CN113388141A - PET film for laminating and compounding home decoration building materials and preparation method thereof - Google Patents
PET film for laminating and compounding home decoration building materials and preparation method thereof Download PDFInfo
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- CN113388141A CN113388141A CN202110861802.1A CN202110861802A CN113388141A CN 113388141 A CN113388141 A CN 113388141A CN 202110861802 A CN202110861802 A CN 202110861802A CN 113388141 A CN113388141 A CN 113388141A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/056—Forming hydrophilic coatings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/14—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
- C08J2433/16—Homopolymers or copolymers of esters containing halogen atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
Abstract
The invention belongs to the technical field of PET films, and particularly relates to a PET film for laminating and compounding home decoration building materials and a preparation method thereof; the transparent PET base film comprises a transparent PET base film and a precoating layer, wherein the precoating layer comprises the following components in percentage by mass: 30-40% of waterborne resin WR-01; 60-70% of deionized water; 0.1-0.5% of water-based wetting and leveling agent; the waterborne resin WR-01 is prepared from hydrophilic acrylic shell resin and hydrophobic core layer resin of which the end group has double-bond functional groups; the invention improves the permeability of the precoating layer by designing the core shell of the high polymer material used by the online coating liquid, using trifluoroethyl methacrylate with lower refractive index as the shell, introducing a double-bond-containing functional group into the core layer, and controlling the activity of the double-bond-containing functional group, so that the coated film can be kept stable under room temperature storage. The pretreatment layer and the upper layer solvent-free UV adhesive are integrally and synchronously cured during curing to improve the interlayer adhesion and the high temperature and high humidity resistance.
Description
Technical Field
The invention belongs to the technical field of PET films, and particularly relates to a PET film for laminating and compounding home decoration building materials and a preparation method thereof.
Background
With the increasing requirements for quality and environmental problems worldwide, the home decoration industry has raised higher requirements for the quality and environmental protection of the raw materials used.
The plates used in the home decoration industry are usually decorated by spraying in the past, and the method mainly has the following defects: 1. the outward appearance is decorated and is had the limitation, and special decorative pattern can not realize, hardly makes flawless highlight high fullness panel, 2, in the aspect of the environmental protection, the spraying can lead to a large amount of organic solvents to volatilize atmospheric environment, and the material utilization ratio of spraying is not high, and the overspray leads to the waste of material and the pollution of environment.
The home decoration plate is manufactured by adopting the process of precoating a PET film in a factory and then laminating a film, and the defects can be overcome. However, due to the diversity of the processes of downstream customers in the processing process, the antifouling and scratch-resistant film for home decoration building materials at present needs to meet a series of requirements that the film and a hot melt adhesive film, a solvent-free UV adhesive, a hard UV coating and melamine impregnated paper have good interlayer adhesion and the like. However, the above requirements cannot be met by means of corona treatment on the surface of the PET film, and even if the pre-coating film on the market at present is adopted, the problem of insufficient use universality exists, so that the use is inconvenient and the product quality fluctuates.
Disclosure of Invention
One object of the present invention is: the PET base film is mainly characterized in that a hydrophilic acrylic resin shell layer with low refractive index is synthesized to disperse a hydrophobic nuclear layer with a terminal group having a double-bond functional group, and a cross-linking agent and an auxiliary agent with excellent adhesion with PET are matched to realize adhesion to the PET base film and adhesion to a subsequent coating.
In order to achieve the technical purpose, the technical scheme of one aspect of the invention is as follows:
the PET film for laminating and compounding the home decoration building materials comprises a transparent PET base film and a precoating layer, wherein the precoating layer comprises the following components in percentage by mass:
30-40% of waterborne resin WR-01;
60-70% of deionized water;
0.1-0.5% of water-based wetting and leveling agent;
the waterborne resin WR-01 is prepared from hydrophilic acrylic shell resin and hydrophobic core layer resin with a double-bond functional group at the end group.
Further, the preparation method of the waterborne resin WR-01 comprises the following steps: uniformly mixing hydrophilic acrylic resin shell resin and hydrophobic core layer resin with double-bond functional groups at the end groups, adding N, N dimethylethanolamine for neutralization, adding deionized water, and dispersing at high speed to obtain the waterborne resin WR-01.
Further, the hydrophilic acrylic shell resin comprises the following components in parts by mass in some preferred embodiments:
further, the preparation method of the hydrophilic acrylic shell resin comprises the following steps:
1) weighing the raw materials, putting trifluoroethyl methacrylate, butyl acrylate, isobornyl methacrylate, acrylic acid and an initiator LUPEROX 531M80 into a dropwise adding kettle,
2) adding an organic solvent diethylene glycol dimethyl ether into a reaction kettle, heating until reflux begins, beginning to dropwise add the mixed monomer, and controlling the dropwise adding speed to finish dropwise adding within 3 hours;
3) and adding an initiator LUPEROX 531M80 accounting for 0.4-0.6% of the total monomer mass after the dripping is finished, and continuing to perform heat preservation reaction for 2 hours to obtain a hydrophilic acrylic resin shell layer with low refractive index.
Further, the hydrophobic core layer resin with the end group having the double-bond functional group comprises the following components in percentage by mass:
70% of hydrophobic core layer epoxy resin with bifunctional end groups and double-bond functional groups;
diethylene glycol dimethyl ether 30%.
Further, the hydrophobic core layer epoxy resin with the bifunctional end group and the double-bond functional group is NeoRad E-20.
A preparation method of a PET film for laminating and compounding home decoration building materials comprises the following steps:
1) sequentially adding the waterborne resin WR-01, the deionized water and the waterborne wetting and leveling agent into a reaction kettle in sequence, stirring and dispersing uniformly, filtering to remove impurities and foams,
2) adding a cross-linking agent before coating, and diluting with water to a solid content of 5-10%, preferably 10% to obtain PE T online coating liquid;
3) the prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried at 230 ℃ for 30 seconds to obtain a pretreatment layer with the dry film thickness of about 50 nm, and cooled to room temperature to obtain the PET film for laminating and compounding the home decoration building materials.
Compared with the prior art, the invention has the beneficial effects that:
the invention improves the permeability of the precoating layer by designing the core shell of the high polymer material used by the online coating liquid, using trifluoroethyl methacrylate with lower refractive index as the shell, introducing a double-bond-containing functional group into the core layer, and controlling the activity of the double-bond-containing functional group, so that the coated film can be kept stable under room temperature storage.
By selecting and using a carbodiimide crosslinking agent CX-300 to carry out crosslinking, and carrying out on-line coating on the premise of not changing the prior production process of PET, the PET film for laminating and compounding the home decoration building materials is obtained. Even if the UV coating is coated on the two sides of the base film in the using process, the base film cannot penetrate through the base film due to UV irradiation during coating on the first side, so that the adhesive force of the UV adhesive on the other side is not influenced. The pretreatment layer and the upper layer solvent-free UV adhesive are integrally and synchronously cured during curing to improve the interlayer adhesion and the high temperature and high humidity resistance.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The raw materials in the invention are as follows:
waterborne resin WR-01 self-made
Water-based acrylic resin RX-7740 Nippon carbide Industrial Co., Ltd
Water-soluble saturated polyester resin Z-730 Cross-reactive chemical industry Co., Ltd
Aqueous hydrolysis resistant agent CX-300 Shanghai DSM
Aqueous amino resin CYMEL 385 Shanghai Wen Keel
Aqueous enclosed curing agent BL XP 2706 CorsiChun (China) Co., Ltd
Water dispersible curing agent XP-2655 CorsiChuang (China) Co., Ltd
Aqueous oxazoline cross-linking agent WS +500 Japanese catalyst
Solvent-free UV glue Changxing of Taiwan China
Jiangsu science and technology company Limited for melamine impregnated paper
Hot melt adhesive film Zhejiang Hongmai New Material Co Ltd
Tech-tech. Co Ltd for PET-based film Ningbo Material from Zhejiang
The preparation method of WR-01 comprises the following steps:
the waterborne resin WR-01 is prepared by uniformly mixing 70% of self-made hydrophilic acrylic resin shell resin and 30% of hydrophobic core layer resin with double-bond functional groups at end groups, adding N, N dimethylethanolamine with the mass being 7% of the total mass of the core layer resin and the shell layer resin for neutralization, and adding deionized water for high-speed dispersion to obtain the waterborne polymer resin WR-01 with high anti-reflection and enhanced adhesive force and the solid content being 25%.
The shell resin of the self-made hydrophilic acrylic resin in the present invention is preferably 75%, and if the addition amount is less than 70%, the hydrophilicity of the obtained resin gradually becomes poor, resulting in poor workability, and if the addition amount is more than 70%, the hydrophilicity of the obtained resin gradually becomes good, resulting in poor water resistance of the final coating layer.
According to the invention, N dimethyl ethanolamine (DMEA) is added, the boiling point is 134 ℃, the volatilization speed is moderate, and the water resistance of a paint film is excellent due to little residual quantity of carboxyl when the paint film is cured.
The formula of the hydrophilic acrylic resin shell resin is as follows:
according to the invention, trifluoroethyl methacrylate is used as a fluorine-containing monomer, which does not affect the mechanical and chemical stability of the emulsion, but is based on the surface activity effect of fluorine, the monomer is helpful for improving the stability of the emulsion in the polymerization process, has a low refractive index (the refractive index is 1.359 at 25 ℃), can improve the hydrophobicity, stain resistance, glossiness, transparency and other properties of the polymer, and preferably, the addition amount is 32-40%, too much causes the deterioration of the flexibility and temperature resistance grade of a coating film, and too little refractive index cannot meet the design requirement. Isobornyl methacrylate (IBOMA) contains a huge rigid side group, namely isobornyl, has a strong inhibiting effect on the movement of polymer chain segments, greatly improves the heat resistance, the wear resistance, the water absorption resistance, the shrinkage resistance and the toughness of the polymer, and is beneficial to the subsequent coating and high-temperature baking of a coating. The polymer of acrylic acid has excellent water resistance, low temperature flexibility resistance and excellent weather and sunlight resistance. LUPEROX 531M80 is a 1, 1' -bis (t-amylperoxy) cyclohexane initiator with better color and narrower molecular distribution.
The preparation method comprises the following steps: 50 g (34.84%) of trifluoroethyl methacrylate, 41 g (28.57%) of butyl acrylate, 35 g (24.39%) of isobornyl methacrylate, 14 g (9.76%) of acrylic acid and 3.5 g (2.43%) of LUPEROX 531M80 in the above proportion are put into a dropping kettle, 60 g of organic solvent diethylene glycol dimethyl ether is added into the reaction kettle, the mixture is heated to 150 ℃ to start reflux, the dropping of the mixed monomer is started, and the dropping speed is controlled to be completed within 3 hours. After the dropwise addition, 0.5 percent of initiator LUPEROX 531M80 of the total monomer mass is added, and the heat preservation reaction is continued for 2 hours to obtain a hydrophilic acrylic resin shell layer with low refractive index (solid content is 70 percent).
The formula of the hydrophobic core layer resin with the end group having double bond functional group is as follows:
the bifunctionality end group of the hydrophobic core layer epoxy resin NeoRad E-2070 percent with double bond functional groups
Diethylene glycol dimethyl ether 30%
Adding into a reaction kettle, and stirring and dispersing uniformly.
The proportion of the coating liquid is as follows:
WR-0140% aqueous resin
59.5 percent of deionized water
6040.5 percent of water-based wetting leveling agent
The preparation method comprises the following steps:
1) sequentially adding the waterborne resin WR-01, the deionized water and the waterborne wetting and leveling agent into a reaction kettle in sequence, stirring and dispersing uniformly, filtering to remove impurities and foams,
2) adding a cross-linking agent before coating, and diluting with water to obtain a solid content of 10% to obtain a PET online coating liquid;
the solids content of the coating liquor in this step is 5 to 15%, particularly preferably 10%. When the solid content is 10%, the light transmittance of the coated coating layer is better, when the solid content is less than 5%, the gluing amount is small, the adhesive force of the UV glue is influenced, and when the solid content is more than 15%, the cost is increased, the curing is poor, and the film is easy to break.
In the step, a carbodiimide crosslinking agent CX-300 is selected, so that the system can be rapidly crosslinked, and the coating performance is better than that of other crosslinking agents. Of course, other suitable crosslinking agents are equally suitable and will not be described in further detail herein.
3) Coating the prepared PET online coating liquid on a 250 mu transparent PET base film by using a 3 mu wire rod, drying at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of about 50 nanometers, and cooling to room temperature to obtain the PET film for laminating and compounding the home decoration building materials.
The following specific examples are further illustrated, and the percentages in the present invention are by mass unless otherwise specified.
Example 1
WR-0140% aqueous resin
59.5 percent of deionized water
6040.5 percent of water-based wetting leveling agent
The preparation method comprises the following steps:
sequentially adding the waterborne polymer resin WR-01, the deionized water and the waterborne wetting and leveling agent 604, stirring and dispersing uniformly, and filtering to remove impurities and foams. Adding a carbodiimide crosslinking agent CX-300 of waterborne resin WR-01 with the mass of 5% before coating, and diluting the mixture with water to the solid content of 10% to obtain the PET online coating liquid.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of about 50 nanometers, and cooled to room temperature for performance test, and the specific table is shown in Table 1.
In the embodiments of the present invention, the coating is performed on one surface of the PET base film, and may be performed on both sides of the PET base film as needed in the actual production process.
Example 2
WR-0140% aqueous resin
59.5 percent of deionized water
6040.5 percent of water-based wetting leveling agent
The water-based polymer resin WR-01 with the proportion is deionized, the water-based wetting and leveling agent 604 is sequentially added, stirred and dispersed evenly, and impurities and foams are removed by filtration. Before coating, adding waterborne amino resin CYMEL 385 with the mass of 5 percent of waterborne resin WR-01, and diluting with water to the solid content of 10 percent to obtain the PET online coating liquid.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of about 50 nanometers, and cooled to room temperature for performance test, and the specific table is shown in Table 1.
Example 3
WR-0140% aqueous resin
59.5 percent of deionized water
6040.5 percent of water-based wetting leveling agent
The water-based polymer resin WR-01 with the proportion is deionized, the water-based wetting and leveling agent 604 is sequentially added, stirred and dispersed evenly, and impurities and foams are removed by filtration. Before coating, adding a waterborne closed curing agent BL XP 2706 with the mass of 5% of waterborne resin WR-01, and diluting with water to the solid content of 10% to obtain the online PE coating liquid.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of about 50 nanometers, and cooled to room temperature for performance test, and the specific table is shown in Table 1.
Example 4
WR-0140% aqueous resin
59.5 percent of deionized water
6040.5 percent of water-based wetting leveling agent
The water-based polymer resin WR-01 with the proportion is deionized, the water-based wetting and leveling agent 604 is sequentially added, stirred and dispersed evenly, and impurities and foams are removed by filtration. Before coating, adding waterborne oxazoline WS-500 with the mass of 5% of waterborne resin WR-01, and diluting with water to the solid content of 10% to obtain the PET online coating liquid.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried for 30 seconds at 230 ℃ to obtain a pretreatment layer with the dry film thickness of about 50 nanometers, and cooled to room temperature for performance test.
Example 5
The water-based resin WR-01 and the water-based acrylic resin RX-7740 in the proportion are deionized, the water-based wetting and leveling agent 604 is sequentially added in sequence, the mixture is stirred and dispersed uniformly, and impurities and foams are removed by filtration. Before coating, adding a water dispersible curing agent XP-2655 with the mass of 5 percent of waterborne resin WR-01, and diluting the mixture with water to the solid content of 10 percent to obtain the PET online coating liquid.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of about 50 nanometers, and cooled to room temperature for performance test, and the specific table is shown in Table 1.
Example 6
The water-based resin WR-01 and the water-based acrylic resin RX-7740 in the proportion are deionized, the water-based wetting and leveling agent 604 is sequentially added in sequence, the mixture is stirred and dispersed uniformly, and impurities and foams are removed by filtration. Adding a carbodiimide crosslinking agent CX-300 of waterborne resin WR-01 with the mass of 5% before coating, and diluting the mixture with water to the solid content of 10% to obtain the PET online coating liquid.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of about 50 nanometers, and cooled to room temperature for performance test, and the specific table is shown in Table 1.
Comparative example 1
Water-soluble saturated polyester resin Z-73040%
59.5 percent of deionized water
6040.5 percent of water-based wetting leveling agent
The water-soluble saturated polyester resin, the deionized water and the water-based wetting and leveling agent 604 are sequentially added according to the proportion, stirred and dispersed uniformly, and filtered to remove impurities and foams. Adding a carbodiimide crosslinking agent CX-300 of waterborne resin WR-01 with the mass of 5% before coating, and diluting the mixture with water to the solid content of 10% to obtain the PET online coating liquid.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried for 30 seconds at 230 ℃ to obtain a pretreatment layer with the dry film thickness of about 50 nanometers, and cooled to room temperature for performance test. See table 1 for details.
Comparative example 2
WR-0240% of water-based resin
59.5 percent of deionized water
6040.5 percent of water-based wetting leveling agent
The preparation method comprises the following steps:
the waterborne resin WR-02 is prepared by uniformly mixing 70% of self-made hydrophilic acrylic resin shell resin and 30% of hydrophobic core layer resin with double bond functional groups at the end groups, adding N, N dimethylethanolamine with the mass being 7% of the total mass of the core layer resin and the shell layer resin for neutralization, and adding deionized water for high-speed dispersion to obtain the waterborne polymer resin WR-02 with the solid content being 25%.
The formula of the hydrophilic acrylic resin shell resin is as follows:
the preparation method comprises the following steps: 50 g of methyl methacrylate, 41 g of butyl acrylate, 35 g of isobornyl methacrylate, 14 g of acrylic acid and 3.5 g of LUPEROX 531M80 which are proportioned above are put into a dropping kettle, 60 g of organic solvent diethylene glycol dimethyl ether is added into a reaction kettle, the mixture is heated to 150 ℃ until reflux begins, the mixed monomer is dropped, and the dropping speed is controlled to be completed within 3 hours. After the dropwise addition, an initiator LUPEROX 531M80 with the total monomer content of 0.5% is added, and the heat preservation reaction is continued for 2 hours to obtain a hydrophilic acrylic resin shell (with the solid content of 70%).
The formula of the hydrophobic core layer resin with the end group having double bond functional group is as follows:
the bifunctionality end group of the hydrophobic core layer epoxy resin NeoRad E-2070 percent with double bond functional groups
Diethylene glycol dimethyl ether 30%
Adding into a reaction kettle, and stirring and dispersing uniformly.
Sequentially adding the waterborne polymer resin WR-02, the deionized water and the waterborne wetting and leveling agent 604, stirring and dispersing uniformly, and filtering to remove impurities and foams. Adding a carbodiimide cross-linking agent CX-300 of which the mass is 5 percent of that of waterborne resin WR-02 before coating, and diluting the mixture with water to obtain the PET online coating liquid with the solid content of 10 percent.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of about 50 nanometers, and cooled to room temperature for performance test, and the specific table is shown in Table 1.
Comparative example 3
WR-0340% of aqueous resin
59.5 percent of deionized water
6040.5 percent of water-based wetting leveling agent
The preparation method comprises the following steps:
the waterborne resin WR-03 is prepared by uniformly mixing 70% of self-made hydrophilic acrylic resin shell resin and 30% of hydrophobic core layer resin with double bond functional groups at the end groups, adding N, N dimethylethanolamine with the mass being 7% of the total mass of the core layer resin and the shell layer resin for neutralization, and adding deionized water for high-speed dispersion to obtain the waterborne polymer resin WR-03 with the solid content being 25%.
The formula of the hydrophilic acrylic resin shell resin is as follows:
the preparation method comprises the following steps: 50 g of styrene, 41 g of butyl acrylate, 35 g of isobornyl methacrylate, 14 g of acrylic acid and 3.5 g of LUPEROX 531M80 serving as an initiator are put into a dropwise adding kettle, 60 g of organic solvent diethylene glycol dimethyl ether is added into a reaction kettle, the temperature is heated to 150 ℃ until reflux begins, the mixed monomer is dropwise added, and the dropwise adding speed is controlled to be completed within 3 hours. After the dropwise addition, an initiator LUPEROX 531M80 with the total monomer content of 0.5% is added, and the heat preservation reaction is continued for 2 hours to obtain a hydrophilic acrylic resin shell (with the solid content of 70%).
The formula of the hydrophobic core layer resin with the end group having double bond functional group is as follows:
the bifunctionality end group of the hydrophobic core layer epoxy resin NeoRad E-2070 percent with double bond functional groups
Diethylene glycol dimethyl ether 30%
Adding into a reaction kettle, and stirring and dispersing uniformly.
Sequentially adding the waterborne polymer resin WR-03, the deionized water and the waterborne wetting and leveling agent 604, stirring and dispersing uniformly, and filtering to remove impurities and foams. Adding a carbodiimide cross-linking agent CX-300 of which the mass is 5 percent of that of waterborne resin WR-03 before coating, and diluting the mixture with water to obtain the PET online coating liquid with the solid content of 10 percent.
The prepared PET online coating liquid is coated on a 250 mu transparent PET base film by a 3 mu wire rod, dried at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of about 50 nanometers, and cooled to room temperature for performance test, and the specific table is shown in Table 1.
The test method comprises the following steps:
the method for testing the light transmittance refers to GB/T2410-2008.
The haze test method is referred to GB/T2410-2008.
The adhesion test method is referred to GB/T9286-1998.
The hardness test method comprises the following steps: mitsubishi pencil, load 500g, (coating pushed off).
The surface tension test method is referred to GB/T14216-2008.
The method for testing the adhesive force of the UV adhesive without the solvent refers to GB/T9286-1998.
The test method of blocking resistance is as follows: 20 pieces of 100cm2The samples were stacked and laminated with a 10Kg weight for 7 days at 60 ℃.
The method for testing the moist heat resistance comprises the following steps: constant temperature and humidity chamber (65 deg.C, 95% RH) 500h, and adhesive force with solvent-free UV glue.
The method for testing the adhesive force with the melamine impregnated paper comprises the following steps: laminating the PET pre-coating film and melamine dipped paper for 20 minutes at 180 ℃ under the pressure of 8 MPa.
The testing method of the hot melt adhesive film comprises the following steps: laminating the PET pre-coating film and the hot melt adhesive film at 140 ℃ under the pressure of 8 MPa for 10 seconds.
The cold and heat resistance cycle test method comprises the following steps: and (3) adopting a temperature and humidity regulating box to carry out temperature measurement of-40 ℃ multiplied by 1.5H on the sample piece, raising the temperature to room temperature, then raising the temperature to 65 ℃ multiplied by 1.5H, and then lowering the temperature to room temperature, thus carrying out appearance and adhesion measurement with a hot melt adhesive film circulation test.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (8)
1. A home decoration building material lamination composite PET film is characterized in that: the transparent PET base film comprises a transparent PET base film and a precoating layer, wherein the precoating layer comprises the following components in percentage by mass:
30-40% of waterborne resin WR-01;
60-70% of deionized water;
0.1-0.5% of water-based wetting and leveling agent.
2. The home decoration building material laminate composite PET film according to claim 1, wherein: the waterborne resin WR-01 is prepared from hydrophilic acrylic shell resin and hydrophobic core layer resin with a double-bond functional group at the end group.
The preparation method comprises the following steps: uniformly mixing hydrophilic acrylic resin shell resin and hydrophobic core layer resin with double-bond functional groups at the end groups, adding N, N dimethylethanolamine for neutralization, adding deionized water, and dispersing at high speed to obtain the waterborne resin WR-01.
3. The home decoration building material laminated composite PET film according to claim 2, wherein the hydrophilic acrylic shell resin comprises the following components in percentage by mass:
4. the PET film for laminating and compounding home decoration and building materials according to claim 3, wherein the preparation method of the hydrophilic acrylic shell resin comprises the following steps:
1) weighing the raw materials, putting trifluoroethyl methacrylate, butyl acrylate, isobornyl methacrylate, acrylic acid and an initiator LUPEROX 531M80 into a dropwise adding kettle,
2) adding an organic solvent diethylene glycol dimethyl ether into a reaction kettle, heating until reflux begins, beginning to dropwise add the mixed monomer, and controlling the dropwise adding speed to finish dropwise adding within 3 hours;
3) and adding an initiator LUPEROX 531M80 accounting for 0.4-0.6% of the total monomer mass after the dripping is finished, and continuing to perform heat preservation reaction for 2 hours to obtain a hydrophilic acrylic resin shell layer with low refractive index.
5. The PET film for laminating and compounding home decoration and building materials according to claim 2, wherein the hydrophobic core layer resin with the terminal group having the double bond functional group comprises the following components in percentage by mass:
70% of hydrophobic core layer epoxy resin with bifunctional end groups and double-bond functional groups;
diethylene glycol dimethyl ether 30%.
6. The PET film for laminated composite home decoration and building material as claimed in claim 5, wherein the hydrophobic core layer epoxy resin having a bifunctional end group and a double bond functional group is NeoRad E-20.
7. A preparation method of a PET film for laminating and compounding home decoration building materials is characterized by comprising the following steps: the preparation method comprises the following steps:
1) sequentially adding the waterborne resin WR-01, deionized water and the waterborne wetting and leveling agent into a reaction kettle in sequence, stirring and dispersing uniformly, and filtering to remove impurities and foams;
2) adding a cross-linking agent before coating, and diluting the mixture with water to a solid content of 5-10% to obtain the online coating liquid for the pre-coating;
3) coating the prepared PET online coating liquid on a 250 mu transparent PET base film by using a 3 mu wire rod, drying at 230 ℃ for 30 seconds to obtain a pretreatment layer with a dry film thickness of 50 nm, and cooling to room temperature to obtain the PET film for laminating and compounding the home decoration building materials.
8. The method for preparing the PET film for laminating and compounding home decoration and building materials according to claim 7, wherein the method comprises the following steps: the addition amount of the cross-linking agent is 1-5% of the mass of the waterborne resin WR-01.
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