is one or more of ultraviolet absorber UV-P, ultraviolet absorber UVP-327 or light stabilizer 744; the introduction of the ultraviolet absorber can improve the ultraviolet resistance and the photo-aging resistance of the PET substrate.
Further, the lubricant is one or more of zinc stearate, calcium stearate, polyethylene wax, ethylene bis-stearamide and pentaerythritol stearate.
Further, the modified PET resin is prepared by the steps of:
s1, adding furoic acid, triethylamine and anhydrous methylene dichloride into a dry three-neck flask provided with a stirring device, a condensing reflux device and a nitrogen guide pipe, introducing nitrogen, continuously introducing for 10min, then adding ethylenediamine and DIC (N, N-diisopropylcarbodiimide, a dehydrating agent), and after the addition, cooling to room temperature and N 2 Stirring under protection for reaction for 3h, extracting with hot distilled water (at 60-70deg.C) for three times after the reaction, drying the organic layer with anhydrous magnesium sulfate, and rotary evaporating to remove dichloromethane to obtain intermediate 1; the dosage ratio of furancarboxylic acid, triethylamine, anhydrous dichloromethane, ethylenediamine and DIC is 0.1mol:10.1g:300mL:0.105mol:12.6g;
under the action of triethylamine and DIC, the-COOH on furancarboxylic acid molecule and the-NH on ethylenediamine molecule 2 Amidation reaction is carried out, and only one-NH of one end of the ethylenediamine is enabled by controlling the molar ratio of the two to be close to 1:1 and slightly excessive ethylenediamine 2 Takes part in the reaction to obtain intermediate 1, the reaction process is as follows:
s2, adding the intermediate 1 and absolute ethyl alcohol into a three-neck flask with a stirring device, starting 250r/min to stir at a constant speed, heating, slowly dripping the epoxyfluoropropane into the flask by adopting a constant pressure dropping funnel when the temperature is stabilized at 65-70 ℃, stirring and reacting for 2 hours at the constant temperature of 70 ℃ after the dripping is completed, and removing the ethanol and the excessive epoxyfluoropropane by rotary evaporation after the reaction is completed to obtain an intermediate 2; the dosage ratio of the intermediate 1, the absolute ethyl alcohol and the epoxyfluoropropane is 15.4g:150mL:19g;
epoxy groups on the epoxyfluoropropane molecule and-NH on intermediate 1 2 The ring-opening reaction takes place to obtain intermediate 2, the reaction process is as follows:
s3, adding the intermediate 2 and acetonitrile into a three-neck flask with a stirring device, adding methyl iodide after stirring and dissolving, stirring and reacting for 10 hours at room temperature, stopping the reaction, concentrating under reduced pressure (removing acetonitrile), adding deionized water, and carrying out anion (Cl) - ) Exchange resin, decompress and concentrate to get modified monomer; the ratio of the amount of intermediate 2 to the amount of methyl iodide is 30.6g to 17.1g;
the tertiary amine on the intermediate 2 and methyl iodide are subjected to alkylation reaction to obtain a modified monomer, wherein the reaction process is shown as follows, and the modified monomer molecule contains a dihydric alcohol structure and can participate in the subsequent polymerization process;
s4, adding terephthalic acid, ethylene glycol and antimony trioxide into a reaction kettle, reacting for 2 hours at the temperature of 240 ℃ and the pressure of 0.35MPa, adding a modified monomer into a reaction system, performing a preshrinking reaction for 1 hour at the temperature of 240 ℃ and the vacuum degree of 1000Pa, then heating to 250 ℃ and reacting for 3 hours at the vacuum degree of 100Pa, finally discharging to a water tank, rapidly cooling, and granulating and drying to obtain modified PET resin; the dosage ratio of terephthalic acid, ethylene glycol, antimony trioxide and modified monomer is 100g:40-50g:0.04-0.05g:10-12g;
under the catalysis of antimony trioxide, terephthalic acid, ethylene glycol and a modified monomer undergo a polymerization reaction to obtain the modified PET resin.
The modified monomer is distributed in a PET molecular chain in a block mode, namely, the main chain of the modified PET molecular contains nitrogen positive ions, the side chain contains amide bonds, furan rings and fluorine-containing groups, the nitrogen positive ions on the main chain can increase charge density and promote charge transfer, and the nitrogen in the amide bonds on the side chain and the oxygen in the furan rings carry lone pair electrons, so that the modified PET resin has the capability of accepting protons, and can realize electrostatic dissipation effect through the transfer of internal protons, so that the nitrogen positive ions on the main chain, the amide bonds on the side chain and the furan rings can realize antistatic effect through different mechanisms, and have synergistic effect, and therefore, the modified PET resin is endowed with excellent antistatic performance; in addition, nitrogen positive ions on the main chain belong to quaternary ammonium salt functional groups and antibacterial active ingredients, and can endow the modified PET resin with certain antibacterial performance, so that the situations of short service life and functional failure caused by microbial pollution of the PET substrate in the process of storage or use are improved; it should be further noted that, because the antistatic and antibacterial active ingredients are distributed in the PET molecular chain in a block manner, compared with the blending or external addition manner, the anti-static and antibacterial active ingredients are difficult to exude, and have the durability of the functional effect;
in addition, the fluorine-containing groups contained in the modified PET molecular side chains have low surface free energy and stable chemical properties, and can migrate to the surface of the film material in the film forming process to play a synergistic effect with the organosilicon release agent, so that the amphiphobic performance, the antifouling capacity and the chemical corrosion resistance of the release agent are improved.
The invention has the beneficial effects that:
the PET substrate adopted by the release film disclosed by the invention has good toughness and photo-aging resistance after being modified, has lasting antistatic performance and antibacterial property, and can be used for generating a synergistic promotion effect with an organosilicon release agent to improve the amphiphobic performance, the antifouling capability and the chemical corrosion resistance of the release agent, so that the obtained release film has extremely high application value.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, 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.
Example 1
Preparation of modified PET resin:
s1, adding 0.1mol of furancarboxylic acid, 10.1g of triethylamine and 300mL of anhydrous methylene dichloride into a dry three-neck flask provided with a stirring device, a condensing reflux device and a nitrogen guide pipe, introducing nitrogen, continuously introducing for 10min, then adding 0.105mol of ethylenediamine and 12.6g of DIC, and after the addition, cooling to room temperature and N 2 Stirring under protection for reaction for 3h, extracting with hot distilled water (60 ℃) for three times after the reaction is finished, taking an organic layer, drying with anhydrous magnesium sulfate, and finally removing dichloromethane by rotary evaporation to obtain an intermediate 1;
s2, adding 15.4g of intermediate 1 and 150mL of absolute ethyl alcohol into a three-neck flask with a stirring device, starting 250r/min to stir at a constant speed, heating, slowly dripping 19g of epoxyfluoropropane into the flask by adopting a constant pressure dropping funnel when the temperature is stabilized at 65-70 ℃, stirring and reacting for 2 hours at the constant temperature of 70 ℃ after the dripping is completed, and removing ethanol and excessive epoxyfluoropropane by rotary evaporation after the reaction is completed to obtain an intermediate 2;
s3, adding 30.6g of intermediate 2 and 150mL of acetonitrile into a three-neck flask with a stirring device, adding 17.1g of methyl iodide after stirring and dissolving, stirring at room temperature for reaction for 10 hours, stopping the reaction, concentrating under reduced pressure, adding deionized water, and adding anions (Cl) - ) Exchange resin, decompress and concentrate to get modified monomer;
s4, adding 100g of terephthalic acid, 40g of ethylene glycol and 0.04g of antimony trioxide into a reaction kettle, reacting for 2 hours at the temperature of 240 ℃ and the pressure of 0.35MPa, adding 10g of modified monomer into the reaction system, performing a preshrinking reaction for 1 hour at the temperature of 240 ℃ and the vacuum degree of 1000Pa, then heating to 250 ℃ and reacting for 3 hours at the vacuum degree of 100Pa, finally discharging to a water tank, rapidly cooling, and performing the procedures of granulating and drying to obtain the modified PET resin.
Example 2
Preparation of modified PET resin:
s1, adding 0.1mol of furancarboxylic acid, 10.1g of triethylamine and 300mL of anhydrous methylene dichloride into a dry three-neck flask provided with a stirring device, a condensing reflux device and a nitrogen guide pipe, introducing nitrogen, continuously introducing for 10min, then adding 0.105mol of ethylenediamine and 12.6g of DIC, and after the addition, cooling to room temperature and N 2 Stirring under protection for reaction for 3h, extracting with hot distilled water (70 ℃) for three times after the reaction is finished, taking an organic layer, drying with anhydrous magnesium sulfate, and finally removing dichloromethane by rotary evaporation to obtain an intermediate 1;
s2, adding 15.4g of intermediate 1 and 150mL of absolute ethyl alcohol into a three-neck flask with a stirring device, starting 250r/min to stir at a constant speed, heating, slowly dripping 19g of epoxyfluoropropane into the flask by adopting a constant pressure dropping funnel when the temperature is stabilized at 65-70 ℃, stirring and reacting for 2 hours at the constant temperature of 70 ℃ after the dripping is completed, and removing ethanol and excessive epoxyfluoropropane by rotary evaporation after the reaction is completed to obtain an intermediate 2;
s3, adding 30.6g of intermediate 2 and 150mL of acetonitrile into a three-neck flask with a stirring device, adding 17.1g of methyl iodide after stirring and dissolving, stirring at room temperature for reaction for 10 hours, stopping the reaction, concentrating under reduced pressure, adding deionized water, and adding anions (Cl) - ) Exchange resin, decompress and concentrate to get modified monomer;
s4, adding 100g of terephthalic acid, 50g of ethylene glycol and 0.05g of antimony trioxide into a reaction kettle, reacting for 2 hours at the temperature of 240 ℃ and the pressure of 0.35MPa, adding 12g of modified monomer into the reaction system, performing a preshrinking reaction for 1 hour at the temperature of 240 ℃ and the vacuum degree of 1000Pa, then heating to 250 ℃ and reacting for 3 hours at the vacuum degree of 100Pa, finally discharging to a water tank, rapidly cooling, and performing the procedures of granulating and drying to obtain the modified PET resin.
Example 3
Preparing a PET substrate:
50 parts of modified PET resin prepared in example 1, 20 parts of polybutylene terephthalate, 0.8 part of ultraviolet absorber UV-P and 3 parts of zinc stearate are weighed according to parts by weight, fully and uniformly mixed, heated and dried, then added into a melt extrusion device for extrusion, and stretched, heat-set, cooled and rolled to obtain the PET substrate.
Example 4
Preparing a PET substrate:
55 parts of modified PET resin prepared in example 2, 25 parts of polybutylene terephthalate, 0.9 part of ultraviolet absorber UVP-327 and 3.5 parts of calcium stearate are weighed according to parts by weight, fully and uniformly mixed, heated and dried, then added into a melt extrusion device for extrusion, and stretched, heat-set, cooled and rolled to obtain the PET substrate.
Example 5
Preparing a PET substrate:
60 parts of modified PET resin prepared in example 1, 30 parts of polybutylene terephthalate, 744 parts of light stabilizer and 4 parts of polyethylene wax are weighed according to parts by weight, fully and uniformly mixed, heated and dried, then added into a melt extrusion device for extrusion, and the PET substrate is obtained through stretching, heat setting, cooling and rolling.
Comparative example 1
Preparing a PET substrate:
50 parts of PET resin, 20 parts of polybutylene terephthalate, 0.8 part of ultraviolet absorber UV-P and 3 parts of zinc stearate are weighed according to parts by weight, fully and uniformly mixed, heated and dried, then added into a melt extrusion device for extrusion, and the PET substrate is obtained through stretching, heat setting, cooling and rolling.
The PET substrates obtained in examples 3 to 5 and comparative example 1 were subjected to antibacterial property test, and the antibacterial rates of the PET substrates in examples 3 to 5 against Staphylococcus aureus and Escherichia coli were >95%, and the antibacterial rates of the PET substrate in comparative example 1 against Staphylococcus aureus and Escherichia coli were <70%.
Example 6
A release film was prepared by coating a release agent of Sly-off SL9106 on one side of the PET substrate prepared in example 3.
Example 7
A release film was prepared by coating a release agent of Sly-off SL7558 on one side of the PET substrate prepared in example 4.
Example 8
A release film was prepared by coating a release agent of Sly-off SL7920 on one side of the PET substrate prepared in example 5.
Comparative example 2
A release film was prepared by coating a release agent of Sly-off SL9106 on one side of the PET substrate prepared in comparative example 1.
The release films obtained in examples 6 to 8 and comparative example 2 were subjected to performance test, and the results are shown in the following table:
from the data in the table, the release film obtained by the invention simultaneously meets antistatic property and release property; and as can be seen from the data of comparative example 2, the PET substrate modified by the modified monomer can effectively improve the antistatic property of the release film, and can act with the release agent to improve the release property.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (9)
1. The release film comprises a PET substrate, wherein one side of the PET substrate is coated with an organosilicon release agent, and the release film is characterized by comprising the following raw materials in parts by weight: 50-60 parts of modified PET resin, 20-30 parts of polybutylene terephthalate, 0.8-1 part of ultraviolet absorber and 3-4 parts of lubricant;
wherein the modified PET resin is prepared by the following steps:
s1, adding furoic acid, triethylamine and anhydrous methylene dichloride into a dry three-neck flask provided with a stirring device, a condensing reflux device and a nitrogen guide pipe, introducing nitrogen, continuously introducing for 10min, then adding ethylenediamine and DIC, and after the addition, cooling to room temperature and N 2 Stirring under protection for reaction for 3h, extracting with hot distilled water for three times after the reaction is finished, drying an organic layer with anhydrous magnesium sulfate, filtering, and finally removing dichloromethane by rotary evaporation to obtain an intermediate 1;
s2, adding the intermediate 1 and absolute ethyl alcohol into a three-neck flask with a stirring device, starting uniform stirring, heating, slowly dripping the epoxyfluoropropane into the flask by adopting a constant-pressure dropping funnel when the temperature is stabilized at 65-70 ℃, stirring and reacting for 2 hours at the constant temperature of 70 ℃ after the dripping is completed, and removing the ethanol and excessive epoxyfluoropropane by rotary evaporation after the reaction is completed to obtain an intermediate 2;
s3, adding the intermediate 2 and acetonitrile into a three-neck flask with a stirring device, stirring and dissolving, then adding methyl iodide, stirring and reacting for 10 hours at room temperature, stopping the reaction, concentrating under reduced pressure, adding deionized water, exchanging by anion exchange resin, concentrating under reduced pressure, and obtaining a modified monomer;
s4, taking terephthalic acid, ethylene glycol and a modified monomer as raw materials to carry out polymerization reaction, so as to obtain the modified PET resin.
2. The release film of claim 1, wherein the amount of furancarboxylic acid, triethylamine, anhydrous methylene chloride, ethylenediamine, DIC in step S1 is 0.1mol:10.1g:300ml:0.105mol:12.6g.
3. The release film according to claim 1, wherein the ratio of the amounts of intermediate 1, absolute ethanol and epoxyfluoropropane in step S2 is 15.4g:150ml:19g.
4. A release film according to claim 1, wherein the ratio of the amounts of intermediate 2 and methyl iodide in step S3 is 30.6g to 17.1g.
5. The release film according to claim 1, wherein the specific operation of step S4 is as follows: adding terephthalic acid, ethylene glycol and antimony trioxide into a reaction kettle, reacting for 2 hours at the temperature of 240 ℃ and the pressure of 0.35MPa, adding a modified monomer into a reaction system, performing a preshrinking reaction for 1 hour at the temperature of 240 ℃ and the vacuum degree of 1000Pa, then heating to 250 ℃ and reacting for 3 hours at the vacuum degree of 100Pa, finally discharging to a water tank, rapidly cooling, and granulating and drying to obtain the modified PET resin.
6. The release film of claim 5, wherein the amount of terephthalic acid, ethylene glycol, antimony trioxide, and modifying monomer is 100g to 50g to 0.04 to 0.05g to 10 to 12g.
7. A release film according to claim 1, wherein the ultraviolet light absorber is one or more of ultraviolet light absorber UV-P, ultraviolet light absorber UVP-327 or light stabilizer 744.
8. The release film of claim 1, wherein the lubricant is one or more of zinc stearate, calcium stearate, polyethylene wax, ethylene bis stearamide, pentaerythritol stearate.
9. The method for preparing a release film according to claim 1, which is characterized by comprising the following steps:
weighing the raw materials in the PET substrate according to a proportion, fully and uniformly mixing, heating and drying, adding into a melt extrusion device for extrusion, stretching, heat setting, cooling and rolling to obtain the PET substrate, and coating an organosilicon release agent on one side of the PET substrate to obtain the release film.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117024806A (en) * | 2023-08-14 | 2023-11-10 | 苏州市奥贝新材料科技有限公司 | Preparation method of high-temperature-resistant enhanced PET release film |
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| CN111363319A (en) * | 2020-03-22 | 2020-07-03 | 李丹丹 | Antibacterial and antistatic polyester film |
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| CN108676188A (en) * | 2018-05-17 | 2018-10-19 | 天津宝兴威科技股份有限公司 | A kind of preparation process of antistatic modified PET release films |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117024806A (en) * | 2023-08-14 | 2023-11-10 | 苏州市奥贝新材料科技有限公司 | Preparation method of high-temperature-resistant enhanced PET release film |
| CN117024806B (en) * | 2023-08-14 | 2024-01-30 | 苏州市奥贝新材料科技有限公司 | Preparation method of high-temperature-resistant enhanced PET release film |
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