CN1597304A - Preparation method of self-adhesive polyethylene base protection film - Google Patents
Preparation method of self-adhesive polyethylene base protection film Download PDFInfo
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- CN1597304A CN1597304A CN 200410011040 CN200410011040A CN1597304A CN 1597304 A CN1597304 A CN 1597304A CN 200410011040 CN200410011040 CN 200410011040 CN 200410011040 A CN200410011040 A CN 200410011040A CN 1597304 A CN1597304 A CN 1597304A
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Abstract
A process for preparing self-adhesive polyethene-base protecting film includes such steps as extruding out basic film, middle layer and self-adhesive layer, and blowing film to obtain a composite film. Said basic film is prepared from low-density polyethene and low-density linear polyethene. Said middle layer is prepared from the polyethene of basic film and ethene-vinyl acetate. Said self-adhesive layer is prepared from 6 chemicals including ethene-vinyl acetate, polyethene of basic film, dioctyl adiptate, etc.
Description
Technical field
The invention belongs to the preparation method of tack polyvinyl diaphragm.
Background technology
Many products are arranged; decorating paint film from little mobile phone screen outside big car all needs to protect, with prevent store and transportation middle-ultraviolet lamp, atmosphere in acid rain, birds droppings, small insect, microorganism and seawater in salt fog etc. to erosion that these products were caused.Diaphragm is born for adapting to this market demand.Another function of diaphragm be prevent the protected object surface store and transportation in contaminatedly make dirty, scratch or cause scratch.Many household electrical appliance, top-grade furniture, ornament materials are also all used this diaphragm protection.
The tack diaphragm is normally by the two-layer above composite membrane that (containing two-layer), macromolecular material was formed.Its basement membrane can be polyethylene (PE), polypropylene (PP), and polyvinyl chloride (PVC), homopolymers such as polyester also can be blending type or compound high polymer.Basement membrane does not have viscosity, and they have mechanical property preferably, can be used as the matrix of diaphragm.The tack coat of diaphragm mainly provides attachment function, and this adhesive property depends primarily on the composition and the preparation method of binding resin.With the production method classification, diaphragm can be divided into three major types: the gluing method; Double-deck or multi-layer co-extruded blown film and The tape casting.
The diaphragm of gluing type be by polyethylene, polypropylene, polyvinyl chloride, ethylene-vinyl acetate copolymer (EVA), they blend or they make basement membrane with all kinds of elastomeric blends, and then on basement membrane, scribble one or more layers tack coat with attachment function.The macromolecule of forming tack coat mainly has polyisobutene, polyacrylic acid and ester class thereof, ethylene-vinyl acetate copolymer, polyurethane (PU), elastomer etc., it wherein mainly is first three class, be mainly used in aluminium-plastic panel, building and ornament materials, dustproof, the anti-scratch, anticorrosion of antitheft door.But this class material all has lower glass transition temperature, lower molecular weight, and therefore, often binding resin easily shifts and remains on the surface of protected body after tearing diaphragm.This shortcoming is definitely unallowable in high-grade protection process.The whole lacquer painting diaphragm of car also can adopt the gluing method to produce.By regulating the molecular weight of binding resin, the ratio of regulating low-molecular-weight and high molecular weight resin can reach binding resin and not shift and have higher viscosity, makes high performance coating protective film.Another shortcoming of filming be in the production process with an organic solvent, can pollute, impair workers'health and the fire safety problem is arranged environment.
Adopt method two-layer or multilayer melt coextrusion film blowing to prepare diaphragm and belong to environmental protection technology, almost do not pollute in the whole process of production.But technical difficulty will be much larger than filming.Wherein successfully solving three conflicting factor restrictions is key technologies.The first, must guarantee that the tack coat of diaphragm will have enough viscosity, with enough adhesion strengths are arranged between the protection body.The second, binding resin can not shift on by protection body, and is after diaphragm tears, no any residual on the anti-mask of quilt.The 3rd, the film bubble can not stick together through still separating after the herringbone folder in the blown film process, with the continuity that guarantees to produce.In order to satisfy this 3 requirements, binding resin must have enough melt strengths, melt viscosity and melt elasticity.Binding resin should have enough viscosity, and part low molecular weight substance, tackifier etc. should be arranged.But, must have again between high molecular weight material that enough melt strengths, melt elasticity are provided and these components and have good compatible.
Basement membrane resin and binding resin must have good compatibility between the two, and enough interlaminar bonding intensity is arranged, to prevent that tack coat is with peeling off between the basement membrane and coming off.Be divided into the diaphragm of high temperature subsides and the diaphragm that room temperature is pasted again according to this class diaphragm of serviceability temperature.The former can be on being attached to by protection body about 50 ℃, and the latter can at room temperature use.
Diaphragm is called adhesive protecting film (Self-adhesive protective film) again, from mucous membrane (Self-adhesive film), and multiple-level surface diaphragm (multilayer surfaceprotective film) etc.
Surface protection film described in the European patent EP 0592913 (Surfaceprotection film) is made by undersaturated polar comonomers and alpha olefin copolymer.What EP 0519278 and US 5601917 described is polyisobutene (PIB) diaphragm.US 6319353 has described the alpha olefin copolymer diaphragm, and its performance is more outstanding.It is cold drawn from mucous membrane (cold-stretchable, self-adhesive film) that U.S. Pat 4624991 is described, and comprised ethylene-alpha-olefin copolymer, polyisobutene (PIB), random polypropylene (aPP), butadiene rubber (PB) and brombutyl adopt and extrude the production of blown film method.French Patent (FRP) French Patent 2277852 from mucous membrane by thermoplastic elastomer (TPE), polyolefin, the carboxylic acid of partial esterification and polyalcohol, polybutadiene (PB) or polyisobutene are formed.
The existing patented technology of analysis-by-synthesis, the high polymer that is used to make the diaphragm binding resin mainly contains two big classes, and a class is to be the nonpolar binding agent of representative with polyisobutene (PIB); Another kind of is the polarity binding agent of polyester-type, comprises polyacrylic acid and ester class thereof and ethene-polyvinyl acetate copolymer (EVA).
Polyisobutene and butyl rubber (containing chlorination butyl and brombutyl) have excellent tack and ageing-resistant performance; be suitable for many application scenarios, change more steadily and slightly having a declining tendency by its peeling forces of diaphragm of these polymer manufacture in time.Polyacrylate is the olefin polymer that is used for contact adhesive of a quasi-representative, and it has excellent durability, and good surface appearance and bigger cohesive force are development in recent years pressure-sensitive adhesives the most rapidly.Common this adhesive is made up of polyacrylic acid long-chain fat adoption ester and polyacrylic acid short-chain fat adoption ester blend.The former has lower softening point and lower glass transition temperature, and to adhesion property, the resistance to low temperature contribution is bigger.The latter has higher softening point and high glass transition, is used to increase the cohesive strength of adhesive.If contain reactive comonomer in the adhesive, cohesive strength is further improved by cross-linking reaction.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of tack polyvinyl diaphragm.
It is the basement membrane resin that the present invention selects low density polyethylene (LDPE) (LDPE) and LLDPE (LLDPE) mixture, because low density polyethylene (LDPE) (LDPE) has excellent film forming, LLDPE (LLDPE) can increase the mechanical properties such as intensity of low density polyethylene (LDPE) (LDPE).Being mixed with basement membrane by this two resinoid can make diaphragm have mechanical property preferably.The intermediate layer is that the ethylene-vinyl acetate copolymer (EVA) of 18wt% is formed by basement membrane resin and vinyl acetate content, can ensure effectively that it is with the secure bond between basement membrane and the self-adhesive layer and help the tackify of self-adhesive layer.The composition of self-adhesive layer is a core content of the present invention.Its main component is ethylene-vinyl acetate copolymer (EVA), and when the content of vinylacetate (VA) in ethylene-vinyl acetate copolymer (EVA) was 28-33wt%, ethylene-vinyl acetate copolymer itself just had tack.The purpose that adds the basement membrane polyvinyl resin of 10-20 part in self-adhesive layer is the viscosity of regulating self-adhesive layer, and self-adhesive layer is not easily separated when preventing blown film, in addition, can also increase the mechanical property of self-adhesive layer.The polyethylene of maleic anhydride graft and acrylic acid-grafted polyethylene provide acid anhydrides and carboxyl in the self-adhesive layer, and the former meets water also can become carboxyl.This class binding resin is different from ethylene-vinyl acetate copolymer (EVA), and many metals, hydroxyl isopolarity group object surfaces are had fine cementation and protective effect.Usually the adhesive property between diaphragm and the protected body depends on three processes, at first is that two kinds of materials are wetting at the interface, secondly is the phase counterdiffusion, is at last strong interaction or chemical reaction combination take place.According to the character of protected body, the composition of design, adjusting self-adhesive layer can strengthen the adhesion strength between diaphragm and the protected body.The tackifier dioctyl adipate can be separated out on the surface to film with standing time after film forming, thereby diaphragm is increased with the growth viscosity of standing time.Antifoggant sorbierite oleic acid monoester can increase the transparency of diaphragm.
Diaphragm of the present invention is to be made by three-layer co-extruded blowing, and the thickness of each layer respectively accounts for 1/3rd, can at room temperature paste.Wherein basement membrane is made up of with the ratio mixing of 30/70-70/30wt% low density polyethylene (LDPE) and linear low density polyethylene resin.The ethylene-vinyl acetate copolymer that the intermediate layer is 18wt% by basement membrane polyvinyl resin and vinylacetate (VA) content of 10/90-90/10wt% mixes to be formed.Self-adhesive layer is ethylene-vinyl acetate copolymer 80-100 part of 28-33wt% by vinylacetate (VA) content by weight, basement membrane polyvinyl resin 10-20 part, maleic anhydride (MA) grafted polyethylene 1-10 part (maleic anhydride content is 1-3wt%), acrylic acid (AA) grafted polyethylene 1-10 part (wherein acrylic acid-grafted content is 0.5-1.5wt%), tackifier dioctyl adipate 1-2 part, antifoggant sorbierite oleic acid monoester 0.5-1.0 part is formed.
Major part is commercial blown film grade resins in the above-mentioned resin.Wherein low density polyethylene (LDPE), LLDPE, maleic anhydride grafted polyethylene and acrylic acid-grafted poly melt flow index are 0.7-1.5g/10min; Vinyl acetate content is that the melt flow index of the ethylene-vinyl acetate copolymer of 18wt% is 2.0-3.0g/10min; Vinyl acetate content is that the melt flow index of the ethylene-vinyl acetate copolymer of 28-33wt% is 5.0-6.0g/10min.For example, low density polyethylene (LDPE) (LDPE) can be but be not limited to the 18D that Daqing petrochemical is produced that its melt flow index is 1.5g/10min.LLDPE (LLDPE) can be but be not limited to 1001 XV or the LL1201 of Exxon company that their melt flow index is between the 0.75-1.0g/10min.Vinyl acetate content is that the ethylene-vinyl acetate copolymer (EVA) of 18wt% can be but is not limited to the EVA18-3 that Beijing Organic Chemical Plant produces, and its melt flow index is 3.0g/10min.Vinylacetate (VA) content is that the ethylene-vinyl acetate copolymer (EVA) of 28-33wt% can be selected but is not limited to Mitsui, Korea S's Samsung, and the product of SUMITOMO CHEMICAL chemistry, melt flow index is 5.0-6.0g/10min.Tackifier and antifoggant are chemically pure reagent.Maleic anhydride grafted polyethylene and acrylic acid connect polyethylene all with reference to Journal of materialsscience, 2002,37, the prior art of delivering on the 1215-1221 is made by oneself by the present inventor, polyethylene wherein is low density polyethylene (LDPE) (LDPE), as the 18D of Daqing petrochemical production.
The diaphragm that makes according to said components, composition and preparation method has excellent tack, good mechanical performance, the higher transparency, easily processing forming and can not shifting on protected body.
The specific embodiment
Embodiment 1:
Get 70 parts of low density polyethylene (LDPE) (LDPE) 18D that Daqing petrochemical produces, 30 parts of mixing of LLDPE (LLDPE) 1001 XV that Exxon company produces are as the basement membrane resin of diaphragm.Get 90 parts of above-mentioned basement membrane resin compounds, vinyl acetate content is the intermediate layer resins of 10 parts of mixing of ethylene-vinyl acetate copolymer (EVA) EVA18-3 resin of 18wt% as diaphragm.Get 10 parts of basement membrane hybrid resins; vinyl acetate content is that 28wt%, melt flow index are 100 parts of ethylene-vinyl acetate copolymer (EVA) resins of 5.0g/10min; maleic anhydride content is 1 part of the polyethylene of the maleic anhydride graft of 1wt%; acrylic acid-grafted content is 1 part of the acrylic acid-grafted polyethylene of 0.5wt%; 1 part of tackifier dioctyl adipate; 0.5 part of antifoggant sorbierite oleic acid monoester mixes as diaphragm self-adhesive layer resin.
Three kinds of hybrid resins are by three extruder co-extrusions, and blown film obtains three layers of composite protection film.Extruder in three coextrusion blown film units all is single screw extrusion machines of 30: 1 of draw ratio, and each extruder is 5 sections heating, and the temperature from head to 5 sections of charge doors is set to 190 ℃, 180 ℃, and 170 ℃, 160 ℃ and 100 ℃.
The diaphragm longitudinal tensile strength is greater than 22MPa, and transverse tensile strength is greater than 18MPa, and the elongation at break of vertical and horizontal is all greater than 500%.The self-adhesive layer of diaphragm has enough viscosity, can be used for glass, the surface protection of polycarbonate plate (sheet) material, polyester sheet (sheet) material, polyvinyl chloride panel (sheet) material, building stone, lacquer painting metallic plate etc.
Embodiment 2:
Get 70 parts of low density polyethylene (LDPE) (LDPE) the 1F7B resins that Yanshan Petrochemical is produced, melt flow index is 0.7g/10min, 30 parts of basement membrane resins of LLDPE (LLDPE) LL149 (Korea S SK) as diaphragm.Get 10 parts of above-mentioned basement membrane resin compounds, it is that 18wt%, melt flow index are 90 parts of mixing of ethylene-vinyl acetate copolymer (EVA) 18-2 resin of 2.0g/10min that Mitsui company produces vinyl acetate content, as the intermediate layer of diaphragm.Get 20 parts of above-mentioned basement membrane resin compounds; vinyl acetate content is that 28wt%, melt flow index are 100 parts of ethylene-vinyl acetate copolymer (EVA) resins of 5.0g/10min; maleic anhydride content is 3 parts of the maleic anhydride grafted polyethylenes of 2.0wt%; acrylic acid-grafted content is 3 parts of the acrylic acid-grafted polyethylene of 1.0wt%; 1 part of tackifier dioctyl adipate; 0.5 part of antifoggant sorbierite oleic acid monoester mixes as diaphragm self-adhesive layer resin.
Three kinds of hybrid resins are by three extruder co-extrusions, and blown film obtains three layers of composite protection film.Extruder in three coextrusion blown film units all is single screw extrusion machines of 30: 1 of draw ratio, and each extruder is 5 sections heating, and the temperature from head to 5 sections of charge doors is set to 190 ℃, 180 ℃, and 170 ℃, 160 ℃ and 100 ℃.
The diaphragm longitudinal tensile strength is greater than 22MPa, and transverse tensile strength is greater than 18MPa, and the elongation at break of vertical and horizontal is all greater than 500%.The self-adhesive layer of diaphragm has enough viscosity, can be used for glass, the surface protection of polycarbonate plate (sheet) material, polyvinyl chloride panel (sheet) material, polyester sheet (sheet) material, building stone, lacquer painting metallic plate etc.
Embodiment 3:
Get 30 parts of low density polyethylene (LDPE) (LDPE) 18D that Daqing petrochemical produces, 70 parts of mixing of product LLDPE (LLDPE) 1001 XV of Exxon company are as the basement membrane resin of diaphragm.Get 50 parts of above-mentioned basement membrane resin compounds, vinyl acetate content is the intermediate layer resins of 50 parts of mixing of ethylene-vinyl acetate copolymer (EVA) 18-3 resin of 18wt% as diaphragm.Get 10 parts of basement membrane hybrid resins; vinyl acetate content is that 33wt%, melt flow index are 80 parts of ethylene-vinyl acetate copolymer (EVA) resins of 6.0g/10min; maleic anhydride content is 10 parts of the maleic anhydride grafted polyethylenes of 3.0wt%; acrylic acid-grafted content is 3 parts of the acrylic acid-grafted polyethylene of 1.5wt%; 2 parts of tackifier dioctyl adipates; 1 part of antifoggant sorbierite oleic acid monoester mixes as diaphragm self-adhesive layer resin.
Three kinds of hybrid resins are by three extruder co-extrusions, and blown film obtains three layers of composite protection film.Extruder in three coextrusion blown film units all is single screw extrusion machines of 30: 1 of draw ratio, and each extruder is 5 sections heating, and the temperature from head to 5 sections of charge doors is set to 190 ℃, 180 ℃, and 170 ℃, 160 ℃ and 100 ℃.
The diaphragm longitudinal tensile strength is greater than 22MPa, and transverse tensile strength is greater than 18MPa, and the elongation at break of vertical and horizontal is all greater than 500%.The self-adhesive layer of diaphragm has enough viscosity, can be used for glass, the surface protection of polycarbonate plate (sheet) material, polyester sheet (sheet) material, polyvinyl chloride panel (sheet) material, building stone, lacquer painting metallic plate etc.
Embodiment 4:
Get 30 parts of low density polyethylene (LDPE) (LDPE) 18D that Daqing petrochemical produces, 70 parts of mixing of product LLDPE (LLDPE) 1001 XV of Exxon company are as the basement membrane resin of diaphragm.Get 50 parts of above-mentioned basement membrane resin compounds, vinyl acetate content is 50 parts of ethylene-vinyl acetate copolymer (EVA) the 18-3 resins of 18wt%, mixes the intermediate layer resin as diaphragm.Get 10 parts of basement membrane hybrid resins; vinyl acetate content is that 33wt%, melt flow index are 80 parts of ethylene-vinyl acetate copolymer (EVA) resins of 6.0g/10min; maleic anhydride content is 3 parts of the maleic anhydride grafted polyethylenes of 3.0wt%; acrylic acid-grafted content is 10 parts of the acrylic acid-grafted polyethylene of 1.5wt%; 2 parts of tackifier dioctyl adipates; 1 part of antifoggant sorbierite oleic acid monoester mixes as diaphragm self-adhesive layer resin.
Three kinds of hybrid resins are by three extruder co-extrusions, and blown film obtains three layers of composite protection film.Extruder in three coextrusion blown film units all is single screw extrusion machines of 30: 1 of draw ratio, and each extruder is 5 sections heating, and the temperature from head to 5 sections of charge doors is set to 190 ℃, 180 ℃, and 170 ℃, 160 ℃ and 100 ℃.
The diaphragm longitudinal tensile strength is greater than 22MPa, and transverse tensile strength is greater than 18MPa, and the elongation at break of vertical and horizontal is all greater than 500%.The self-adhesive layer of diaphragm has enough viscosity, can be used for glass, the surface protection of polycarbonate plate (sheet) material, polyester sheet (sheet) material, polyvinyl chloride panel (sheet) material, building stone, lacquer painting metallic plate etc.
Embodiment 5:
Get 70 parts of low density polyethylene (LDPE) (LDPE) 18D that Daqing petrochemical produces, 30 parts of mixing of product LLDPE (LLDPE) 1001 XV of Exxon company are as the basement membrane resin of diaphragm.Get 50 parts of above-mentioned basement membrane resin compounds, vinyl acetate content is 50 parts of mixing of ethylene-vinyl acetate copolymer (EVA) 18-3 resin of 18wt%, as the intermediate layer resin of diaphragm.Get 10 parts of basement membrane hybrid resins; vinyl acetate content is that 28wt%, melt flow index are 80 parts of ethylene-vinyl acetate copolymer (EVA) resins of 5.0g/10min; maleic anhydride content is 2 parts of the maleic anhydride grafted polyethylenes of 2.0wt%; acrylic acid-grafted content is 5 parts of the acrylic acid-grafted polyethylene of 0.7wt%; 1.6 parts of tackifier dioctyl adipates; 0.5 part of antifoggant sorbierite oleic acid monoester mixes, as diaphragm self-adhesive layer resin.
Three kinds of hybrid resins are by three extruder co-extrusions, and blown film obtains three layers of composite protection film.Extruder in three coextrusion blown film units all is single screw extrusion machines of 30: 1 of draw ratio, and each extruder is 5 sections heating, and the temperature from head to 5 sections of charge doors is set to 190 ℃, 180 ℃, and 170 ℃, 160 ℃ and 100 ℃.
The diaphragm longitudinal tensile strength is greater than 22MPa, and transverse tensile strength is greater than 18MPa, and the elongation at break of vertical and horizontal is all greater than 500%.The self-adhesive layer of diaphragm has enough viscosity, can be used for glass, the surface protection of polycarbonate plate (sheet) material, polyester sheet (sheet) material, polyvinyl chloride panel (sheet) material, building stone, lacquer painting metallic plate etc.
Claims (7)
1, a kind of preparation method of tack polyvinyl diaphragm is characterized in that being made up of following material in weight fraction: basement membrane is mixed with the ratio of 30/70-70/30wt% by low density polyethylene (LDPE) and LLDPE and forms; The intermediate layer is made up of basement membrane polyethylene and the ethylene-vinyl acetate copolymer mixing of 10/90-90/10wt%; Self-adhesive layer is by weight by ethylene-vinyl acetate copolymer 80-100 part, basement membrane polyethylene 10-20 part, maleic anhydride grafted polyethylene 1-10 part, acrylic acid-grafted polyethylene 1-10 part, tackifier dioctyl adipate 1-2 part, antifoggant sorbierite oleic acid monoester 0.5-1.0 part is formed.
2,, it is characterized in that vinyl acetate content is 18wt% in the used ethylene-vinyl acetate copolymer in described diaphragm intermediate layer as the preparation method of claims 1 described tack polyvinyl diaphragm.
3,, it is characterized in that vinyl acetate content is 28-33wt% in the used ethylene-vinyl acetate copolymer of described diaphragm self-adhesive layer as the preparation method of claims 1 described tack polyvinyl diaphragm.
4, as the preparation method of claims 1 described tack polyvinyl diaphragm; it is characterized in that used low density polyethylene (LDPE), LLDPE, ethylene-vinyl acetate copolymer; maleic anhydride grafted polyethylene, acrylic acid-grafted polyvinyl resin is the blown film grade resins.Wherein low density polyethylene (LDPE), LLDPE, maleic anhydride grafted polyethylene and acrylic acid-grafted poly melt flow index are 0.7-1.5g/10min; Vinyl acetate content is that the melt flow index of the ethylene-vinyl acetate copolymer of 18wt% is 2-3g/10min; Vinyl acetate content is that the melt flow index of the ethylene-vinyl acetate copolymer of 28-33wt% is 5.0-6.0g/10min.
5,, it is characterized in that maleic anhydride content is 1-3wt% in the used maleic anhydride grafted polyethylene as the preparation method of claims 1 described class tack polyvinyl diaphragm.
6,, it is characterized in that acrylic acid-grafted content is 0.5-1.5wt% in the used acrylic acid-grafted polyethylene as the preparation method of claims 1 described class tack polyvinyl diaphragm.
7, as the preparation method of claims 1 described class tack polyvinyl diaphragm; it is characterized in that the extruder in three used coextrusion blown film units all is single screw extrusion machines of 30: 1 of draw ratio; each extruder is 5 sections heating; temperature setting from head to 5 sections of charge doors is respectively 190 ℃; 180 ℃; 170 ℃, 160 ℃ and 100 ℃.
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Assignee: CHANGCHUN ZHONGKE YINGHUA SPECIAL MATERIAL CO.,LTD. Assignor: CHANGCHUN INSTITUTE OF APPLIED CHEMISTRY CHINESE ACADEMY OF SCIENCES Contract fulfillment period: 2006.4.27 to 2011.4.26 Contract record no.: 2009220000082 Denomination of invention: Preparation method of self-adhesive polyethylene base protection film Granted publication date: 20090610 License type: Exclusive license Record date: 20091104 |
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