CN113953168A - Surface micro-crosslinking process suitable for preparing deep texture film - Google Patents
Surface micro-crosslinking process suitable for preparing deep texture film Download PDFInfo
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- CN113953168A CN113953168A CN202111222368.9A CN202111222368A CN113953168A CN 113953168 A CN113953168 A CN 113953168A CN 202111222368 A CN202111222368 A CN 202111222368A CN 113953168 A CN113953168 A CN 113953168A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
- B05D5/061—Special surface effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
- B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
- B05D3/065—After-treatment
- B05D3/067—Curing or cross-linking the coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
- B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2201/00—Polymeric substrate or laminate
- B05D2201/02—Polymeric substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2502/00—Acrylic polymers
Abstract
The invention discloses a surface micro-crosslinking process suitable for preparing a deep texture film, which comprises a roller die with deep textures on the outer surface, wherein the depth of the deep textures on the roller die is 10-20 mu m, the distance between adjacent deep textures is 5 mu m, and the surface micro-crosslinking process comprises the following steps: A. forming a UV sol layer on the PET base film; B. forming a micro-crosslinked surface on the UV sol layer; C. pressing the UV sol layer and a roller mold; D. and (5) carrying out photocuring and rolling by adopting a UV lamp. The invention adopts a texture transfer printing process, namely, a deep texture structure, namely a microstructure on the surface of the roller die is transferred to the surface of the PET base film and firmly combined to form uniform deep texture. The invention can transfer high-precision micro-structure and deep texture with the depth of 10-20 μm. According to the invention, micro-crosslinking and UV curing are organically combined, so that the step-by-step effective control of surface micro-crosslinking and integral crosslinking curing of the UV resin is realized.
Description
Technical Field
The invention relates to the technical field of preparation of UV films, in particular to a surface micro-crosslinking process suitable for preparing a deep texture film.
Background
The UV film is a film having a special texture prepared by UV transfer printing on the surface of a substrate, and the substrate is generally made of a transparent material, such as PET, PC, PMMA, or the like.
The texture pattern and fineness of the UV film are determined by the roller mold for UV transfer printing, and the finer the roller mold is, the finer the texture film is, so the key point of the technology lies in the texture mold and the transfer printing process. Currently, the most popular textured film is a drawn film. There are also many patents published now that report the basic technical content of the UV transfer process.
For example, patent No. CN102520465A, "a method for preparing an optical film" specifically discloses the following preparation steps: dripping solvent-free photosensitive resin coating on the surface of a transparent base material, and rolling by using a guide roller, wherein the surface of the guide roller is provided with micro-structure cavities, and the micro-structure cavities can be filled with the photosensitive resin coating in the rolling process. And (3) curing the solvent-free photosensitive resin coating after rolling by using an ultraviolet curing device while rolling so as to firmly adhere to the surface of the resin film. The method has the advantages of simple process, low manufacturing cost, energy conservation and environmental protection, and can be widely applied to the production of optical films such as optical films and electronic product decorative films.
In combination with other prior art patents, the applicant has concluded from practical experience that the existing UV transfer process still has the following problems:
1. during UV transfer printing, UV resin is dripped on the surface of a base material or dripped on the interface between a roller die and the base material, flowing UV resin can fill all texture structure grooves of the roller die, but the UV resin can remain in the texture of the roller die, namely the problem of adhesive residue is solved, so that the texture transfer printing is incomplete, pits exist on the surface of a UV film finally, and the surface flatness and the integrity of the texture are influenced;
2. the UV transfer printing process has high requirements on the roller die, the surface of the roller die is very smooth, and accurate transfer printing can be realized, but the higher the surface processing precision is, the higher the cost is, the more obvious the transfer printing is;
3. the existing UV transfer printing technology can not meet the transfer printing requirement of narrow (width 5um) and deep texture (depth is more than 10 mu m).
Based on the present situation as described above, the UV transfer process is used for improvement.
Disclosure of Invention
Aiming at the defects of incomplete texture transfer printing, residual UV resin in the texture of a roller die, high preparation cost of a high-precision die and the like in the existing UV transfer printing process, the invention provides a novel surface micro-crosslinking process suitable for preparing a deep texture film.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a surface micro-crosslinking process suitable for preparing a deep texture film, the surface micro-crosslinking process comprising a roller mold having a deep texture on an outer surface, the depth of the deep texture on the roller mold being 10 μm to 20 μm, and a distance between adjacent deep textures being 5 μm, the surface micro-crosslinking process comprising the steps of:
A. coating a layer of UV resin on a PET (polyethylene terephthalate) base film with the thickness of 30-50 mu m to form a UV sol layer, wherein the thickness of the UV sol layer is 15-30 mu m;
B. carrying out radiation curing on the UV sol layer at normal temperature and normal pressure to enable the upper surface of the UV sol layer to form a micro-crosslinking surface, wherein the thickness of the micro-crosslinking surface is 0.05-0.1 time of that of the UV sol layer, and the micro-crosslinking degree of the micro-crosslinking surface is controlled to be 1-8%;
C. pressing the UV sol layer and a roller die to ensure that the micro-crosslinked surface is completely attached to the deep texture, and filling the deep texture on the roller die with UV resin under the action of pressure;
D. and C, after the pressing in the step C, carrying out photocuring by adopting a UV lamp, curing for 1-2s under ultraviolet waves, and rolling to obtain the deep texture film.
The invention adopts a texture transfer printing process, namely, a deep texture structure, namely a microstructure on the surface of the roller die is transferred to the surface of the PET base film and firmly combined to form uniform deep texture. The invention can transfer high-precision micro-structure and deep texture with the depth of 10-20 μm.
The step A is mainly used for accurately controlling the coating thickness of the UV sol layer. And step B is mainly used for forming a micro-crosslinking surface with controllable thickness and micro-crosslinking degree on the surface of the UV sol layer. And step C is mainly used for transferring the deep texture on the roller die to the PET base film. And step D is mainly to completely crosslink and solidify the UV sol layer still having certain fluidity through a UV lamp to form the final deep texture film.
The UV resin adopted by the invention can realize micro-crosslinking under a certain condition, and the micro-crosslinking degree is controllable. The surface micro-crosslinking of the invention means that the upper surface of the UV resin coated on the PET base film is enabled to realize a micro-crosslinking state by means of radiation curing, the thickness of the micro-crosslinking surface is only 0.05-0.1 times of the coating thickness, the main purpose is to make the surface of a film layer of the UV sol layer lose activity and reduce the adhesion to the surface of a roller die, thereby avoiding the filling of some tiny cavities in deep texture by the UV resin, thoroughly improving the defect of poor demoulding and completely overcoming the defects of the prior art.
After the micro-crosslinking is finished, the micro-crosslinking surface still has certain flow deformation capacity, and the UV sol layer below the micro-crosslinking surface still has larger fluidity, so that when a PET base film is pressed with a roller mold, a deep texture structure on the surface of the roller mold can be completely pressed into the UV sol layer, uncured UV resin can be deformed into the shape of a roller surface microstructure under the action of pressure, the shape is kept to be irradiated and cured by a UV lamp, and the deep texture is copied and transferred, wherein the wave section of the UV lamp is generally selected from the most extensive 280-plus 365nm ultraviolet waves, and better curing is realized.
Because the fluidity of the micro-crosslinked surface and the UV sol layer can completely duplicate the deep texture structure on the surface of the roller die, the integral crosslinking and solidification can still be realized under the irradiation of a UV lamp, the invention finally transfers the deep texture structure to the surface of the PET base film, and the transfer printing effect is very accurate without the defect of residual glue. According to the invention, micro-crosslinking and UV curing are organically combined, so that the step-by-step effective control of surface micro-crosslinking and integral crosslinking curing of the UV resin is realized.
Preferably, the surface micro-crosslinking process for preparing the deep texture film comprises the following components in parts by weight:
the preparation method comprises the following steps: firstly, adding all epoxy acrylate resin and polyester acrylate resin into a reaction container, uniformly stirring, then mixing all trifunctional monomer, monofunctional monomer, light stabilizer, antioxidant, photoinitiator and coupling agent, adding into the reaction container, controlling the temperature of the reaction container to be kept at 25-30 ℃, and obtaining UV resin after the reaction is finished, wherein the viscosity of the UV resin is 300-500 cps.
The invention selects the two resins of epoxy acrylate resin and polyester acrylate resin as main resin, and the two resins are most widely applied in the UV transfer printing process, so that the invention has universal applicability.
The trifunctional monomer and the monofunctional monomer are combined for use, so that the effects of crosslinking aid and viscosity adjustment are achieved, and the UV resin can be fully reacted and cured. The light stabilizer can enhance the subsequent ultraviolet aging performance of the product. The antioxidant can enhance the aging test performance of the product, such as high temperature and high humidity, cold and hot circulation and the like. The photoinitiator can generate free radicals under ultraviolet irradiation to initiate the polymerization reaction of the crosslinking monomer. The coupling agent can increase the bonding force between the resin and the substrate.
Preferably, the surface micro-crosslinking process for preparing the deep texture film is characterized in that the micro-crosslinking degree of the micro-crosslinked surface is measured according to the following method:
s1: b, after radiation curing, forming a UV sol layer and a micro-crosslinked surface composite structure on the PET base film, cutting a sample with a three-layer film structure of the PET base film, the UV sol layer and the micro-crosslinked surface from the PET base film, weighing the sample, recording the weight W1, then putting the sample into a stainless steel mesh bag, and recording the total weight W2 of the sample and the stainless steel mesh bag;
s2: then taking the stainless steel wire to seal the stainless steel mesh bag, wherein the total weight of the stainless steel mesh bag is recorded as W3;
s3: carrying out xylene reflux extraction on the sealed stainless steel mesh bag, drying, and weighing the stainless steel mesh bag, wherein the weight is recorded as W4;
s4: the density of the PET base film is ρ, the thickness of the PET base film is b, the weight M of the PET base film per square meter of the sample is ρ × b, and if the coating amount per square meter of the UV resin is V g, the degree of micro-crosslinking is
The invention determines the micro-crosslinking degree according to the mode, thereby realizing the artificial regulation of the micro-crosslinking degree and the thickness of the micro-crosslinking surface by controlling the micro-crosslinking process and the irradiation intensity. In addition, the invention can indirectly adjust the wettability and the adhesiveness between the UV resin filled in the deep texture and the surface of the deep texture by regulating the micro-crosslinking degree, is beneficial to smoothly and completely stripping the completely cured deep texture film from the surface of the roller die, thereby realizing the control of the residual glue point of the deep texture film, finding out the optimized process path and solving the problems of complicated preparation of the UV transfer printing process and easy residual glue of a rough texture structure in the prior art.
Preferably, the surface micro-crosslinking process for preparing the deep texture film has a coating weight V of 10-30g per square meter.
The invention sets the coating weight, can obtain the optimum UV sol layer thickness and is convenient to operate.
Preferably, in the surface micro-crosslinking process for preparing the deep texture film, the radiation curing in the step B is one of EB radiation, infrared radiation and ultraviolet radiation.
EB radiation, infrared radiation and ultraviolet radiation are all radiation curing means which are mature in application and are suitable for industrial mass production and manufacture.
Preferably, the EB radiation is irradiated by an electron beam with 200-300MeV, the radiation atmosphere is a 95% nitrogen environment, and the radiation time is 0.5-1S.
By adopting the EB radiation process with the parameters, the invention can better obtain the effect of radiation curing and effectively control the micro-crosslinking degree.
Preferably, the surface micro-crosslinking process suitable for preparing the deep texture film is adopted, and the ultraviolet radiation is irradiation by using UVC short-wave ultraviolet rays, the wavelength range is 280-365nm, and the irradiation time is 0.5-1 s.
The invention adopts the ultraviolet radiation with the parameters, can better obtain the radiation curing effect, thereby effectively controlling the micro-crosslinking degree.
Preferably, the surface micro-crosslinking process is suitable for preparing a deep texture film, the light stabilizer is a hindered amine light stabilizer, the antioxidant is triethylene glycol ether-bis (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, the photoinitiator comprises TPO and 184, and the coupling agent is one or a mixture of vinyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane.
The combination of the light stabilizer, the antioxidant and the coupling agent is adopted, so that the optimal radiation curing and UV curing effects can be obtained, the viscosity of the prepared UV resin can be directly influenced, and the final UV sol layer can be fully crosslinked and cured.
Preferably, the surface micro-crosslinking process suitable for preparing the deep texture film is one or two of trimethylolpropane triacrylate, pentaerythritol triacrylate and propoxylated glycerol triacrylate, and the monofunctional monomer is one of 2-phenoxyethyl acrylate, cetyl acrylate and isodecyl acrylate.
The invention combines the trifunctional monomer and the monofunctional monomer for use, and better plays roles in crosslinking assistant and viscosity adjustment, so that the UV resin can be fully reacted and cured.
Preferably, the surface micro-crosslinking process suitable for preparing the deep texture film is characterized in that the deep texture on the roller die is in a deep V shape, the diameter of the roller die is 250-270 mm, the front side and the rear side of the roller die are provided with supporting rubber rollers, and the diameter of the supporting rubber rollers is 180-220 mm.
Supporting rubber rollers are arranged on the front side and the rear side of the roller mold in the horizontal direction, the opening and closing of the roller and the rubber rollers can be controlled through a hydraulic device, and the pressure between the rubber rollers and the roller can also be controlled, so that the smooth proceeding of a transfer printing process is ensured. The diameter of the roller die and the diameters of the front and rear supporting rubber rollers are within the parameter range, so that the UV transfer printing process can be better optimized.
Compared with the prior art, the invention has the following prominent substantive characteristics and remarkable progress:
1) the invention realizes the transfer printing preparation of the UV film with deep texture (the depth is more than 10 mu m), and is particularly suitable for the mass preparation of the wire drawing film;
2) the invention effectively avoids the problem of adhesive residue in the UV transfer printing production process, and the UV film has smoother appearance and no flaw;
3) according to the invention, by means of micro-crosslinking, the curing time can be reduced, the demolding effect can be improved, and the thickness of deep texture can be effectively controlled;
4) the invention has stronger adaptability to the roller die, can well finish the transfer printing and copying of deep textures no matter the roller die carved by a diamond knife, the roller die carved by laser or the wire drawing roller die obtained by grinding by a grinding wheel, and the produced texture film has good appearance and smooth and fine texture, so the invention can realize the mass production of the deep texture film and is particularly suitable for producing the touch wire drawing texture for decorative films and the Fresnel lens texture used by intelligent sensing equipment.
5) The process has wide applicability, including but not limited to transfer printing of roller molds, and transfer printing of flat plate molds.
Drawings
FIG. 1 is a first schematic structural diagram of a deep texture film of the present invention;
FIG. 2 is a second schematic structural diagram of the deep texture film of the present invention.
Detailed Description
The invention will be described in further detail with reference to the following figures 1-2 and the detailed description, which are not intended to limit the invention:
example 1
A surface micro-crosslinking process suitable for preparing a deep texture film, the surface micro-crosslinking process comprising a roller mold 4 having a deep texture on an outer surface thereof, the depth of the deep texture on the roller mold 4 being 10 μm, and a distance between adjacent deep textures being 5 μm, the surface micro-crosslinking process comprising the steps of:
A. coating a layer of UV resin on a PET (polyethylene terephthalate) base film 3 with the thickness of 30 microns to form a UV sol layer 2, wherein the thickness of the UV sol layer 2 is 15 microns;
B. carrying out radiation curing on the UV sol layer 2 at normal temperature and normal pressure to form a micro-crosslinking surface 1 on the upper surface of the UV sol layer 2, wherein the thickness of the micro-crosslinking surface 1 is 0.05 times of that of the UV sol layer 2, and the micro-crosslinking degree of the micro-crosslinking surface 1 is controlled to be 1%;
C. pressing the UV sol layer 2 and a roller mold 4 to ensure that the micro-crosslinked surface 1 is completely attached to the deep texture, and filling the deep texture on the roller mold 4 with UV resin under the action of pressure;
D. and C, after the pressing in the step C, carrying out photocuring by adopting a UV lamp, curing for 1s under ultraviolet waves, and rolling to obtain the deep texture film.
Preferably, the UV resin comprises the following components in percentage by weight:
the preparation method comprises the following steps: firstly, adding all epoxy acrylate resin and polyester acrylate resin into a reaction container, uniformly stirring, then mixing all trifunctional monomer, monofunctional monomer, light stabilizer, antioxidant, photoinitiator and coupling agent, adding into the reaction container together, controlling the temperature of the reaction container to be kept at 25 ℃, and obtaining UV resin after the reaction is finished, wherein the viscosity of the UV resin is 300 cps.
Preferably, the degree of micro-crosslinking of the micro-crosslinked surface 1 is measured as follows:
s1: b, after radiation curing, forming a composite structure of a UV sol layer 2 and a micro-crosslinked surface 1 on the PET base film 3, cutting a sample with a three-layer film structure of the PET base film 3, the UV sol layer 2 and the micro-crosslinked surface 1 from the composite structure, weighing the sample, recording the weight W1, then putting the sample into a stainless steel mesh bag, and recording the total weight W2 of the sample and the stainless steel mesh bag;
s2: then taking the stainless steel wire to seal the stainless steel mesh bag, wherein the total weight of the stainless steel mesh bag is recorded as W3;
s3: carrying out xylene reflux extraction on the sealed stainless steel mesh bag, drying, and weighing the stainless steel mesh bag, wherein the weight is recorded as W4;
s4: when the density of the PET base film 3 is ρ and the thickness of the PET base film 3 is b, the weight M of the PET base film 3 per square meter of the sample is ρ × b, and when the coating amount per square meter of the UV resin is V g, the micro-crosslinking degree is V
Preferably, the coating weight V per square meter is 10 g.
Preferably, the radiation curing in step B is one of EB radiation, infrared radiation, ultraviolet radiation.
Preferably, the EB radiation is irradiation with an electron beam having 200MeV in a 95% nitrogen atmosphere for 0.5S.
Preferably, the ultraviolet radiation is irradiation with UVC short-wave ultraviolet rays, the wavelength range is 280-365nm, and the irradiation time is 0.5 s.
Preferably, the light stabilizer is a hindered amine light stabilizer, the antioxidant is triethylene glycol ether-bis (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, the photoinitiator comprises TPO and 184, and the coupling agent is one or a mixture of vinyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane.
Preferably, the trifunctional monomer is one or two of trimethylolpropane triacrylate, pentaerythritol triacrylate and propoxylated glycerol triacrylate, and the monofunctional monomer is one of 2-phenoxyethyl acrylate, cetyl acrylate and isodecyl acrylate.
Preferably, the deep texture on the roller die 4 is in a deep V shape, the diameter of the roller die 4 is 250mm, the front side and the rear side of the roller die 4 are provided with supporting rubber rollers, and the diameter of the supporting rubber rollers is 180 mm.
Example 2
A surface micro-crosslinking process suitable for preparing a deep texture film, the surface micro-crosslinking process comprising a roller mold 4 having a deep texture on an outer surface thereof, the depth of the deep texture on the roller mold 4 being 20 μm, and a distance between adjacent deep textures being 5 μm, the surface micro-crosslinking process comprising the steps of:
A. coating a layer of UV resin on a PET (polyethylene terephthalate) base film 3 with the thickness of 50 microns to form a UV sol layer 2, wherein the thickness of the UV sol layer 2 is 30 microns;
B. carrying out radiation curing on the UV sol layer 2 at normal temperature and normal pressure to form a micro-crosslinking surface 1 on the upper surface of the UV sol layer 2, wherein the thickness of the micro-crosslinking surface 1 is 0.1 time of that of the UV sol layer 2, and the micro-crosslinking degree of the micro-crosslinking surface 1 is controlled to be 8%;
C. pressing the UV sol layer 2 and a roller mold 4 to ensure that the micro-crosslinked surface 1 is completely attached to the deep texture, and filling the deep texture on the roller mold 4 with UV resin under the action of pressure;
D. and C, after the pressing in the step C, carrying out photocuring by adopting a UV lamp, curing for 2s under ultraviolet waves, and rolling to obtain the deep texture film.
Preferably, the UV resin comprises the following components in percentage by weight:
the preparation method comprises the following steps: firstly, adding all epoxy acrylate resin and polyester acrylate resin into a reaction container, uniformly stirring, then mixing all trifunctional monomer, monofunctional monomer, light stabilizer, antioxidant, photoinitiator and coupling agent, adding into the reaction container, controlling the temperature of the reaction container to be kept at 30 ℃, and obtaining UV resin after the reaction is finished, wherein the viscosity of the UV resin is 500 cps.
Preferably, the degree of micro-crosslinking of the micro-crosslinked surface 1 is measured as follows:
s1: b, after radiation curing, forming a composite structure of a UV sol layer 2 and a micro-crosslinked surface 1 on the PET base film 3, cutting a sample with a three-layer film structure of the PET base film 3, the UV sol layer 2 and the micro-crosslinked surface 1 from the composite structure, weighing the sample, recording the weight W1, then putting the sample into a stainless steel mesh bag, and recording the total weight W2 of the sample and the stainless steel mesh bag;
s2: then taking the stainless steel wire to seal the stainless steel mesh bag, wherein the total weight of the stainless steel mesh bag is recorded as W3;
s3: carrying out xylene reflux extraction on the sealed stainless steel mesh bag, drying, and weighing the stainless steel mesh bag, wherein the weight is recorded as W4;
s4: when the density of the PET base film 3 is ρ and the thickness of the PET base film 3 is b, the weight M of the PET base film 3 per square meter of the sample is ρ × b, and when the coating amount per square meter of the UV resin is V g, the micro-crosslinking degree is V
Preferably, the coating weight V per square meter is 30 g.
Preferably, the radiation curing in step B is ultraviolet radiation.
Preferably, the ultraviolet radiation is irradiation with UVC short-wave ultraviolet rays, the wavelength range is 280-365nm, and the irradiation time is 1 s.
Preferably, the light stabilizer is a hindered amine light stabilizer, the antioxidant is triethylene glycol ether-bis (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, the photoinitiator comprises TPO and 184, and the coupling agent is one or a mixture of vinyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane.
Preferably, the trifunctional monomer is one or two of trimethylolpropane triacrylate, pentaerythritol triacrylate and propoxylated glycerol triacrylate, and the monofunctional monomer is one of 2-phenoxyethyl acrylate, cetyl acrylate and isodecyl acrylate.
Preferably, the deep texture on the roller die 4 is deep V-shaped, the diameter of the roller die 4 is 270mm, the front side and the rear side of the roller die 4 are provided with supporting rubber rollers, and the diameter of the supporting rubber rollers is 220 mm.
Example 3
Preferably, the radiation curing in step B is EB radiation.
Preferably, the EB radiation is irradiation with an electron beam having 300MeV in a nitrogen atmosphere of 95% for a radiation time of 1S.
The other embodiments in this example are the same as example 2.
Example 4
A surface micro-crosslinking process suitable for preparing a deep texture film, the surface micro-crosslinking process comprising a roller mold 4 having a deep texture on an outer surface thereof, the depth of the deep texture on the roller mold 4 being 15 μm, and a distance between adjacent deep textures being 5 μm, the surface micro-crosslinking process comprising the steps of:
A. coating a layer of UV resin on a PET (polyethylene terephthalate) base film 3 with the thickness of 40 mu m to form a UV sol layer 2, wherein the thickness of the UV sol layer 2 is 20 mu m;
B. carrying out radiation curing on the UV sol layer 2 at normal temperature and normal pressure to form a micro-crosslinking surface 1 on the upper surface of the UV sol layer 2, wherein the thickness of the micro-crosslinking surface 1 is 0.08 times of that of the UV sol layer 2, and the micro-crosslinking degree of the micro-crosslinking surface 1 is controlled to be 4%;
C. pressing the UV sol layer 2 and a roller mold 4 to ensure that the micro-crosslinked surface 1 is completely attached to the deep texture, and filling the deep texture on the roller mold 4 with UV resin under the action of pressure;
D. and C, after the pressing in the step C, carrying out photocuring by adopting a UV lamp, curing for 1.5s under ultraviolet waves, and rolling to obtain the deep texture film.
Preferably, the UV resin comprises the following components in percentage by weight:
the preparation method comprises the following steps: firstly, adding all epoxy acrylate resin and polyester acrylate resin into a reaction container, uniformly stirring, then mixing all trifunctional monomer, monofunctional monomer, light stabilizer, antioxidant, photoinitiator and coupling agent, adding into the reaction container, controlling the temperature of the reaction container to be kept at 28 ℃, and obtaining UV resin after the reaction is finished, wherein the viscosity of the UV resin is 400 cps.
Preferably, the degree of micro-crosslinking of the micro-crosslinked surface 1 is measured as follows:
s1: b, after radiation curing, forming a composite structure of a UV sol layer 2 and a micro-crosslinked surface 1 on the PET base film 3, cutting a sample with a three-layer film structure of the PET base film 3, the UV sol layer 2 and the micro-crosslinked surface 1 from the composite structure, weighing the sample, recording the weight W1, then putting the sample into a stainless steel mesh bag, and recording the total weight W2 of the sample and the stainless steel mesh bag;
s2: then taking the stainless steel wire to seal the stainless steel mesh bag, wherein the total weight of the stainless steel mesh bag is recorded as W3;
s3: carrying out xylene reflux extraction on the sealed stainless steel mesh bag, drying, and weighing the stainless steel mesh bag, wherein the weight is recorded as W4;
s4: when the density of the PET base film 3 is ρ and the thickness of the PET base film 3 is b, the weight M of the PET base film 3 per square meter of the sample is ρ × b, and when the coating amount per square meter of the UV resin is V g, the micro-crosslinking degree is V
Preferably, the coating weight V per square meter is 20 g.
Preferably, the radiation curing in step B is one of EB radiation, infrared radiation, ultraviolet radiation.
Preferably, the EB radiation is performed by using an electron beam with 250MeV, the radiation atmosphere is a nitrogen environment with 95 percent, and the radiation time is 0.8S.
Preferably, the ultraviolet radiation is irradiation with UVC short-wave ultraviolet rays, the wavelength range is 280-365nm, and the irradiation time is 0.8 s.
Preferably, the light stabilizer is a hindered amine light stabilizer, the antioxidant is triethylene glycol ether-bis (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, the photoinitiator comprises TPO and 184, and the coupling agent is one or a mixture of vinyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane.
Preferably, the trifunctional monomer is one or two of trimethylolpropane triacrylate, pentaerythritol triacrylate and propoxylated glycerol triacrylate, and the monofunctional monomer is one of 2-phenoxyethyl acrylate, cetyl acrylate and isodecyl acrylate.
Preferably, the deep texture on the roller die 4 is in a deep V shape, the diameter of the roller die 4 is 260mm, the front side and the rear side of the roller die 4 are provided with supporting rubber rollers, and the diameter of the supporting rubber rollers is 200 mm.
Example 5
In the actual production process, the roller mold can be engraved by laser or diamond knife, therefore, the roller mold engraved by laser or diamond knife is selected to be implemented according to the method of example 2, then the existing integral curing UV transfer printing method is selected to be implemented and used as a comparative example, and finally the 4 implementation processes and results are recorded, the main parameters and the comparison are as follows:
in summary, the above-mentioned embodiments are only preferred embodiments of the present invention, and all equivalent changes and modifications made within the scope of the claims of the present invention should be covered by the present invention.
Claims (10)
1. A surface micro-crosslinking process suitable for preparing a deep-textured film, the surface micro-crosslinking process comprising a roller mold (4) having a deep texture on the outer surface, characterized in that: the depth of the deep texture on the roller mold (4) is 10-20 μm, the distance between adjacent deep textures is 5 μm, and the surface micro-crosslinking process comprises the following steps:
A. taking a PET base film (3) with the thickness of 30-50 mu m, and coating a layer of UV resin on the upper surface of the PET base film (3) to form a UV sol layer (2), wherein the thickness of the UV sol layer (2) is 15-30 mu m;
B. carrying out radiation curing on the UV sol layer (2) at normal temperature and normal pressure to form a micro-crosslinking surface (1) on the upper surface of the UV sol layer (2), wherein the thickness of the micro-crosslinking surface (1) is 0.05-0.1 time of that of the UV sol layer (2), and the micro-crosslinking degree of the micro-crosslinking surface (1) is controlled to be 1-8%;
C. pressing the UV sol layer (2) and a roller mold (4) to enable the micro-crosslinked surface (1) to be completely attached to the deep texture, and filling the deep texture on the roller mold (4) with UV resin under the action of pressure;
D. and C, after the pressing in the step C, carrying out photocuring by adopting a UV lamp, curing for 1-2s under ultraviolet waves, and rolling to obtain the deep texture film.
2. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 1, wherein: the UV resin comprises the following components in percentage by weight:
the preparation method comprises the following steps: firstly, adding all epoxy acrylate resin and polyester acrylate resin into a reaction container, uniformly stirring, then mixing all trifunctional monomer, monofunctional monomer, light stabilizer, antioxidant, photoinitiator and coupling agent, adding into the reaction container, controlling the temperature of the reaction container to be kept at 25-30 ℃, and obtaining UV resin after the reaction is finished, wherein the viscosity of the UV resin is 300-500 cps.
3. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 1, wherein: the degree of micro-crosslinking of the micro-crosslinked surface (1) is determined as follows:
s1: b, after radiation curing, forming a UV sol layer (2) and micro-crosslinked surface (1) composite structure on the PET base film (3), cutting a sample with a three-layer film structure of the PET base film (3), the UV sol layer (2) and the micro-crosslinked surface (1), weighing the sample, recording the weight W1, then placing the sample into a stainless steel mesh bag, and recording the total weight of the sample and the stainless steel mesh bag as W2;
s2: then taking the stainless steel wire to seal the stainless steel mesh bag, wherein the total weight of the stainless steel mesh bag is recorded as W3;
s3: carrying out xylene reflux extraction on the sealed stainless steel mesh bag, drying, and weighing the stainless steel mesh bag, wherein the weight is recorded as W4;
s4: the density of the PET base film (3) is rho, the thickness of the PET base film (3) is b, the weight M of the PET base film (3) per square meter of the sample is rho b, and if the coating amount of the UV resin per square meter is V g, the micro-crosslinking degree is V
4. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 3, wherein: the coating weight V per square meter is 10-30 g.
5. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 3, wherein: and B, curing the radiation in the step B into one of EB radiation, infrared radiation and ultraviolet radiation.
6. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 5, wherein: the EB radiation is performed by adopting an electron beam with 200-300MeV, the radiation atmosphere is 95 percent of nitrogen environment, and the radiation time is 0.5-1S.
7. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 5, wherein: the ultraviolet radiation is irradiation by UVC short wave ultraviolet rays, the wavelength range is 280-365nm, and the irradiation time is 0.5-1 s.
8. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 2, wherein: the light stabilizer is a hindered amine light stabilizer, the antioxidant is triethylene glycol ether-bis (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, the photoinitiator comprises TPO and 184, and the coupling agent is one or a mixture of vinyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane.
9. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 8, wherein: the trifunctional monomer is one or two of trimethylolpropane triacrylate, pentaerythritol triacrylate and propoxylated glycerol triacrylate, and the monofunctional monomer is one of 2-phenoxyethyl acrylate, hexadecanol acrylate and isodecyl alcohol acrylate.
10. A surface micro-crosslinking process suitable for preparing deep textured films according to claim 1, wherein: the deep texture on the roller mold (4) is in a deep V shape, the diameter of the roller mold (4) is 250-270 mm, the front side and the rear side of the roller mold (4) are provided with supporting rubber rollers, and the diameter of the supporting rubber rollers is 180-220 mm.
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