CN115433528A - PET (polyethylene terephthalate) protective film and preparation method thereof - Google Patents
PET (polyethylene terephthalate) protective film and preparation method thereof Download PDFInfo
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- CN115433528A CN115433528A CN202211269311.9A CN202211269311A CN115433528A CN 115433528 A CN115433528 A CN 115433528A CN 202211269311 A CN202211269311 A CN 202211269311A CN 115433528 A CN115433528 A CN 115433528A
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- 230000001681 protective effect Effects 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229920000139 polyethylene terephthalate Polymers 0.000 title claims description 108
- -1 polyethylene terephthalate Polymers 0.000 title claims description 57
- 239000005020 polyethylene terephthalate Substances 0.000 title description 95
- 239000000853 adhesive Substances 0.000 claims abstract description 7
- 230000001070 adhesive effect Effects 0.000 claims abstract description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 72
- 239000002585 base Substances 0.000 claims description 45
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 36
- 238000000576 coating method Methods 0.000 claims description 33
- 239000011248 coating agent Substances 0.000 claims description 32
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 24
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 24
- 229920002799 BoPET Polymers 0.000 claims description 23
- 238000010534 nucleophilic substitution reaction Methods 0.000 claims description 19
- 238000000605 extraction Methods 0.000 claims description 18
- 238000004821 distillation Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000012074 organic phase Substances 0.000 claims description 15
- 239000003208 petroleum Substances 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 12
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 11
- 238000006467 substitution reaction Methods 0.000 claims description 11
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- RXNYJUSEXLAVNQ-UHFFFAOYSA-N 4,4'-Dihydroxybenzophenone Chemical compound C1=CC(O)=CC=C1C(=O)C1=CC=C(O)C=C1 RXNYJUSEXLAVNQ-UHFFFAOYSA-N 0.000 claims description 9
- 238000003851 corona treatment Methods 0.000 claims description 8
- 125000001273 sulfonato group Chemical class [O-]S(*)(=O)=O 0.000 claims description 8
- SGRHVVLXEBNBDV-UHFFFAOYSA-N 1,6-dibromohexane Chemical compound BrCCCCCCBr SGRHVVLXEBNBDV-UHFFFAOYSA-N 0.000 claims description 7
- 238000007142 ring opening reaction Methods 0.000 claims description 7
- VWEYDBUEGDKEHC-UHFFFAOYSA-N 3-methyloxathiolane 2,2-dioxide Chemical compound CC1CCOS1(=O)=O VWEYDBUEGDKEHC-UHFFFAOYSA-N 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 5
- 230000005855 radiation Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 14
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000003287 optical effect Effects 0.000 abstract description 5
- 230000003749 cleanliness Effects 0.000 abstract description 2
- 238000005520 cutting process Methods 0.000 abstract description 2
- 238000004100 electronic packaging Methods 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract description 2
- 238000013508 migration Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 230000009967 tasteless effect Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 37
- 238000012360 testing method Methods 0.000 description 13
- 239000000758 substrate Substances 0.000 description 10
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 8
- 239000012528 membrane Substances 0.000 description 8
- 230000003068 static effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229920000767 polyaniline Polymers 0.000 description 6
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000012790 adhesive layer Substances 0.000 description 5
- 239000002216 antistatic agent Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical group OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002801 charged material Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000012777 electrically insulating material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- AQFWNELGMODZGC-UHFFFAOYSA-N o-ethylhydroxylamine Chemical compound CCON AQFWNELGMODZGC-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
-
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
-
- 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
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- 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
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
-
- 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
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
Abstract
The invention discloses a PET protective film and a preparation method thereof, and belongs to the technical field of layered products. The PET protective film prepared by the invention is environment-friendly, nontoxic and tasteless, and the surface of the product has no electrostatic material migration phenomenon; the adhesive has the advantages of excellent cleanliness, excellent antistatic performance, durable and stable performance after adhesion and good weather resistance. The invention is suitable for optical industry and electronic packaging, and can be used for surface protection of various electronic optical materials in the die cutting process.
Description
Technical Field
The invention relates to the technical field of layered products, in particular to a PET (polyethylene terephthalate) protective film and a preparation method thereof.
Background
The PET film is a film material with excellent and comprehensive performance, good transparency and mechanical performance, and better toughness, tensile strength and impact strength than the common film. The PET film also has excellent heat resistance, cold resistance and good chemical resistance and oil resistance, but is not resistant to strong alkali and is easy to be charged with static electricity. The PET film is a polar electrically insulating material, and has characteristics of low dielectric constant and high surface resistance, which makes it impossible to transfer charges generated by friction, shearing, and the like, and easily accumulates electrostatic charges to constitute static electricity. Therefore, the method reduces the static electricity of the PET film material by various means, and has important significance for expanding the application field of the PET film material.
Chinese patent CN107245192a discloses a PET antistatic protective film, which comprises: substrate thin layer and antistatic thin layer, antistatic thin layer covers substrate thin layer surface, the substrate thin layer is made by PET, synthetic resin and polytetrafluoroethylene material, antistatic thin layer is made by zirconium dioxide, polypropylene, look female, antistatic agent material includes the mixture of glycerin monostearate and ethoxy amine. Through the mode, the PET anti-static protective film is suitable for packaging of static sensitive products such as PCBs and ICs, damage caused by static discharge can be prevented, and sensing parts such as MOS, CMOS and FET accessories can be safely carried out after being packaged by an anti-static shielding bag. However, there is a drawback in that the substrate film layer and the antistatic film layer are bonded to prevent generation of static electricity, and the bonding ability between the antistatic agent in the antistatic film layer and the substrate is weak. In the long-term use process, the antistatic film layer can be gradually aged under the influence of environmental factors such as illumination and rainwater, so that the antistatic agent is lost, and the service life of the PET antistatic protective film is shortened.
The functional substance with the antistatic effect is connected with the substrate through grafting reaction, so that the binding capacity of the antistatic component and the substrate can be improved, and the functional loss caused by the loss of the antistatic agent is overcome to a certain extent. Chinese patent CN108623976A provides an antistatic shading PET film and a preparation method thereof, and the antistatic shading PET film takes polyethylene terephthalate grafted styrene sulfonic acid, polyaniline coated nano-copper, a coupling agent, an antioxidant and a lubricant as raw materials. Compared with the prior art, the invention takes the sulfonic acid group of polyethylene glycol terephthalate grafted styrene sulfonic acid as a doping agent to greatly improve the conductivity of polyaniline, and simultaneously, the existence of the styrene sulfonic acid group weakens the rigidity of a polyethylene glycol terephthalate chain, reduces the processing melting temperature of the polyethylene glycol terephthalate, and further improves the compatibility of the polyethylene glycol terephthalate grafted styrene sulfonic acid with polyaniline microspheres; secondly, the nano-copper particles coated with the polyaniline have good conductivity, and the nano-copper coated with the polyaniline has greatly improved compatibility with a matrix due to the existence of the conductive polyaniline on the surface, and meanwhile, the antistatic performance of the nano-copper is not reduced. The patent improves the binding capacity of the antistatic component and the substrate, but in the process of grafting and combining the antistatic component and the substrate through the PET surface active group, the molecular structure of the surface can be locally damaged, the surface roughness is increased, the mechanical property is reduced, and the application range of the antistatic component is further limited.
Disclosure of Invention
In view of the above defects in the prior art, the present invention provides a PET protective film with excellent mechanical properties and good antistatic effect, and a preparation method thereof.
In order to improve the adhesion capability of the antistatic component on the surface of the PET protective film and further improve the weather resistance of the PET protective film, the antistatic treatment agent is combined with the base film in a covalent bond combination mode to form the antistatic layer. Compared with the mode that materials such as resin are used as antistatic layer matrixes to form coatings on the PET base film in the prior art, the antistatic treatment agent disclosed by the invention cannot be lost due to decomposition damage and aging of the resin, and is beneficial to prolonging the service life of the PET protective film.
In addition, compared with the traditional mode that the PET base membrane is processed, active groups such as hydroxyl and carboxyl are formed and then coupling or grafting is carried out to form a covalent bond, the method uses hydrogen extraction reaction catalyzed by ultraviolet light to combine quaternary ammonium salt type compounds and sulfonate type compounds on PET molecular chains. Compared with the traditional process, the covalent connection formed by adopting the method has small damage to the surface of PET, greatly reduces the damage to the connection bond of the PET molecular chain skeleton, and cannot cause the reduction of the mechanical property of the PET protective film.
A preparation method of a PET protective film comprises the following steps:
s1, base film treatment: carrying out corona treatment on one side of the PET base film through a corona device to obtain a single-side corona PET base film for later use;
s2, preparing a dry glue layer: coating adhesive on the corona surface of the single-sided corona PET base film by adopting automatic coating equipment, and curing to obtain a viscous PET film for later use;
s3, preparing an antistatic layer: and coating an antistatic treatment agent on the non-corona surface of the viscous PET film by automatic coating equipment, and performing ultraviolet irradiation treatment after coating to obtain the PET protective film.
Preferably, the thickness of the PET base film in the step S1 is 50 to 80 μm.
Preferably, the power of the corona treatment in the step S1 is 0.5 to 2kW, the frequency is 10 to 20kHz, and the linear speed of the film during treatment is 2 to 6m/min.
Preferably, the adhesive in step S2 is any one of an organic silicon pressure-sensitive adhesive, a polyacrylate pressure-sensitive adhesive, and a polyurethane pressure-sensitive adhesive.
Preferably, the curing temperature in the step S2 is 35 to 45 ℃, and the curing time is 12 to 48h.
Preferably, the thickness of the dry adhesive layer of the adhesive PET film in the step S2 is 10 to 15 μm.
Preferably, the ultraviolet light irradiation treatment in the step S3 has an ultraviolet light wavelength of 320 to 380nm and an irradiation illuminance of 1.5 to 1.8mW/cm 2 The processing time is 0.5 to 2min.
Preferably, the thickness of the antistatic layer of the PET protective film in the step S3 is 0.2 to 0.8 μm.
Preferably, the antistatic treatment agent in step S3 is one or both of a quaternary ammonium salt type compound and a sulfonate type compound.
Preferably, the antistatic treatment agent is a mixture of a quaternary ammonium salt type compound and a sulfonate type compound in a mass ratio of 3.5 to 6:1 of the mixture formed.
The invention takes 4,4' -dihydroxy benzophenone and 1,6-dibromohexane as reaction raw materials, a bromo compound is obtained through substitution reaction, and the bromo compound is taken as a base to be respectively subjected to nucleophilic substitution with decyl dimethyl tertiary amine or dimethylamine. The product obtained by the reaction with the product, namely the quaternary ammonium salt compound with a long-chain structure, is reacted with dimethylamine to obtain a product, and then the product is subjected to ring-opening addition with 2,4-butyl sultone to obtain the sulfonate compound, wherein the end group hydrophilicity of the obtained sulfonate compound is strong, the chain length of the obtained sulfonate compound is shorter than that of the quaternary ammonium salt compound, and the sulfonate compound and the quaternary ammonium salt compound can complement each other by adopting the combination and the use of a specific proportion.
The quaternary ammonium salt type compound and the sulfonate type compound are combined through a photochemical hydrogen abstraction reaction between carbonyl and a carbon hydrogen bond on a PET framework, and a polar effect between the quaternary ammonium salt type compound and the end group of the sulfonate type compound can promote a three-dimensional conductive network to be formed on the surface of the PET base film. The molecular chain of the quaternary ammonium salt compound has the length advantage, so that the required lapping times are less, and a longer conductive path can be formed; the quaternary ammonium salt compound is easier to connect adjacent conductive paths, thereby forming more crossed conductive paths, releasing the charges accumulated on the surface of the PET in time and achieving the antistatic effect. The sulfonate compound has a slightly short chain length, and the terminal group has polarity, so that the interaction between molecular chains can be enhanced, and the cohesion of the quaternary ammonium compound and the sulfonate compound chain can be improved. The long chains form loose reticular conductive paths, and the short chains form a more compact structure in the conductive paths, so that the conductive paths are further increased; due to the strong interaction force among molecules, the mechanical strength of the antistatic layer is also optimized macroscopically, and the mechanical property of the PET protective film is enhanced.
Preferably, the quaternary ammonium salt compound is prepared by the following method in parts by weight:
m1, uniformly mixing 2.8 to 3.6 parts of 4,4' -dihydroxybenzophenone, 6.4 to 8.2 parts of 1,6-dibromohexane and 75 to 150 parts of acetonitrile, and then adding 10.8 to 14 parts of potassium carbonate as alkali and 0.65 to 0.84 part of potassium iodide as a catalyst; heating and carrying out substitution reaction, removing acetonitrile by reduced pressure distillation after the reaction is finished, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified bromo-compound for later use;
m2, taking 3.2 to 4.2 parts of the purified brominated compound, 2.3 to 2.9 parts of decyl dimethyl tertiary amine and 50 to 100 parts of acetonitrile, uniformly mixing, and then adding 9.0 to 11.7 parts of potassium carbonate as an alkali and 0.53 to 0.69 part of potassium iodide as a catalyst; heating and carrying out nucleophilic substitution, removing acetonitrile through reduced pressure distillation after the reaction is finished, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain the quaternary ammonium salt compound.
More preferably, the temperature of the substitution reaction in the step M1 is 65 to 75 ℃, and the reaction time is 3 to 5h.
Further preferably, the temperature of the nucleophilic substitution in the step M2 is 80 to 95 ℃, and the reaction time is 4 to 6h.
Preferably, the sulfonate compound is prepared by the following steps in parts by weight:
n1, uniformly mixing 2.8 to 3.6 parts of 4,4' -dihydroxybenzophenone, 6.4 to 8.2 parts of 1,6-dibromohexane and 75 to 150 parts of acetonitrile, and then adding 10.8 to 14 parts of potassium carbonate as alkali and 0.65 to 0.84 part of potassium iodide as a catalyst; heating and carrying out substitution reaction, removing acetonitrile by reduced pressure distillation after the reaction is finished, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified bromo compound for later use;
n2, taking 3.2 to 4.2 parts of the purified bromo compound, 0.54 to 0.70 part of dimethylamine and 75 to 125 parts of acetone, uniformly mixing, and then adding 9.0 to 11.7 parts of potassium carbonate as an alkali and 0.53 to 0.69 part of potassium iodide as a catalyst; heating and carrying out nucleophilic substitution, removing acetone through reduced pressure distillation after the reaction is finished, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified nucleophilic substitution product for later use;
and N3, uniformly mixing 2.8 to 3.6 parts of the purified nucleophilic substitution product, 0.8 to 1.0 part of 2,4-butanesultone and 75 to 150 parts of acetonitrile, heating in an anaerobic closed environment to perform ring-opening addition, removing the acetonitrile through reduced pressure distillation after the reaction is finished, then adding water and petroleum ether to perform extraction and liquid separation, collecting an organic phase, and drying to obtain the sulfonate type compound.
More preferably, the temperature of the substitution reaction in the step N1 is 65 to 75 ℃, and the reaction time is 3 to 5h.
Further preferably, the temperature of nucleophilic substitution in the step N2 is 60 to 65 ℃, and the reaction time is 2 to 4h.
More preferably, the temperature of the ring-opening addition in the step N3 is 125 to 140 ℃, and the reaction time is 2 to 6h.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The introduction and the function of part of raw materials in the formula of the invention are as follows:
PET basal membrane: the PET base film is a packaging film with relatively comprehensive performance. The transparency is good and the gloss is good; the air tightness and the fragrance retention are good; moderate moisture resistance and reduced moisture permeability at low temperatures. The PET basal membrane has excellent mechanical property, the toughness of the PET basal membrane is the best of all thermoplastic plastics, and the tensile strength and the impact strength are much higher than those of common films; and the product has good stiffness and stable size, and is suitable for secondary processing of printing, paper bags and the like. The PET base film also has excellent heat resistance, cold resistance and good chemical resistance and oil resistance, but is not resistant to strong alkali and is easy to be charged with static electricity.
The invention has the beneficial effects that:
compared with the prior art, the PET protective film with a multilayer structure is prepared, is environment-friendly, nontoxic and tasteless, and has no electrostatic material migration phenomenon on the surface of the product; the adhesive has the advantages of excellent cleanliness, excellent antistatic performance, durable and stable performance after adhesion and good weather resistance. The invention is suitable for optical industry and electronic packaging, and can be used for surface protection of various electronic optical materials in the die cutting process.
Compared with the prior art, the antistatic treatment agent is combined with the base film to form the antistatic layer in a covalent bond combination mode, and compared with a mode of forming a coating on the PET base film by using materials such as resin as an antistatic layer substrate, the antistatic treatment agent disclosed by the invention cannot be lost due to decomposition damage and aging of the resin, so that the adhesion capability of antistatic components on the surface of the PET protective film is improved, the weather resistance of the PET protective film is further improved, and the service life of the PET protective film is favorably prolonged.
Compared with the prior art, the method disclosed by the invention has the advantages that the antistatic treatment agent is combined on the PET molecular chain by using the hydrogen extraction reaction catalyzed by ultraviolet light, and compared with a mode that the PET base film is treated by forming a covalent bond formed by coupling or grafting after forming active groups such as hydroxyl, carboxyl and the like, the method disclosed by the invention has small damage to the PET surface, greatly reduces the damage to the connecting bond of the PET molecular chain skeleton, and is beneficial to maintaining the mechanical property of the PET protective film.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the invention thereto. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Some raw material parameters in the comparative examples and examples of the invention are as follows:
PET base film, thickness: 50 μm, the longitudinal tensile strength is more than or equal to 150MPa, and the method is provided by Henan golden insulating new materials Co.Ltd;
organic silicon pressure sensitive adhesive, grade: SH-9168 is provided by chemical industry Co., ltd in New four seas in Hubei;
4,4' -dihydroxybenzophenone, CAS number: 611-99-4, provided by Nantong Runfeng petrochemical company, inc.;
decyl dimethyl tertiary amine, CAS number: 1120-24-7, available from Shandong Jiapeng New materials, inc.;
2,4-butanesultone, CAS number: 1121-03-5, available from chemical Limited, wande Hubei.
Example 1
The PET protective film is composed of a dry glue layer, a PET base film and an antistatic layer, and is prepared by the following method:
s1, base film treatment: carrying out corona treatment on one surface of the PET base film through a corona device, wherein the corona power is 0.5kW, the frequency is 15kHz, and the linear speed of the film during treatment is 3.5m/min, so as to obtain a single-surface corona PET base film for later use;
s2, preparing a dry glue layer: coating organic silicon pressure-sensitive adhesive on the corona surface of the single-side corona PET base film by using automatic coating equipment, and curing at the temperature of 130 ℃ for 24 hours after coating to obtain a viscous PET film for later use;
s3, preparing an antistatic layer: coating the non-corona surface of the viscous PET film with a quaternary ammonium salt compound by automatic coating equipment, and performing ultraviolet irradiation treatment after coating, wherein the wavelength of ultraviolet light is 360nm, and the irradiation illumination is 1.5mW/cm 2 And treating for 1min to obtain the PET protective film.
The thickness of the PET basal membrane is 50 mu m, the thickness of the dry adhesive layer of the viscous PET film is 10 mu m, and the thickness of the antistatic layer is 0.5 mu m.
The preparation method of the quaternary ammonium salt compound comprises the following steps:
m1, mixing 2.8kg of 4,4' -dihydroxybenzophenone, 6.4kg of 1, 6-dibromohexane and 75kg of acetonitrile uniformly, and then adding 10.8kg of potassium carbonate as alkali and 0.65kg of potassium iodide as catalyst; heating and carrying out substitution reaction at 75 ℃ for 3h; after the reaction is finished, removing acetonitrile through reduced pressure distillation, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified bromo-compound for later use;
m2, taking 3.2kg of the purified brominated compound, 2.3kg of decyl dimethyl tertiary amine and 75kg of acetonitrile, uniformly mixing, and then adding 9.0kg of potassium carbonate serving as an alkali and 0.53kg of potassium iodide serving as a catalyst; heating and carrying out nucleophilic substitution, wherein the temperature of the nucleophilic substitution is 85 ℃, and the reaction time is 5h; and after the reaction is finished, removing acetonitrile through reduced pressure distillation, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain the quaternary ammonium salt compound.
Example 2
The PET protective film is composed of a dry glue layer, a PET base film and an antistatic layer, and is prepared by the following method:
s1, base film treatment: carrying out corona treatment on one side of the PET base film by a corona device, wherein the corona power is 0.5kW, the frequency is 15kHz, and the linear speed of the film is 3.5m/min during treatment, so as to obtain a single-side corona PET base film for later use;
s2, preparing a dry glue layer: coating organic silicon pressure-sensitive adhesive on the corona surface of the single-side corona PET base film by using automatic coating equipment, and curing at the temperature of 130 ℃ for 24 hours after coating to obtain a viscous PET film for later use;
s3, preparing an antistatic layer: coating sulfonate compound on the non-corona surface of the viscous PET film by automatic coating equipment, and performing ultraviolet irradiation treatment after coating, wherein the wavelength of ultraviolet light is 360nm, and the irradiation illumination is 1.5mW/cm 2 And treating for 1min to obtain the PET protective film.
The thickness of the PET basal membrane is 50 μm, the thickness of the dry adhesive layer of the viscous PET film is 10 μm, and the thickness of the antistatic layer is 0.5 μm.
The preparation method of the sulfonate compound comprises the following steps:
n1, 2.8kg of 4,4' -dihydroxybenzophenone, 6.4kg of 1, 6-dibromohexane and 75kg of acetonitrile are mixed uniformly, and then 10.8kg of potassium carbonate serving as alkali and 0.65kg of potassium iodide serving as a catalyst are added; heating and carrying out substitution reaction at 75 ℃ for 3h; after the reaction is finished, removing acetonitrile through reduced pressure distillation, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified bromo-compound for later use;
n2, 3.2kg of the purified brominated compound, 0.54kg of dimethylamine and 75kg of acetone are uniformly mixed, and then 9.0kg of potassium carbonate is added as an alkali, and 0.53kg of potassium iodide is added as a catalyst; heating and carrying out nucleophilic substitution, wherein the temperature of the nucleophilic substitution is 65 ℃, and the reaction time is 3h; after the reaction is finished, removing acetone by reduced pressure distillation, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified nucleophilic substitution product for later use;
n3, taking 2.8kg of the purified nucleophilic substitution product, 0.8kg of 2, 4-butanesultone and 75kg of acetonitrile, uniformly mixing, heating in an oxygen-free closed environment for ring-opening addition, wherein the temperature of the ring-opening addition is 130 ℃, and the reaction time is 4 hours; and after the reaction is finished, removing acetonitrile by reduced pressure distillation, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain the sulfonate compound.
Example 3
The PET protective film is composed of a dry glue layer, a PET base film and an antistatic layer, and is prepared by the following method:
s1, base film treatment: carrying out corona treatment on one side of the PET base film by a corona device, wherein the corona power is 0.5kW, the frequency is 15kHz, and the linear speed of the film is 3.5m/min during treatment, so as to obtain a single-side corona PET base film for later use;
s2, preparing a dry glue layer: coating organic silicon pressure-sensitive adhesive on the corona surface of the single-side corona PET base film by using automatic coating equipment, and curing at the temperature of 130 ℃ for 24 hours after coating to obtain a viscous PET film for later use;
s3, preparing an antistatic layer: coating an antistatic treatment agent on the non-corona surface of the viscous PET film by automatic coating equipment, and performing ultraviolet irradiation treatment after coating, wherein the wavelength of ultraviolet light is 360nm, and the irradiation illumination is 1.5mW/cm 2 And treating for 1min to obtain the PET protective film.
The thickness of the PET basal membrane is 50 μm, the thickness of the dry adhesive layer of the viscous PET film is 10 μm, and the thickness of the antistatic layer is 0.5 μm.
The antistatic treatment agent is prepared from a quaternary ammonium salt compound and a sulfonate compound in a mass ratio of 3.5:1 of the mixture formed.
The method for preparing the quaternary ammonium salt type compound was the same as that of example 1, and the method for preparing the sulfonate type compound was the same as that of example 2.
Comparative example 1
The PET protective film is composed of a dry glue layer, a PET base film and an antistatic layer, and is prepared by the following method:
s1, base film treatment: carrying out corona treatment on one side of the PET base film by a corona device, wherein the corona power is 0.5kW, the frequency is 15kHz, and the linear speed of the film is 3.5m/min during treatment, so as to obtain a single-side corona PET base film for later use;
s2, preparing a dry glue layer: and coating the corona surface of the single-side corona PET base film with organic silicon pressure-sensitive adhesive by adopting automatic coating equipment, and curing at the temperature of 130 ℃ for 24 hours after coating to obtain the PET protective film.
The thickness of the PET basal membrane is 50 μm, and the thickness of the dry adhesive layer of the adhesive PET film is 10 μm.
Test example 1
The electrostatic test of the PET protective film is carried out according to the specific method and steps in the national standard GB/T14447-1993 half-life method of the electrostatic test method of the plastic film. And uniformly intercepting 5 samples in each group according to requirements, wherein each sample can be tested only once, taking the arithmetic mean value of the half-life periods of the 5 samples as a test result, and taking two significant digits. The results of the static electricity test of the PET protective film are shown in table 1.
The shorter the electrostatic half-life is, the stronger the charge leakage performance of the charged material is reflected; for antistatic materials, it is desirable to have a low half-life. As can be seen from the test results in table 1, the example of the present invention using the antistatic treatment agent has a shorter half-life compared to the untreated PET film, wherein the half-life of example 3 is the shortest and the leakage performance to charges is the best. The result of this phenomenon may be that the quaternary ammonium compound and the sulfonate compound are combined through a photochemical hydrogen abstraction reaction between carbonyl groups and carbon hydrogen bonds on the PET skeleton, and a polar effect between the quaternary ammonium compound and the sulfonate compound end groups can promote the formation of a three-dimensional conductive network on the surface of the PET base film. The molecular chain of the quaternary ammonium salt compound has the length advantage, so that the required lapping times are less, and a longer conductive path can be formed; the quaternary ammonium salt compound is easier to connect adjacent conductive paths, so that more crossed conductive paths are formed, and the charges accumulated on the surface of the PET are released in time; the chain length of the sulfonate compound is slightly short, the long chain forms a loose reticular conductive path, the short chain is matched in the conductive path to form a more compact structure, the conductive path is increased, and the antistatic effect is achieved.
Test example 2
The tensile property test of the PET protective film is carried out according to the specific method and steps in the national standard GB/T25255-2010 method for measuring the tensile property of the optical function film polyethylene terephthalate (PET) film. The number of specimens per test direction was 5, the specimen width was 15mm, the length was 200mm, and the grip pitch was 100mm. Before testing, the sample is regulated for 48 hours at the temperature of 23 ℃ and the relative humidity of 50 percent; during testing, the testing speed is 100mm/min, and the arithmetic mean value is taken as the testing result. The tensile properties of the PET protective film were measured and the results are shown in table 2.
The tensile strength is the maximum bearing capacity of the material under the tensile condition, and the strength of the mechanical property of the PET protective film is reflected. As can be seen from the test results of table 2, the PET protective film of the present invention did not show a decrease in tensile strength, and is due to comparative example 1. The reason for the phenomenon is probably that the invention combines the antistatic treatment agent on the PET molecular chain by using the hydrogen extraction reaction catalyzed by ultraviolet light, has small damage to the PET surface, greatly reduces the damage to the connecting bond of the PET molecular chain skeleton, and is beneficial to maintaining the mechanical property of the PET protective film. The quaternary ammonium salt compound and the sulfonate compound are combined through photochemical hydrogen abstraction reaction between carbonyl and carbon-hydrogen bonds on a PET framework, a three-dimensional network structure can be promoted to be formed on the surface of the PET base film through a polar effect between the quaternary ammonium salt compound and the end group of the sulfonate compound, the sulfonate compound is short in chain length, the end group has polarity, interaction between molecular chains can be enhanced, and accordingly cohesion of the quaternary ammonium salt compound and the sulfonate compound chain is improved. Due to the strong interaction force among molecules, the mechanical strength of the antistatic layer is also optimized macroscopically, and the mechanical property of the PET protective film is enhanced.
Claims (7)
1. A preparation method of a PET protective film is disclosed, wherein the PET protective film is composed of a dry glue layer, a PET base film and an antistatic layer, and is characterized by comprising the following steps:
s1, treatment of a base film: carrying out corona treatment on one side of the PET base film through a corona device to obtain a single-side corona PET base film for later use;
s2, preparing a dry glue layer: coating adhesive on the corona surface of the single-side corona PET base film by using automatic coating equipment, and curing to obtain a viscous PET film for later use;
s3, preparing an antistatic layer: coating an antistatic treatment agent on the non-corona surface of the viscous PET film by automatic coating equipment, and performing ultraviolet irradiation treatment after coating to obtain the PET protective film;
the antistatic treatment agent is prepared by mixing a quaternary ammonium salt compound and a sulfonate compound in a mass ratio of (3.5-6): 1;
the preparation method of the quaternary ammonium salt compound comprises the following steps of:
m1, uniformly mixing 2.8 to 3.6 parts of 4,4' -dihydroxybenzophenone, 6.4 to 8.2 parts of 1,6-dibromohexane and 75 to 150 parts of acetonitrile, and then adding 10.8 to 14 parts of potassium carbonate serving as a base and 0.65 to 0.84 part of potassium iodide serving as a catalyst; heating and carrying out substitution reaction, removing acetonitrile by reduced pressure distillation after the reaction is finished, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified bromo compound for later use;
m2, taking 3.2 to 4.2 parts of the purified brominated compound, 2.3 to 2.9 parts of decyl dimethyl tertiary amine and 50 to 100 parts of acetonitrile, uniformly mixing, and then adding 9.0 to 11.7 parts of potassium carbonate as an alkali and 0.53 to 0.69 part of potassium iodide as a catalyst; heating and carrying out nucleophilic substitution, removing acetonitrile through reduced pressure distillation after the reaction is finished, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain the quaternary ammonium salt compound;
the preparation method of the sulfonate compound comprises the following steps of:
n1, uniformly mixing 2.8 to 3.6 parts of 4,4' -dihydroxybenzophenone, 6.4 to 8.2 parts of 1,6-dibromohexane and 75 to 150 parts of acetonitrile, and then adding 10.8 to 14 parts of potassium carbonate serving as a base and 0.65 to 0.84 part of potassium iodide serving as a catalyst; heating and carrying out substitution reaction, removing acetonitrile by reduced pressure distillation after the reaction is finished, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified bromo-compound for later use;
n2, taking 3.2 to 4.2 parts of the purified bromo compound, 0.54 to 0.70 part of dimethylamine and 75 to 125 parts of acetone, uniformly mixing, and then adding 9.0 to 11.7 parts of potassium carbonate as alkali and 0.53 to 0.69 part of potassium iodide as a catalyst; heating and carrying out nucleophilic substitution, removing acetone through reduced pressure distillation after the reaction is finished, then adding water and petroleum ether for extraction and liquid separation, collecting an organic phase, and drying to obtain a purified nucleophilic substitution product for later use;
and N3, uniformly mixing 2.8 to 3.6 parts of the purified nucleophilic substitution product, 0.8 to 1.0 part of 2,4-butanesultone and 75 to 150 parts of acetonitrile, heating in an anaerobic closed environment to perform ring-opening addition, removing the acetonitrile through reduced pressure distillation after the reaction is finished, then adding water and petroleum ether to perform extraction and liquid separation, collecting an organic phase, and drying to obtain the sulfonate type compound.
2. The method for preparing a PET protective film according to claim 1, wherein: in the step S1, the power of the corona treatment is 0.5-2kW, the frequency is 10-20kHz, and the linear speed of the film during treatment is 2-6 m/min.
3. The method for preparing a PET protective film according to claim 1, wherein: in the step S2, the curing temperature is 35 to 45 ℃, and the curing time is 12 to 48h.
4. The method for preparing a PET protective film according to claim 1, wherein: the ultraviolet light irradiation treatment in the step S3 has the ultraviolet light wavelength of 320 to 380nm and the radiation illumination of 1.5 to 1.8mW/cm 2 The treatment time is 0.5 to 2min.
5. The method for preparing a PET protective film according to claim 1, wherein: the temperature of the substitution reaction in the step M1 is 65 to 75 ℃, and the reaction time is 3 to 5 hours; the temperature of nucleophilic substitution in the step M2 is 80-95 ℃, and the reaction time is 4-6h.
6. The method for preparing a PET protective film according to claim 1, wherein: the temperature of the substitution reaction in the step N1 is 65 to 75 ℃, and the reaction time is 3 to 5 hours; the temperature of the nucleophilic substitution in the step N2 is 60 to 65 ℃, and the reaction time is 2 to 4 hours; the temperature of the ring-opening addition in the step N3 is 125-140 ℃, and the reaction time is 2-6 h.
7. A PET protection film is characterized in that: prepared by the method of any one of claims 1~6.
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| CN101597196A (en) * | 2003-06-23 | 2009-12-09 | 贝卢斯健康(国际）有限公司 | Improved drug candidate and preparation method thereof |
| CN101185867A (en) * | 2006-11-17 | 2008-05-28 | 天津科技大学 | Gemini quaternary ammonium salt cationic surfactant and preparation method thereof |
| CN105315912A (en) * | 2015-11-26 | 2016-02-10 | 东莞市纳利光学材料有限公司 | Anti-microbial and anti-static complex film and preparation method thereof |
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