CN116814147B - Coating liquid of water-based high-smoothness antistatic coating layer and preparation method thereof - Google Patents
Coating liquid of water-based high-smoothness antistatic coating layer and preparation method thereof Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 73
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000576 coating method Methods 0.000 title claims abstract description 60
- 239000011248 coating agent Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000011247 coating layer Substances 0.000 title claims abstract description 15
- 229920006257 Heat-shrinkable film Polymers 0.000 claims abstract description 31
- 229920000728 polyester Polymers 0.000 claims abstract description 27
- 239000000835 fiber Substances 0.000 claims description 104
- 240000002853 Nelumbo nucifera Species 0.000 claims description 72
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 52
- 229910021389 graphene Inorganic materials 0.000 claims description 51
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 claims description 45
- 239000000843 powder Substances 0.000 claims description 43
- 239000008367 deionised water Substances 0.000 claims description 41
- 229910021641 deionized water Inorganic materials 0.000 claims description 41
- 239000003795 chemical substances by application Substances 0.000 claims description 39
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 35
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 30
- 239000002344 surface layer Substances 0.000 claims description 29
- -1 polysiloxane Polymers 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 24
- 239000003364 biologic glue Substances 0.000 claims description 20
- CMDGQTVYVAKDNA-UHFFFAOYSA-N propane-1,2,3-triol;hydrate Chemical compound O.OCC(O)CO CMDGQTVYVAKDNA-UHFFFAOYSA-N 0.000 claims description 20
- 239000005543 nano-size silicon particle Substances 0.000 claims description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims description 18
- 229920001296 polysiloxane Polymers 0.000 claims description 15
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 14
- 239000012792 core layer Substances 0.000 claims description 14
- 229920000570 polyether Polymers 0.000 claims description 14
- 230000007062 hydrolysis Effects 0.000 claims description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims description 12
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 11
- 239000002216 antistatic agent Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
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- 238000004140 cleaning Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000012948 isocyanate Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
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- 230000000694 effects Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 3
- 239000002985 plastic film Substances 0.000 description 3
- 229920006300 shrink film Polymers 0.000 description 3
- 239000002518 antifoaming agent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 1
- BUZRAOJSFRKWPD-UHFFFAOYSA-N isocyanatosilane Chemical compound [SiH3]N=C=O BUZRAOJSFRKWPD-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
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- 239000004814 polyurethane Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- BKLGNGGEJNHIQT-UHFFFAOYSA-N prop-2-enoic acid;silicon Chemical compound [Si].OC(=O)C=C BKLGNGGEJNHIQT-UHFFFAOYSA-N 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
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- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a coating liquid of a water-based high-smoothness antistatic coating layer and a preparation method thereof, and aims to solve the problems in the prior art, comprehensively improve the smoothness and antistatic property of a polyester heat-shrinkable film, and realize the processing of a film by an online coating process.
Description
Technical Field
The invention belongs to the field of polymer material processing, and particularly relates to a coating liquid for a high-smoothness antistatic coating layer and a preparation method thereof.
Background
Polyester heat-shrinkable films, particularly polyethylene terephthalate-1, 4-cyclohexanedimethanol terephthalate (PETG) heat-shrinkable films prepared from polyethylene terephthalate (PET) as a raw material, are widely used in the field of bottle labels. With the change of the demands of downstream products, the market has put more characteristic demands on the performance of PETG heat-shrinkable films, such as high slip performance, high antistatic performance, and the like. Insufficient slip can affect the speed of the sleeve marks and the accuracy of the sleeve standards. Poor antistatic properties can affect the cutting speed, causing cutting positioning errors during high-speed cutting. Meanwhile, the surface static of the film is easy to cause the missing printing, halation and dyeing during printing, and impurities are easy to adsorb, so that the product quality is influenced. Currently, the functional material is coated on the surface of the film by using online coating, so that the surface performance of the film can be greatly improved on the premise of having very little influence on the processing performance and the thermal stability of the raw materials. Therefore, the smoothness and antistatic property of the PETG heat shrink film can be improved by a coating mode.
Related patent: the coating liquid which is described in a coating process (CN 110760259A) of the aluminum-plastic film and takes polyether modified polysiloxane as a leveling agent, silicon-polyurethane copolymer and silicon-acrylic acid copolymer as main components and organic solvent as a carrier effectively reduces the friction coefficient of the polyamide-aluminum foil-polypropylene film; the antistatic coating and the antistatic ionization film with high adhesion and stability and the preparation method (CN 113604088A) select single-wall carbon nano tubes, double-wall carbon nano tubes, multi-wall carbon nano tubes, graphite and carbon black as antistatic materials, and the coating liquid prepared by taking vinyl polysiloxane, aminosilane, vinyl silane and isocyanato silane as smooth components effectively reduces the surface resistance and the release force of the film. However, both of the coating solutions are non-aqueous coating solutions and are not suitable for the on-line coating process of the PETG heat-shrinkable film.
Disclosure of Invention
In order to solve the problems in the prior art, the method comprehensively improves the smoothness and antistatic property of the polyester heat-shrinkable film, and realizes the processing of the film by using an online coating process.
The invention provides a coating liquid of an aqueous high-smoothness antistatic coating layer, which comprises a slipping agent, an antistatic agent, a leveling agent, a crosslinking agent and deionized water; the antistatic agent is nano graphene modified by lotus fibers.
Further, the slipping agent comprises 15-25 parts of polyether modified polysiloxane and 0.3-0.5 part of nano silicon dioxide in parts by weight, wherein the particle size of the nano silicon dioxide is 80-130 nm; the antistatic agent comprises 0.9-1.5 parts of nano graphene modified by lotus fibers; the leveling agent comprises 5-10 parts of polyvinylpyrrolidone; the crosslinking agent comprises 15-20 parts of blocked aliphatic polyisocyanate.
Further, the preparation method of the nano graphene modified by the lotus fiber comprises the following steps:
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1-10 parts by weight of the lotus stem fiber fine powder, adding 1 part by weight of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture for 1.0 hr to obtain modified lotus stem fiber fine powder;
⑤ And adding 0.1-0.5 part by weight of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr parts by weight to obtain the nano graphene modified by the lotus fiber.
The invention provides a preparation method of the coating liquid, which comprises the following steps:
① Adding 5 parts by weight of glycerol into 50 parts by weight of deionized water, and stirring at room temperature for 0.5 hr to obtain a glycerol-water solution;
② And adding 0.9-1.5 parts by weight of the nano graphene modified by the lotus fibers into the glycerol-water solution, and stirring at 90 ℃ for 1.0 hr parts. Mixing 1.0 hr by using ultrasonic waves to obtain antistatic liquid;
③ 15-25 parts of polyether modified polysiloxane, 0.3-0.5 part of nano silicon dioxide and 5-10 parts of polyvinylpyrrolidone are added into 50 parts of deionized water by weight, and stirred at 60 ℃ for 0.5 hr to obtain a smooth liquid;
④ The antistatic liquid and the slipping liquid are mixed according to parts by weight and stirred at 90 ℃ for 0.5 hr. And (3) after standing to room temperature, adding 15-20 parts of closed aliphatic isocyanate, and continuously stirring for 0.5 hr to obtain the coating liquid of the aqueous high-smoothness antistatic coating layer (deionized water can be used for diluting by 15-20 times as required during use).
The invention also provides a high-smoothness antistatic polyester heat-shrinkable film which is produced by adopting the coating liquid and utilizing an online coating process.
Further, the heat-shrinkable film structurally comprises an upper surface layer, a core layer, a lower surface layer and a coating layer; the upper surface layer comprises 77-83 parts of PETG slices, 15-20 parts of PET slices and 2-3 parts of opening agents in parts by weight; the core layer comprises 80-85 parts of PETG slices and 15-20 parts of PET slices; the lower surface layer comprises 77-83 parts of PETG slices, 13-20 parts of PET slices and 2-5 parts of hydrolysis inhibitor; the coating liquid used for the coating layer is the coating liquid described above.
Further, the intrinsic viscosity of the PETG slice is 0.765-0.795 dl.g -1, the water content is less than or equal to 0.2%, the L value is 54-58, the b value is-1-2, and the opening agent is nano silicon dioxide; the anti-hydrolysis agent is polycarbodiimide powder.
Further, the PET slice has an intrinsic viscosity of 0.630-0.660 dl.g -1, a water content of less than or equal to 0.2%, an L value of 54-58, and a b value of-1-3.
Advantageous effects
① The uniformity of the dispersion of the nano graphene in the coating layer can be improved by adopting the lotus fiber modified nano graphene. The concrete steps are as follows: the lotus fiber belongs to plant fiber, and the adsorption of nano graphene can be increased after the lotus fiber is modified by using a silane coupling agent KH 560. After being coated on a PETG cast sheet, the fiber is transversely oriented after being transversely stretched, so that the nano graphene is driven to be uniformly dispersed, the agglomeration of the nano graphene is reduced, and the powder falling on the surface of a finished PETG film is reduced.
② The lotus fiber is added into the coating layer, so that the penetration of the ink on the surface of the PETG film can be promoted, the printability is improved, and the phenomena of printing lost points and the like caused by the smooth surface of the film and low friction coefficient are reduced.
③ The nano graphene has good electric conduction and heat conduction properties, and in the high-speed reprocessing process of the PETG heat shrink film, generated charges can be quickly leaked, and the surface temperature of the film can be reduced, so that the electrostatic effect is further inhibited, and the influence of thermal deformation on the processing size is reduced.
④ The polyether modified polysiloxane can play roles of an antifoaming agent and a slipping agent, so that no antifoaming agent is required to be added in the coating liquid. Meanwhile, a small amount of nano silicon dioxide is added to convert local surface friction into point friction, so that the slipping performance is improved.
⑤ The hydrolysis resistance agent is added into the lower surface layer, so that the hydrolysis of the water in the coating liquid to the PETG can be reduced, and the mechanical property of the PETG film can be maintained.
⑥ The high-smoothness antistatic polyester heat-shrinkable film has low friction coefficient and high antistatic property.
Drawings
FIG. 1 is a schematic cross-sectional view of a high slip antistatic polyester heat shrink film.
Reference numerals: 1. the composite material comprises an upper surface layer, a core layer, a lower surface layer, a coating layer, an antistatic agent in the coating layer and nano silicon dioxide in the coating layer.
Detailed Description
The invention will now be described in more detail with reference to the following examples, in which parts are by weight.
Example 1
Preparation of conventional polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of opening agent are respectively added into three corresponding extruders of a three-layer casting sheet machine. Casting, stretching and cutting to obtain the conventional polyester heat-shrinkable film.
Example two
1. Preparation of nano graphene modified by lotus fiber
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1 part of the lotus stem fiber fine powder, adding 1 part of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture to obtain modified lotus stem fiber fine powder of 1.0 hr;
⑤ And adding 0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr to obtain the modified nano graphene.
2. Preparing a coating liquid
① 5 Parts of glycerol is added into 50 parts of deionized water, and the mixture is stirred at room temperature for 0.5 hr to obtain a glycerol-water solution.
② 0.5 Part of modified nano graphene is taken and added into the glycerol-water solution, and stirred at 90 ℃ for 1.0 hr. Mixing with ultrasonic wave 1.0 hr to obtain antistatic liquid.
③ 25 Parts of polyether modified polysiloxane, 0.3 part of nano silicon dioxide and 5 parts of polyvinylpyrrolidone are taken and added into 50 parts of deionized water, and the mixture is stirred at 60 ℃ for 0.5 hr to obtain the smooth liquid.
④ The antistatic liquid and the slipping liquid are mixed and stirred at 90 ℃ for 0.5 hr. After standing to room temperature, 15 parts of closed aliphatic isocyanate is added, and stirring is continued for 0.5 hr, so that the aqueous high-smoothness antistatic coating liquid is obtained.
3. Preparation of high-smoothness antistatic polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of hydrolysis resistance agent are respectively added into three corresponding extruders of a three-layer casting machine. The coating solution was diluted 20 times with deionized water and added to an in-line coater. Casting, coating and stretching, and cutting to obtain the high-smoothness antistatic polyester heat-shrinkable film.
Example III
1. Preparation of nano graphene modified by lotus fiber
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1 part of the lotus stem fiber fine powder, adding 1 part of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture to obtain modified lotus stem fiber fine powder of 1.0 hr;
⑤ And adding 0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr to obtain the modified nano graphene.
2. Preparing a coating liquid
① 5 Parts of glycerol is added into 50 parts of deionized water, and the mixture is stirred at room temperature for 0.5 hr to obtain a glycerol-water solution.
② 0.9 Part of modified nano graphene is taken and added into the glycerol-water solution, and stirred at 90 ℃ for 1.0 hr. Mixing with ultrasonic wave 1.0 hr to obtain antistatic liquid.
③ 25 Parts of polyether modified polysiloxane, 0.3 part of nano silicon dioxide and 5 parts of polyvinylpyrrolidone are taken and added into 50 parts of deionized water, and the mixture is stirred at 60 ℃ for 0.5 hr to obtain the smooth liquid.
④ The antistatic liquid and the slipping liquid are mixed and stirred at 90 ℃ for 0.5 hr. After standing to room temperature, 15 parts of closed aliphatic isocyanate is added, and stirring is continued for 0.5 hr, so that the aqueous high-smoothness antistatic coating liquid is obtained.
3. Preparation of high-smoothness antistatic polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of hydrolysis resistance agent are respectively added into three corresponding extruders of a three-layer casting machine. The coating solution was diluted 20 times with deionized water and added to an in-line coater. Casting, coating and stretching, and cutting to obtain the high-smoothness antistatic polyester heat-shrinkable film.
Example IV
1. Preparation of nano graphene modified by lotus fiber
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1 part of the lotus stem fiber fine powder, adding 1 part of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture to obtain modified lotus stem fiber fine powder of 1.0 hr;
⑤ And adding 0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr to obtain the modified nano graphene.
2. Preparing a coating liquid
① 5 Parts of glycerol is added into 50 parts of deionized water, and the mixture is stirred at room temperature for 0.5 hr to obtain a glycerol-water solution.
② 1.5 Parts of modified nano graphene is taken and added into the glycerol-water solution, and stirred at 90 ℃ for 1.0 hr. Mixing with ultrasonic wave 1.0 hr to obtain antistatic liquid.
③ 25 Parts of polyether modified polysiloxane, 0.3 part of nano silicon dioxide and 5 parts of polyvinylpyrrolidone are taken and added into 50 parts of deionized water, and the mixture is stirred at 60 ℃ for 0.5 hr to obtain the smooth liquid.
④ The antistatic liquid and the slipping liquid are mixed and stirred at 90 ℃ for 0.5 hr. After standing to room temperature, 15 parts of closed aliphatic isocyanate is added, and stirring is continued for 0.5 hr, so that the aqueous high-smoothness antistatic coating liquid is obtained.
3. Preparation of high-smoothness antistatic polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of hydrolysis resistance agent are respectively added into three corresponding extruders of a three-layer casting machine. The coating solution was diluted 20 times with deionized water and added to an in-line coater. Casting, coating and stretching, and cutting to obtain the high-smoothness antistatic polyester heat-shrinkable film.
Example five
1. Preparation of nano graphene modified by lotus fiber
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1 part of the lotus stem fiber fine powder, adding 1 part of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture to obtain modified lotus stem fiber fine powder of 1.0 hr;
⑤ And adding 0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr to obtain the modified nano graphene.
2. Preparing a coating liquid
① 5 Parts of glycerol is added into 50 parts of deionized water, and the mixture is stirred at room temperature for 0.5 hr to obtain a glycerol-water solution.
② 2.0 Parts of modified nano graphene is taken and added into the glycerol-water solution, and stirred at 90 ℃ for 1.0 hr. Mixing with ultrasonic wave 1.0 hr to obtain antistatic liquid.
③ 25 Parts of polyether modified polysiloxane, 0.3 part of nano silicon dioxide and 5 parts of polyvinylpyrrolidone are taken and added into 50 parts of deionized water, and the mixture is stirred at 60 ℃ for 0.5 hr to obtain the smooth liquid.
④ The antistatic liquid and the slipping liquid are mixed and stirred at 90 ℃ for 0.5 hr. After standing to room temperature, 15 parts of closed aliphatic isocyanate is added, and stirring is continued for 0.5 hr, so that the aqueous high-smoothness antistatic coating liquid is obtained.
3. Preparation of high-smoothness antistatic polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of hydrolysis resistance agent are respectively added into three corresponding extruders of a three-layer casting machine. The coating solution was diluted 20 times with deionized water and added to an in-line coater. Casting, coating and stretching, and cutting to obtain the high-smoothness antistatic polyester heat-shrinkable film.
Example six
1. Preparation of nano graphene modified by lotus fiber
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1 part of the lotus stem fiber fine powder, adding 1 part of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture to obtain modified lotus stem fiber fine powder of 1.0 hr;
⑤ And adding 0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr to obtain the modified nano graphene.
2. Preparing a coating liquid
① 5 Parts of glycerol is added into 50 parts of deionized water, and the mixture is stirred at room temperature for 0.5 hr to obtain a glycerol-water solution.
② 1.5 Parts of modified nano graphene is taken and added into the glycerol-water solution, and stirred at 90 ℃ for 1.0 hr. Mixing with ultrasonic wave 1.0 hr to obtain antistatic liquid.
③ 10 Parts of polyether modified polysiloxane, 0.3 part of nano silicon dioxide and 5 parts of polyvinylpyrrolidone are taken and added into 50 parts of deionized water, and stirred for 0.5 hr at 60 ℃ to obtain the smooth liquid.
④ The antistatic liquid and the slipping liquid are mixed and stirred at 90 ℃ for 0.5 hr. After standing to room temperature, 15 parts of closed aliphatic isocyanate is added, and stirring is continued for 0.5 hr, so that the aqueous high-smoothness antistatic coating liquid is obtained.
3. Preparation of high-smoothness antistatic polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of hydrolysis resistance agent are respectively added into three corresponding extruders of a three-layer casting machine. The coating solution was diluted 20 times with deionized water and added to an in-line coater. Casting, coating and stretching, and cutting to obtain the high-smoothness antistatic polyester heat-shrinkable film.
Example seven
1. Preparation of nano graphene modified by lotus fiber
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1 part of the lotus stem fiber fine powder, adding 1 part of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture to obtain modified lotus stem fiber fine powder of 1.0 hr;
⑤ And adding 0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr to obtain the modified nano graphene.
2. Preparing a coating liquid
① 5 Parts of glycerol is added into 50 parts of deionized water, and the mixture is stirred at room temperature for 0.5 hr to obtain a glycerol-water solution.
② 1.5 Parts of modified nano graphene is taken and added into the glycerol-water solution, and stirred at 90 ℃ for 1.0 hr. Mixing with ultrasonic wave 1.0 hr to obtain antistatic liquid.
③ 30 Parts of polyether modified polysiloxane, 0.5 part of nano silicon dioxide and 5 parts of polyvinylpyrrolidone are taken and added into 50 parts of deionized water, and stirred for 0.5 hr at 60 ℃ to obtain the smooth liquid.
④ The antistatic liquid and the slipping liquid are mixed and stirred at 90 ℃ for 0.5 hr. After standing to room temperature, 15 parts of closed aliphatic isocyanate is added, and stirring is continued for 0.5 hr, so that the aqueous high-smoothness antistatic coating liquid is obtained.
3. Preparation of high-smoothness antistatic polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of hydrolysis resistance agent are respectively added into three corresponding extruders of a three-layer casting machine. The coating solution was diluted 20 times with deionized water and added to an in-line coater. Casting, coating and stretching, and cutting to obtain the high-smoothness antistatic polyester heat-shrinkable film.
Example eight
1. Preparation of nano graphene modified by lotus fiber
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1 part of the lotus stem fiber fine powder, adding 1 part of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture to obtain modified lotus stem fiber fine powder of 1.0 hr;
⑤ And adding 0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr to obtain the modified nano graphene.
2. Preparing a coating liquid
① 5 Parts of glycerol is added into 50 parts of deionized water, and the mixture is stirred at room temperature for 0.5 hr to obtain a glycerol-water solution.
② 1.5 Parts of modified nano graphene is taken and added into the glycerol-water solution, and stirred at 90 ℃ for 1.0 hr. Mixing with ultrasonic wave 1.0 hr to obtain antistatic liquid.
③ 25 Parts of polyether modified polysiloxane, 0.5 part of nano silicon dioxide and 5 parts of polyvinylpyrrolidone are taken and added into 50 parts of deionized water, and the mixture is stirred at 60 ℃ for 0.5 hr to obtain the smooth liquid.
④ The antistatic liquid and the slipping liquid are mixed and stirred at 90 ℃ for 0.5 hr. After standing to room temperature, 15 parts of closed aliphatic isocyanate is added, and stirring is continued for 0.5 hr, so that the aqueous high-smoothness antistatic coating liquid is obtained.
3. Preparation of high-smoothness antistatic polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of hydrolysis resistance agent are respectively added into three corresponding extruders of a three-layer casting machine. The coating solution was diluted 20 times with deionized water and added to an in-line coater. Casting, coating and stretching, and cutting to obtain the high-smoothness antistatic polyester heat-shrinkable film.
Example nine
1. Preparation of nano graphene modified by lotus fiber
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 hr, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 hr to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1 part of the lotus stem fiber fine powder, adding 1 part of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture to obtain modified lotus stem fiber fine powder of 1.0 hr;
⑤ And adding 0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 hr to obtain the modified nano graphene.
2. Preparing a coating liquid
① 5 Parts of glycerol is added into 50 parts of deionized water, and the mixture is stirred at room temperature for 0.5 hr to obtain a glycerol-water solution.
② 1.5 Parts of modified nano graphene is taken and added into the glycerol-water solution, and stirred at 90 ℃ for 1.0 hr. Mixing with ultrasonic wave 1.0 hr to obtain antistatic liquid.
③ 25 Parts of polyether modified polysiloxane, 0.6 part of nano silicon dioxide and 5 parts of polyvinylpyrrolidone are taken and added into 50 parts of deionized water, and the mixture is stirred at 60 ℃ for 0.5 hr to obtain the smooth liquid.
④ The antistatic liquid and the slipping liquid are mixed and stirred at 90 ℃ for 0.5 hr. After standing to room temperature, 15 parts of closed aliphatic isocyanate is added, and stirring is continued for 0.5 hr, so that the aqueous high-smoothness antistatic coating liquid is obtained.
3. Preparation of high-smoothness antistatic polyester heat-shrinkable film
① The temperature of each zone of a heating zone of the three-layer casting sheet casting machine is increased from 200 ℃ to 240 ℃ from a blanking port to a die, and the temperature of the die head is 240-245 ℃; the blanking speed of the auxiliary extruder and the main extruder is 1:1.5-2.0, and the metering pump speed of the auxiliary extruder and the main extruder is 1:2.0-2.5; the transverse drawing temperature is 85-90 ℃, and the shaping temperature is 75-80 ℃; uniaxially stretched and the transverse stretching ratio was 4.0.
② 77 Parts of PETG slice of the upper surface layer, 20 parts of PET slice, 3 parts of opening agent, 80 parts of PETG slice of the core layer, 20 parts of PET slice, 77 parts of PETG slice of the lower surface layer, 20 parts of PET slice and 3 parts of hydrolysis resistance agent are respectively added into three corresponding extruders of a three-layer casting machine. The coating solution was diluted 20 times with deionized water and added to an in-line coater. Casting, coating and stretching, and cutting to obtain the high-smoothness antistatic polyester heat-shrinkable film.
Example effect comparison:
1. antistatic properties:
① The parts with lower thickness errors on the heat-shrinkable films prepared in the above examples were selected, and 100X 100 mm samples were cut out, 6 sheets of each film being cut out.
② And (3) selecting one cut film, adhering the cut film by using a transparent adhesive tape, and hanging the cut film vertically.
③ And taking one cut film, spreading the film on a glass tabletop, and uniformly and rapidly rubbing the film for 15 times by using a towel made of wool.
④ The rubbed film was immediately attached to the hanging film.
⑤ And starting timing by taking the attached time as a node, and stopping timing by taking the falling time as an end point. And calculating the starting and stopping time difference as T (unit: min), measuring each film three times, calculating an average value T of T, and judging the antistatic performance by taking T as a reference, wherein the smaller the T is, the better the antistatic performance of the film is.
Note that: the test environment temperature was 25 ℃ and the relative humidity was 60%, and rubber gloves were worn during the test.
Antistatic properties comparison results
From the antistatic property comparison result, it can be seen that the antistatic property of the obtained film is improved as the content of the antistatic agent is increased. When the content of the antistatic agent is too low, the antistatic effect is not remarkable. When the content of the antistatic agent is too high, the optical performance of the film can be affected due to the poor light transmittance of the nano graphene. The change in the amount of the slipping agent also causes a change in antistatic properties, but the effect is not great.
2. Friction properties:
the examples were tested for coefficient of friction mu s/μk using a coefficient of friction meter according to national standard GBT10006-2021 determination of coefficient of friction for plastic films and sheets, the results are given in the following table:
Coefficient of friction comparison results
From the comparison of the friction coefficients, it can be seen that the friction coefficient decreases with increasing amount of the slipping agent, but the slipping effect is not obvious when the amount of the slipping agent is too low. On the other hand, when the amount of the slipping agent is too high, the film surface coating substance migrates in spite of the low friction coefficient. In addition, an increase in the content of the modified nanographene also causes a slight decrease in the friction coefficient.
Claims (3)
1. The high-smoothness antistatic polyester heat-shrinkable film is characterized by comprising an upper surface layer, a core layer, a lower surface layer and a coating layer; the upper surface layer comprises 77-83 parts of PETG slices, 15-20 parts of PET slices and 2-3 parts of opening agents in parts by weight; the core layer comprises 80-85 parts of PETG slices and 15-20 parts of PET slices; the lower surface layer comprises 77-83 parts of PETG slices, 13-20 parts of PET slices and 2-5 parts of hydrolysis inhibitor; the coating liquid adopted by each coating layer is as follows: comprises a slipping agent, an antistatic agent, a leveling agent, a cross-linking agent and deionized water; the antistatic agent is nano graphene modified by lotus fibers; the slipping agent comprises 15-25 parts of polyether modified polysiloxane and 0.3-0.5 part of nano silicon dioxide by weight, wherein the particle size of the nano silicon dioxide is 80-130 nm; the antistatic agent comprises 0.9-1.5 parts of nano graphene modified by lotus fibers; the leveling agent comprises 5-10 parts of polyvinylpyrrolidone; the cross-linking agent comprises 15-20 parts of blocked aliphatic polyisocyanate; the preparation method of the nano graphene modified by the lotus fiber comprises the following steps:
① Taking a proper amount of lotus stems, extracting fiber filaments, and naturally air-drying to remove water;
② Soaking the obtained fiber filaments in an alcohol solution for 2.0 h, taking out, cleaning with deionized water, and removing the biological glue on the surfaces of the fiber filaments;
③ Placing the fiber filaments from which the biological glue is removed into an oven, drying at 105 ℃ for 2.0 h to remove water, and grinding into lotus stem fiber fine powder;
④ Taking 1-10 parts by weight of the lotus stem fiber fine powder, adding 1 part by weight of a silane coupling agent KH560, uniformly stirring, and performing ultrasonic treatment on the mixture for 1.0 h to obtain modified lotus stem fiber fine powder;
⑤ Adding 0.1-0.5 part of nano graphene into the modified lotus fiber fine powder, uniformly stirring, and treating with ultrasonic waves for 2.0 h parts to obtain the nano graphene modified by the lotus fiber;
The preparation method of the coating liquid comprises the following steps:
① Adding 5 parts by weight of glycerol into 50 parts by weight of deionized water, and stirring at room temperature for 0.5 h to obtain a glycerol-water solution;
② Adding 0.9-1.5 parts by weight of the nano graphene modified by lotus fibers into the glycerol-water solution, stirring at 90 ℃ for 1.0 h parts, and mixing with ultrasonic waves for 1.0 h parts to obtain antistatic liquid;
③ 15-25 parts of polyether modified polysiloxane, 0.3-0.5 part of nano silicon dioxide and 5-10 parts of polyvinylpyrrolidone are added into 50 parts of deionized water by weight, and stirred at 60 ℃ for 0.5 h to obtain a smooth liquid;
④ And mixing the antistatic liquid and the slipping liquid in parts by weight, stirring at 90 ℃ for 0.5 h, standing to room temperature, adding 15-20 parts of closed aliphatic isocyanate, and continuously stirring for 0.5-h to obtain the coating liquid.
2. The high-smoothness antistatic polyester heat-shrinkable film according to claim 1, wherein the intrinsic viscosity of the PETG slices is 0.765-0.795 dl-g -1, the water content is less than or equal to 0.2%, the L value is 54-58, the b value is-1-2, and the opening agent is nano silicon dioxide; the anti-hydrolysis agent is polycarbodiimide powder.
3. The high-smoothness antistatic polyester heat-shrinkable film according to claim 2, wherein the intrinsic viscosity of the PET chips is 0.630-0.660 dl-g -1, the water content is less than or equal to 0.2%, the L value is 54-58, and the b value is-1-3.
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