CN110724296B - PVC (polyvinyl chloride) pre-coating film and preparation method thereof - Google Patents

PVC (polyvinyl chloride) pre-coating film and preparation method thereof Download PDF

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CN110724296B
CN110724296B CN201911078335.4A CN201911078335A CN110724296B CN 110724296 B CN110724296 B CN 110724296B CN 201911078335 A CN201911078335 A CN 201911078335A CN 110724296 B CN110724296 B CN 110724296B
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pvc
primer layer
coating
layer
acrylate
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CN110724296A (en
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李新雄
龙贺年
李辉
张冬明
李时珍
邓秀琳
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Bonfurt New Materials Co ltd
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Bonfurt New Materials Co ltd
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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
    • C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/002—Priming paints
    • 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
    • C08J2327/00—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 at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—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 at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/04—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 at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2327/06—Homopolymers or copolymers of vinyl chloride
    • 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
    • C08J2427/00—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 at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—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 at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/04—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 at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2427/06—Homopolymers or copolymers of vinyl chloride
    • 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
    • C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2475/04—Polyurethanes
    • C08J2475/14—Polyurethanes having carbon-to-carbon unsaturated bonds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention relates to the technical field of floor surface decoration materials, and particularly provides a PVC (polyvinyl chloride) pre-coating film and a preparation method thereof. The invention provides a PVC pre-coating film, which comprises a PVC transparent film layer and a radiation curing coating from bottom to top, wherein the radiation curing coating sequentially comprises an adhesion primer layer, an elastic primer layer, a functional layer and a finish coating from bottom to top, the adhesion primer layer and the elastic primer layer need to be specially designed, and the functional layer and the finish coating need to be commonly coated; the preparation raw materials of the adhesion primer layer comprise bifunctional polyurethane acrylate resin, vinyl chloride-vinyl acetate resin, bifunctional acrylate monomer and solvent. The invention utilizes the adhesion bottom layer and the elastic bottom layer to match with the PVC flexible film material, improves the adhesion force between the PVC film and the coating on the PVC pre-coating film, and simultaneously, the PVC pre-coating film can be subsequently formed on the PVC floor by high-temperature pressing, and the problems of whitening, cracking, yellowing and the like can not be caused, thereby providing a favorable material base for simplifying the processing production of the traditional PVC floor composite material.

Description

PVC (polyvinyl chloride) pre-coating film and preparation method thereof
Technical Field
The invention relates to the technical field of floor surface decoration materials, and particularly provides a PVC (polyvinyl chloride) pre-coating film and a preparation method thereof.
Background
The PVC floor is a novel light ground decoration material which is very popular in the world at present, has the advantages of environmental protection, super-strong wear resistance, various colors and varieties, quick installation and construction and the like, and is widely used and highly recognized in hospitals, schools, office buildings, markets, supermarkets, transportation tools and other places with large pedestrian volume.
In the actual use process, in order to meet the requirements of consumers on different performances of wear resistance, scratch resistance, strength and the like of the surface of the PVC floor, various functional coatings are often added on the surface of the PVC floor to meet the requirements of different consumers on different types of floors, but when the production of diversified floors is realized, various problems are easy to occur to the prepared PVC floor, for example, the adhesion force of the PVC floor coating is poor, the coating is easy to fall off locally, and the service life of the floor is reduced; in addition, the partially-textured PVC floor is easy to produce into a PVC floor with uneven gloss and large difference among floors.
Based on the problems of the PVC floor composite material in the prior art, a coating material which can effectively avoid the problems of low bonding force between coatings, more uniform gloss and more excellent performance needs to be developed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a PVC pre-coating film, which comprises a PVC transparent film layer and a radiation curing coating from bottom to top, wherein the radiation curing coating sequentially comprises an adhesion primer layer, an elastic primer layer, a functional layer and a finish paint layer from bottom to top; the preparation raw materials of the adhesion primer layer comprise bifunctional polyurethane acrylate resin, vinyl chloride-vinyl acetate resin, bifunctional acrylate monomer and solvent.
According to a preferable technical scheme, the preparation raw materials of the adhesion primer layer comprise, by weight, 2-10 parts of bifunctional polyurethane acrylate resin, 0-5 parts of vinyl chloride-vinyl acetate copolymer, 30-40 parts of bifunctional acrylate monomer, 30-50 parts of solvent and 0-1 part of initiator.
According to a preferable technical scheme, the elastic primer layer is prepared from 30-60 parts by weight of bifunctional polyurethane acrylate resin, 20-40 parts by weight of bifunctional acrylate monomer, 10-15 parts by weight of monofunctional acrylate and 0-5 parts by weight of initiator.
In a preferred embodiment of the present invention, the difunctional acrylate monomer is selected from any one or more of 1, 6-hexanediol diacrylate, neopentyl glycol diacrylate, dipropylene glycol diacrylate and tripropylene glycol diacrylate.
In a preferred embodiment of the present invention, the bifunctional urethane acrylate resin has a relative molecular weight of more than 3000;
preferably, the raw materials for preparing the difunctional urethane acrylate resin comprise polyol, isocyanate and hydroxyl-containing acrylate monomer; wherein the molar ratio of the polyol to the isocyanate is 1: 2 to 5.
In a preferred embodiment of the present invention, the monofunctional acrylate is selected from the group consisting of isobornyl acrylate, acryloylmorpholine, hydroxyethyl methacrylate, acrylic acid, methyl acrylate, ethyl acrylate, n-propyl acrylate, n-butyl acrylate, lauryl acrylate, stearyl acrylate, isopropyl acrylate, isobutyl acrylate, t-butyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate and ethoxyethyl acrylate.
As a preferred technical scheme of the invention, the polyhydric alcohol comprises A component polyhydric alcohol and B component polyhydric alcohol, wherein the relative molecular weight of the A component is 500-10000; the relative molecular weight of the component B is 450-30; preferably, the molar ratio of the component A to the component B is (1-3): 1.
as a preferable technical scheme of the invention, the molecular formula of the A component polyalcohol is OH-R3-COO-R1-COO-R2-OH, and R3、R1、R2Selected from any group.
Preferably, the B component polyol is selected from any one or combination of 1, 4-butanediol, 1, 4-cyclohexanedimethanol, hydroxyethylated bisphenol A, ethylene glycol, propylene glycol, hexylene glycol, p-phenylene glycol, neopentyl glycol, diethylene glycol.
Preferably, the a component polyol is selected from any one or combination of polycaprolactone diol, poly neopentyl glycol adipate diol, polycarbonate diol, poly 1, 4-butanediol adipate diol, poly ethylene glycol-propylene glycol adipate diol, poly neopentyl glycol adipate 1, 4-butanediol diol, poly propylene glycol ether diols, and poly tetrahydrofuran ether diols.
In a preferred embodiment of the present invention, the hydroxyl-containing acrylate monomer is selected from one or more of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxybutyl acrylate, methyl hydroxyacrylate, and hydroxypropyl methacrylate.
The second aspect of the present invention provides a method for preparing the PVC pre-coating film, comprising the steps of:
(1) respectively and uniformly stirring the preparation raw materials of the adhesion primer layer and the elastic primer layer by using a dispersion kettle to obtain a paint finished product;
(2) then, uniformly coating the primer layer on the surface of the PVC transparent film layer by using a roller coater;
(3) uniformly coating the elastic primer layer on the surface of the primer layer by using a roller coater, and carrying out LED-UV curing;
(4) coating the functional layer on the surface of the elastic primer layer uniformly by using a roller coater, and carrying out LED-UV curing;
(5) and (4) making a finish coat on the surface of the functional layer, and performing radiation curing to obtain the PVC pre-coating film.
Compared with the prior art, the PVC pre-coating film is obtained by matching the adhesion bottom layer and the elastic bottom layer with the PVC film material, so that the adhesion force of the coating on the surface of the PVC film is improved, the processing and forming of the PVC pre-coating film under the high-temperature condition are facilitated, the problems of whitening, cracking and yellowing in the processing process are avoided, and a favorable material basis is provided for simplifying the processing and production of the traditional PVC composite material.
Detailed Description
Unless otherwise indicated, implied from the context, or customary in the art, all parts and percentages herein are by weight and the testing and characterization methods used are synchronized with the filing date of the present application. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "preferably", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention. The sources of components not mentioned in the present invention are all commercially available.
In order to solve the problems in the prior art, the invention provides a PVC pre-coating film in a first aspect, which comprises a PVC transparent film layer and a radiation curing coating from bottom to top, wherein the radiation curing coating sequentially comprises a primer layer elastic primer layer, a functional layer and a finish paint layer from bottom to top; the preparation raw materials of the adhesion primer layer comprise bifunctional polyurethane acrylate resin, vinyl chloride-vinyl acetate resin, bifunctional acrylate monomer and solvent.
In one embodiment, the primer layer is prepared from 2-10 parts by weight of bifunctional urethane acrylate resin, 0-5 parts by weight of vinyl chloride-vinyl acetate copolymer resin, 30-40 parts by weight of bifunctional acrylate monomer, 30-50 parts by weight of solvent and 0-1 part by weight of initiator; preferably, the preparation raw materials of the adhesion primer layer comprise 4-8 parts of bifunctional polyurethane acrylate resin, 1-4 parts of vinyl chloride-vinyl acetate copolymer, 33-38 parts of bifunctional acrylate monomer, 35-45 parts of solvent and 0.2-0.8 part of initiator; more preferably, the raw material for preparing the adhesion primer layer includes 6 parts of the bifunctional urethane acrylate resin, 3 parts of the vinyl chloride-vinyl acetate copolymer, 35 parts of the bifunctional acrylate monomer, 40 parts of the solvent, and 0.5 part of the initiator.
In one embodiment, the elastic primer layer is prepared from 30-60 parts by weight of bifunctional polyurethane acrylate resin, 20-40 parts by weight of bifunctional acrylate monomer, 10-15 parts by weight of monofunctional acrylate and 0-5 parts by weight of initiator; preferably, the raw materials for preparing the elastic primer layer comprise 40-50 parts of bifunctional polyurethane acrylate resin, 25-35 parts of bifunctional acrylate monomer, 11-14 parts of monofunctional acrylate and 1-4 parts of initiator; more preferably, the raw materials for preparing the elastic primer layer include 45 parts of the difunctional urethane acrylate resin, 30 parts of the difunctional acrylate monomer, 13 parts of the monofunctional acrylate, and 3 parts of the initiator.
In one embodiment, the difunctional acrylate monomer is selected from any one or combination of 1, 6-hexanediol diacrylate, neopentyl glycol diacrylate, dipropylene glycol diacrylate, tripropylene glycol diacrylate; preferably the difunctional acrylate monomer is 1, 6-hexanediol diacrylate.
In one embodiment, the vinyl chloride-vinyl acetate copolymer is binary vinyl chloride-vinyl acetate copolymer and/or ternary vinyl chloride-vinyl acetate copolymer.
The present invention is not particularly limited to the purchasing manufacturers, and in one embodiment, the vinyl chloride-vinyl acetate copolymer is available from Mono Sam resin Co., Ltd, of Dongguan, from 14 to 50.
In one embodiment, the solvent is selected from the group consisting of any one or more of ethyl acetate, butyl acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, methanol, n-butanol, ethanol.
In one embodiment, the monofunctional acrylate is selected from the group consisting of isobornyl acrylate, acryloylmorpholine, hydroxyethyl methacrylate, n-propyl acrylate, n-butyl acrylate, lauryl acrylate, stearyl acrylate, isopropyl acrylate, isobutyl acrylate, t-butyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, ethoxyethyl acrylate in any combination of one or more thereof; preferably, the monofunctional acrylate is isobornyl acrylate and acryloyl morpholine; further preferably, the weight ratio of isobornyl acrylate to acryloyl morpholine is 1: (0.3 to 0.8); more preferably, the weight ratio of isobornyl acrylate to acryloyl morpholine is 1: 0.5.
in one embodiment, the initiator is selected from one or more of 1-hydroxycyclohexyl phenyl ketone (184), 2-hydroxy-2-methyl-1-phenyl-1-propanone (1173), 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinebenzyl phenyl) butanone (369), phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide (819), and (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide (TPO); preferably, the initiator is (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide (TPO).
In one embodiment, the difunctional urethane acrylate resin has a relative molecular weight greater than 3000; preferably, the raw materials for preparing the difunctional urethane acrylate resin comprise polyol, isocyanate and hydroxyl-containing acrylate monomer; wherein the molar ratio of the polyol to the isocyanate is 1: 2-5; preferably, the molar ratio of polyol to isocyanate is 1: 3.5.
in one embodiment, the hydroxyl-containing acrylate monomer content is used to completely block the isocyanate.
In one embodiment, the polyol comprises a component A polyol and a component B polyol, wherein the relative molecular weight of the component A is 500-10000; the relative molecular weight of the component B is 450-30.
In one embodiment, the molar ratio of the component A to the component B is (1-3): 1; more preferably, the molar ratio of the a component to the B component is 2: 1.
in one embodiment, the polyol of component A has the formula OH-R3-COO-R1-COO-R2-OH, and R3、R1、R2Selected from any group; preferably, the a component polyol is selected from any one or combination of more of polycaprolactone diol, poly neopentyl glycol adipate diol, polycarbonate diol, poly 1, 4-butylene adipate diol, poly ethylene glycol propylene glycol adipate diol, poly butylene glycol succinate diol, poly neopentyl glycol adipate 1, 4-butylene glycol diol, poly propylene glycol ether diol, poly tetrahydrofuran ether diol, poly 1,6 hexanediol adipate diol, and poly dimethyl phthalate propylene glycol diol; preferably, the A component polyol comprises polycaprolactone diol, poly neopentyl glycol adipate diol and polycarbonate diol; further preferably, the weight ratio of polycaprolactone diol to poly neopentyl glycol adipate diol to polycarbonate diol is 1: (0.5-1.5): (0.5 to 1.5); more preferably, the weight ratio of polycaprolactone diol to poly neopentyl glycol adipate diol to polycarbonate diol is 1: 1: 0.6.
in one embodiment, the polycaprolactone diol has a weight average molecular weight of 1000 to 3000; preferably, the weight average molecular weight of the polycaprolactone diol is 2000-2500.
In one embodiment, the weight average molecular weight of the poly neopentyl glycol adipate diol is 2000-4000; preferably, the weight average molecular weight of the polycaprolactone diol is 3000-3500.
In one embodiment, the polycarbonate diol has a weight average molecular weight of 2000 to 4000; preferably, the polycarbonate diol has a weight average molecular weight of 3000 to 3500.
The invention is not particularly limited to the manufacturers of polycaprolactone diol, poly neopentyl glycol adipate diol, and polycarbonate diol, but in one embodiment, polycaprolactone diol, poly neopentyl glycol adipate diol, and polycarbonate diol are respectively obtained from Asahi Sichuan chemistry.
In one embodiment, the B component polyol is selected from any one or combination of 1, 4-butanediol, 1, 4-cyclohexanedimethanol, hydroxyethylated bisphenol A, ethylene glycol, propylene glycol, hexylene glycol, p-phenylene glycol, neopentyl glycol, diethylene glycol; preferably, the B component polyol is selected from any one or combination of more of 1, 4-butanediol, 1, 4-cyclohexanedimethanol, hydroxyethylated bisphenol A; further preferably, the B component polyols include 1, 4-butanediol, 1, 4-cyclohexanedimethanol, and hydroxyethylated bisphenol A; further preferably, the weight ratio of 1, 4-butanediol, 1, 4-cyclohexanedimethanol, and hydroxyethylated bisphenol a is 1: (0.3-0.5): (0.1 to 0.3); more preferably, the weight ratio of 1, 4-butanediol, 1, 4-cyclohexanedimethanol, and hydroxyethylated bisphenol A is 1: 0.45: 0.2.
in one embodiment, the hydroxyl-containing acrylate monomer is selected from any one or a combination of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxybutyl acrylate, methyl hydroxyacrylate, hydroxypropyl methacrylate.
In one embodiment, the isocyanate is selected from any one or combination of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, lysine diisocyanate.
In the preparation process of the traditional PVC floor composite material, a PVC base plate and a PVC film are pressed and pasted at a high temperature to form a PVC plate base material, and then ultraviolet curing coating is made on the PVC plate base material to obtain a finished PVC floor. The PVC floor coating obtained by the process has poor adhesion, and paint is easy to fall off locally, so that the attractiveness of the PVC floor is affected; in addition, the PVC floor with partial texture is easy to produce and uneven gloss sometimes; according to the method, the paint coating is directly made on the PVC film, the obtained PVC pre-coating film is directly pressed and adhered with the PVC base plate at high temperature to form the PVC floor.
The applicant has found that the above problems can be better avoided when the flexible PVC film material is co-acted with two coatings, an adhesion primer layer and an elastic primer, the adhesion primer layer is formed by using a monomer and a solvent which are used for the corrosion of the PVC film, the vinyl chloride-vinyl acetate resin has similar polarity with the vinyl chloride in the structure of the PVC film, can greatly improve the adhesion of the coating to the PVC film, a small amount of difunctional urethane acrylate in the adhesion primer layer plays a bridging connection role between the PVC film and the elastic primer coating, the high proportion of difunctional urethane acrylate is used in the elastic primer coating, the difunctional urethane acrylate has excellent toughness and elongation, good yellowing resistance, through the optimization test of the primer layer and the elastic primer layer, the functional layer and the finish paint layer which are coated subsequently can use conventional and common paint, so that the problems of cracking, whitening and yellowing are avoided.
The source of the PVC transparent film layer is not particularly limited, and in one embodiment, the PVC transparent film layer is purchased from Jiangsu Green Meibang.
The source of the surface paint layer is not particularly limited, and the surface paint layer can be directly purchased or prepared by the user; in one embodiment, the topcoat is obtained from new materials technologies, inc, bang, of shann: UV scratch-resistant matte surface, model BMZ-1052G.
In one embodiment, the functional layer comprises any one or more of a wear-resistant primer layer, a hard primer layer and a matte primer layer, preferably a matte primer layer, the source of the matte primer is not particularly limited, and the matte primer can be directly purchased or prepared by self; in one embodiment, the matte primer is available from new materials technologies, inc, bang, ho, name: UV matte bottom, model BMZ-3331H.
The second aspect of the present invention provides a method for preparing the PVC pre-coating film, comprising the steps of:
(1) respectively and uniformly stirring the preparation raw materials of the adhesion primer layer and the elastic primer layer by using a dispersion kettle to obtain a finished coating;
(2) then, uniformly coating the primer layer on the surface of the PVC transparent film layer by using a roller coater;
(3) uniformly coating the elastic primer layer on the surface of the primer layer by using a roller coater, and carrying out LED-UV curing;
(4) coating the functional layer on the surface of the elastic primer layer uniformly by using a roller coater, and carrying out LED-UV curing;
(5) and (4) making a finish coat on the surface of the functional layer, and performing radiation curing to obtain the PVC pre-coating film.
In one embodiment, the coating amount of the adhesion primer layer is 3 to 15g/m2(ii) a Preferably, the coating weight of the adhesion primer layer is 4-10 g/m2(ii) a More preferably, the coating amount of the adhesion primer layer is 4g/m2。
In one embodiment, the elastic primer layer is coated in an amount of 3 to 20g/m2(ii) a Preferably, the coating amount of the elastic primer layer is 6-15 g/m2(ii) a More preferably, the coating amount of the elastic primer layer is 12g/m2。
In one embodiment, the coating amount of the functional layer is 3 to 20g/m2(ii) a Preferably, the coating weight of the functional layer is 6-15 g/m2(ii) a More preferably, the coating amount of the functional layer is 12g/m2。
In one embodiment, the coating weight of the finish coat is 3-20 g/m2(ii) a Preferably, the coating weight of the finish coat is 6-15 g/m2(ii) a More preferably, the coating weight of the top coat is 12g/m2。
In one embodiment, step (2) is performed by LED-UV curing, preferably, the wavelength of the LED-UV light source is 200-800nm, and the energy intensity of the light source is more than 7W/cm2(ii) a More preferably, the wavelength of the LED-UV light source in the step (2) is selected from 365nm, 385nm and 395nm, and the energy intensity of the light source is 10-12W/cm2。
In one embodiment, the wavelength of the LED-UV light source in the step (3) is 200-800nm, and the energy intensity of the light source is more than 7W/cm2(ii) a Preferably, the wavelength of the LED-UV light source in the step (3) is selected from 365nm, 385nm and 395nm, and the energy intensity of the light source is 10-12W/cm2。
In one embodiment, the wavelength of the LED-UV light source in the step (4) is 200-800nm, and the energy intensity of the light source is more than 7W/cm2(ii) a Preferably, the wavelength of the LED-UV light source in the step (4) is selected from 365nm, 385nm and 395nm, and the energy intensity of the light source is 10-12W/cm2。
In one embodiment, the curing manner in step (5) is electrodeless lamp UV curing.
Example 1
The embodiment 1 of the invention provides a PVC pre-coating film, which comprises a PVC transparent film layer and a radiation curing coating from bottom to top, wherein the radiation curing coating sequentially comprises an adhesion primer layer, an elastic primer layer, a functional layer and a finish paint layer from bottom to top;
the preparation raw materials of the adhesion primer layer comprise 6 parts of bifunctional polyurethane acrylate resin, 3 parts of vinyl chloride-vinyl acetate copolymer, 35 parts of bifunctional acrylate monomer, 40 parts of solvent and 0.5 part of initiator in parts by weight;
the elastic primer layer is prepared from 45 parts by weight of bifunctional polyurethane acrylate resin, 30 parts by weight of bifunctional acrylate monomer, 13 parts by weight of monofunctional acrylate and 3 parts by weight of initiator;
the difunctional acrylate monomer is 1, 6-hexanediol diacrylate; the vinyl chloride-vinyl acetate copolymer is vinyl chloride-vinyl acetate copolymer 14-50, which is available from Yifan resin Co., Ltd, of Dongguan city; the solvent is butyl acetate;
the monofunctional acrylate is isobornyl acrylate and acryloyl morpholine, and the weight ratio of the isobornyl acrylate to the acryloyl morpholine is 1: 0.5;
the initiator is (2,4, 6-trimethylbenzoyl) diphenyl phosphine oxide (TPO);
the preparation raw materials of the difunctional urethane acrylate resin comprise polyol, isocyanate and hydroxyl-containing acrylate monomer; the molar ratio of polyol to isocyanate is 1: 3.5; hydroxyl-containing acrylate monomer content for complete isocyanate blocking;
the polyol comprises A component polyol and B component polyol, wherein the molar ratio of the A component to the B component is 2: 1;
the component A polyol comprises polycaprolactone dihydric alcohol, poly neopentyl glycol adipate dihydric alcohol and polycarbonate dihydric alcohol, and the weight ratio of the polycaprolactone dihydric alcohol to the poly neopentyl glycol adipate dihydric alcohol to the polycarbonate dihydric alcohol is 1: 1: 0.6;
the weight average molecular weight of the polycaprolactone diol is 2000-2500, the weight average molecular weight of the polycaprolactone diol is 3000-3500, and the weight average molecular weight of the polycarbonate diol is 3000-3500;
the polyol of the component B comprises 1, 4-butanediol, 1, 4-cyclohexanedimethanol and hydroxyethylated bisphenol A, 1, 4-butanediol, 1, 4-cyclohexanedimethanol and hydroxyethylated bisphenol A in a weight ratio of 1: 0.45: 0.2;
the hydroxyl-containing acrylate monomer is hydroxyl methyl acrylate; the isocyanate is hexamethylene diisocyanate;
the finish paint is purchased from new material technology limited of bangfor, Hunan, and has the name: UV scratch-resistant matte surface, model BMZ-1052G.
The functional layer is a matte coating;
the matte primer is purchased from new materials technology limited, bang fret, hu nan, under the name: UV matte bottom, model BMZ-3331H;
the preparation method of the PVC pre-coating film comprises the following steps:
(1) uniformly stirring the preparation raw materials of the primer layer, the elastic primer layer, the functional layer and the finish paint layer by using a dispersion kettle respectively to obtain a paint finished product;
(2) then the surface of the PVC transparent film layer is uniformly coated with the adhesion primer layer by a roller, and the coating weight is 4g/m2Carrying out LED-UV curing; the wavelength of the LED-UV light source is 395nm, and the energy intensity of the light source is 10W/cm2；
(3) Then the elastic primer layer is evenly coated on the surface of the adhesion primer layer by a roller, and the coating weight is 12g/m2Carrying out LED-UV curing; the wavelength of the LED-UV light source is 395nm, and the energy intensity of the light source is 10W/cm2；
(4) Then the functional layer is evenly coated on the surface of the elastic priming coat layer by a roller coater, and the coating weight is 12g/m2Carrying out LED-UV curing; the wavelength of the LED-UV light source is 395nm, and the energy intensity of the light source is 10W/cm2；
(5) And (4) making a finish coat on the surface of the functional layer, and carrying out UV curing on the finish coat by using an electrodeless lamp to obtain the PVC pre-coating film.
Example 2
The embodiment 2 of the invention provides a PVC pre-coating film, which comprises a PVC transparent film layer and a radiation curing coating from bottom to top, wherein the radiation curing coating sequentially comprises an adhesion primer layer, an elastic primer layer, a functional layer and a finish paint layer from bottom to top;
the preparation raw materials of the adhesion primer layer comprise, by weight, 10 parts of bifunctional polyurethane acrylate resin, 5 parts of vinyl chloride-vinyl acetate copolymer, 40 parts of bifunctional acrylate monomer, 50 parts of solvent and 1 part of initiator;
the elastic primer layer is prepared from 60 parts by weight of bifunctional polyurethane acrylate resin, 40 parts by weight of bifunctional acrylate monomer, 15 parts by weight of monofunctional acrylate and 5 parts by weight of initiator;
the difunctional acrylate monomer is 1, 6-hexanediol diacrylate; the vinyl chloride-vinyl acetate copolymer is vinyl chloride-vinyl acetate copolymer 14-50, which is available from Yifan resin Co., Ltd, of Dongguan city; the solvent is butyl acetate;
the monofunctional acrylate is isobornyl acrylate and acryloyl morpholine, and the weight ratio of the isobornyl acrylate to the acryloyl morpholine is 1: 0.8;
the initiator is (2,4, 6-trimethylbenzoyl) diphenyl phosphine oxide (TPO);
the preparation raw materials of the difunctional urethane acrylate resin comprise polyol, isocyanate and hydroxyl-containing acrylate monomer; the molar ratio of polyol to isocyanate is 1: 5; hydroxyl-containing acrylate monomer content for complete isocyanate blocking;
the polyol comprises A component polyol and B component polyol, wherein the molar ratio of the A component to the B component is 3: 1;
the component A polyol comprises polycaprolactone dihydric alcohol, poly neopentyl glycol adipate dihydric alcohol and polycarbonate dihydric alcohol, and the weight ratio of the polycaprolactone dihydric alcohol to the poly neopentyl glycol adipate dihydric alcohol to the polycarbonate dihydric alcohol is 1: 1.5: 1.5;
the weight average molecular weight of the polycaprolactone diol is 2000-2500, the weight average molecular weight of the polycaprolactone diol is 3000-3500, and the weight average molecular weight of the polycarbonate diol is 3000-3500;
the polyol of the component B comprises 1, 4-butanediol, 1, 4-cyclohexanedimethanol and hydroxyethylated bisphenol A, 1, 4-butanediol, 1, 4-cyclohexanedimethanol and hydroxyethylated bisphenol A in a weight ratio of 1: 0.5: 0.3;
the hydroxyl-containing acrylate monomer is hydroxyl methyl acrylate; the isocyanate is hexamethylene diisocyanate;
the topcoat layer and the functional layer were the same as in example 1;
the preparation method of the PVC precoating film was the same as in example 1.
Example 3
Embodiment 3 of the present invention provides a PVC pre-coating film, which comprises, from bottom to top, a PVC transparent film layer and a radiation curing coating, wherein the radiation curing coating comprises, from bottom to top, an adhesion primer layer, an elastic primer layer, a functional layer and a finish paint layer in sequence;
the preparation raw materials of the adhesion primer layer comprise, by weight, 2 parts of bifunctional polyurethane acrylate resin, 1 part of vinyl chloride-vinyl acetate copolymer, 30 parts of bifunctional acrylate monomer, 30 parts of solvent and 0.1 part of initiator;
the elastic primer layer is prepared from the raw materials of, by weight, 30 parts of bifunctional polyurethane acrylate resin, 20 parts of bifunctional acrylate monomer, 10 parts of monofunctional acrylate and 1 part of initiator;
the difunctional acrylate monomer is 1, 6-hexanediol diacrylate; the vinyl chloride-vinyl acetate copolymer is vinyl chloride-vinyl acetate copolymer 14-50, which is available from Yifan resin Co., Ltd, of Dongguan city; the solvent is butyl acetate;
the monofunctional acrylate is isobornyl acrylate and acryloyl morpholine, and the weight ratio of the isobornyl acrylate to the acryloyl morpholine is 1: 0.3;
the initiator is (2,4, 6-trimethylbenzoyl) diphenyl phosphine oxide (TPO);
the preparation raw materials of the difunctional urethane acrylate resin comprise polyol, isocyanate and hydroxyl-containing acrylate monomer; the molar ratio of polyol to isocyanate is 1: 3; hydroxyl-containing acrylate monomer content for complete isocyanate blocking;
the polyol comprises A component polyol and B component polyol, wherein the molar ratio of the A component to the B component is 1.5: 1;
the component A polyol comprises polycaprolactone dihydric alcohol, poly neopentyl glycol adipate dihydric alcohol and polycarbonate dihydric alcohol, and the weight ratio of the polycaprolactone dihydric alcohol to the poly neopentyl glycol adipate dihydric alcohol to the polycarbonate dihydric alcohol is 1: 0.5: 0.5;
the weight average molecular weight of the polycaprolactone diol is 2000-2500, the weight average molecular weight of the polycaprolactone diol is 3000-3500, and the weight average molecular weight of the polycarbonate diol is 3000-3500;
the polyol of the component B comprises 1, 4-butanediol, 1, 4-cyclohexanedimethanol and hydroxyethylated bisphenol A, 1, 4-butanediol, 1, 4-cyclohexanedimethanol and hydroxyethylated bisphenol A in a weight ratio of 1: 0.3: 0.1;
the hydroxyl-containing acrylate monomer is hydroxyl methyl acrylate; the isocyanate is hexamethylene diisocyanate;
the topcoat layer and the functional layer were the same as in example 1;
the preparation method of the PVC precoating film was the same as in example 1.
Example 4
Embodiment 4 of the present invention provides a PVC pre-coating film, which is the same as embodiment 1 in specific embodiment, except that the PVC pre-coating film comprises a PVC transparent film layer, an elastic primer layer, a functional layer, and a topcoat layer from bottom to top.
Example 5
Example 5 of the present invention provides a PVC precoating film, which is the same as example 1 except that the amount of the bifunctional urethane acrylate resin in the raw material for preparing the adhesion primer layer was 0.
Example 6
Example 6 of the present invention provides a PVC pre-coating film, which is similar to example 1 in specific embodiment, except that the raw material for preparing the adhesion primer layer includes 30 parts of bifunctional urethane acrylate resin, 3 parts of vinyl chloride-vinyl acetate resin, 35 parts of bifunctional acrylate monomer, 40 parts of solvent, and 0.5 part of initiator.
Example 7
Example 7 of the present invention provides a PVC precoating film, which is the same as example 1 except that the raw material for preparing the primer layer contains 0 parts of vinyl chloride-vinyl acetate copolymer.
Example 8
Embodiment 8 of the present invention provides a PVC precoating film, which is the same as embodiment 1 in specific embodiment, except that the PVC precoating film comprises, from bottom to top, a PVC transparent film layer, an adhesion primer layer, a functional layer, and a topcoat layer.
Example 9
Example 9 of the present invention provides a PVC precoating film, which is the same as example 1 except that the amount of the bifunctional urethane acrylate resin in the raw material for preparing the elastic primer layer was 0.
Example 10
The embodiment 10 of the invention provides a PVC pre-coating film, which is the same as the embodiment 1 in the specific implementation manner, and is characterized in that the raw materials for preparing the elastic primer layer comprise 20 parts of bifunctional polyurethane acrylate resin, 40 parts of bifunctional acrylate monomer, 15 parts of monofunctional acrylate and 5 parts of initiator.
Example 11
Example 11 of the present invention provides a PVC precoating film, the specific embodiment of which is the same as example 1, except that the monofunctional acrylate is hydroxyethyl methacrylate.
Example 12
Example 12 of the present invention provides a PVC precoating film, which is the same as example 1, except that 1, 4-cyclohexanedimethanol was used in an amount of 0.
Example 13
Example 12 of the present invention provides a PVC precoating film, which is substantially the same as example 1, except that the initiator is benzophenone.
Example 14
Example 14 of the present invention provides a PVC precoating film, which is substantially the same as example 1, except that the solvent is propylene glycol.
Performance evaluation
And heating the PVC pre-coating film and the SPC substrate obtained in the embodiment to 175 ℃, rolling for 5s through a steel roller, and cooling and forming to obtain the PVC floor composite material.
1. And (3) testing the adhesive force: the adhesion of the composite material prepared from the PVC pre-coating film obtained in examples 1-12 was measured according to ASTM D3359, and the test results are shown in Table 1;
and 2, PVC pre-coating film processability test: whether the PVC pre-coating film is whitish and cracked or not in the process of preparing the composite material by the PVC pre-coating film obtained in the embodiments 1-12 is observed, each embodiment corresponds to 100 samples, the whitish and cracked probability is calculated, and the test result is shown in Table 1.
Table 1 results of performance testing
Adhesion force Whitening (%) Cracking (%)
Example 1 5B 0 1
Example 2 5B 1 0
Example 3 5B 0 3
Example 4 0B 90 76
Example 5 4B 76 42
Example 6 4B 27 3
Example 7 2B 2 2
Example 8 4B 100 100
Example 9 5B 100 97
Example 10 5B 8 25
Example 11 4B 3 2
Example 12 4B 16 3
Example 13 3B 24 37
Example 14 1B 32 8
According to experimental results, the adhesion force between the PVC film and the coating on the PVC pre-coating film is improved by matching the adhesion bottom layer and the elastic bottom layer with the PVC flexible film material, and the problems of whitening, cracking, yellowing and the like cannot be caused when the PVC pre-coating film is subsequently applied to a PVC floor and is formed by high-temperature pressing on the PVC floor.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.

Claims (8)

1. The PVC pre-coating film is characterized by comprising a PVC transparent film layer and a radiation curing coating from bottom to top, wherein the radiation curing coating sequentially comprises an adhesion primer layer, an elastic primer layer, a functional layer and a finish paint layer from bottom to top;
the preparation raw materials of the primer layer comprise 2-10 parts of bifunctional polyurethane acrylate resin, 1-5 parts of vinyl chloride-vinyl acetate copolymer, 30-40 parts of bifunctional acrylate monomer, 30-50 parts of solvent and 0.1-1 part of initiator;
the solvent is butyl acetate;
the elastic primer layer is prepared from 30-60 parts of bifunctional polyurethane acrylate resin, 20-40 parts of bifunctional acrylate monomer, 10-15 parts of monofunctional acrylate and 1-5 parts of initiator;
the monofunctional acrylate is isobornyl acrylate and acryloyl morpholine; the weight ratio of isobornyl acrylate to acryloyl morpholine is 1: (0.3 to 0.8);
the initiators are all (2,4, 6-trimethylbenzoyl) diphenyl phosphine oxide.
2. The PVC precoating film according to claim 1, wherein the difunctional acrylate monomer is selected from any one or a combination of more of 1, 6-hexanediol diacrylate, neopentyl glycol diacrylate, dipropylene glycol diacrylate, tripropylene glycol diacrylate.
3. The PVC precoat film according to any one of claims 1 to 2, wherein the relative molecular weight of the difunctional urethane acrylate resin is greater than 3000; the preparation raw materials of the difunctional urethane acrylate resin comprise polyol, isocyanate and hydroxyl-containing acrylate monomer; wherein the molar ratio of the polyol to the isocyanate is 1: 2 to 5.
4. The PVC precoating film according to claim 3, wherein the polyol comprises a component A polyol and a component B polyol, the component A having a relative molecular weight of 500 to 10000; the relative molecular weight of the component B is 450-30; the molar ratio of the component A to the component B is (1-3): 1.
5. the PVC precoat film according to claim 3, wherein the polyol of the A-component has the formula OH-R3-COO-R1-COO-R2-OH, and R3、R1、R2Selected from any group; the B component polyalcohol is selected from any one or more of 1, 4-butanediol, 1, 4-cyclohexanedimethanol, hydroxyethylated bisphenol A, ethylene glycol, propylene glycol, hexanediol, p-phenylene glycol, neopentyl glycol and diethylene glycol.
6. The PVC precoat coating film according to claim 3, wherein the hydroxyl-containing acrylate monomer is selected from any one or a combination of more of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxybutyl acrylate, methyl hydroxyacrylate, hydroxypropyl methacrylate.
7. The PVC precoating film according to claim 1, wherein the curing radiation of the adhesion primer layer and the elastic primer layer is LED-UV curing.
8. A method for preparing the PVC pre-coating film according to any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) respectively and uniformly stirring the preparation raw materials of the adhesion primer layer and the elastic primer layer by using a dispersion kettle to obtain a paint finished product;
(2) then, uniformly coating the primer layer on the surface of the PVC transparent film layer by using a roller coater;
(3) uniformly coating the elastic primer layer on the surface of the primer layer by using a roller coater, and carrying out LED-UV curing;
(4) coating the functional layer on the surface of the elastic primer layer uniformly by using a roller coater, and carrying out LED-UV curing
(5) And (4) making a finish coat on the surface of the functional layer, and performing radiation curing to obtain the PVC pre-coating film.
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