Composition extruded jointly with poly(vinylidene fluoride)

FIELD: polymer materials.

SUBSTANCE: composition contains, wt %: vinylidene fluoride 20-40, methyl methacrylate homopolymer or copolymer, acryl elastomer 5-18, and UV-absorbing substance 1-4. Invention also discloses jointly extruded films (options) and substrates covered by these films. Invention enables preparing composition with not rising UV-absorbing substances and manufacturing films showing high mechanical strength and providing high-quality adhesion to substrate while being resistant to radiation.

EFFECT: improved consumer's properties of films.

14 cl, 7 ex

 

The technical field

PVP (polyvinylidene fluoride) is used to protect items and materials due to its high atmospheric stability, resistance to radiation and chemical products. In addition, its value lies in the fact that it attaches to the surface gloss and scratch resistant. Therefore, the film of PVF cover various substrates. However PVP has a very low adhesion to most substrates and, therefore, there is a need to strike between PVP and substrate adhesive composition. The present invention relates to such a composition.

Mainly this song ekstragiruyut together with PVP to obtain a two-layer film, after which the specified film is fixed on the substrate, for example, by hot pressing. You can also place a two-layer film in a form, with a layer PVP will be on the wall of the form, and then enter in the form the substrate in the molten state. You can also, depending on the type of substrate together to ekstradiroval PVP adhesive composition and the substrate in order to directly obtain a substrate coated with PVP, and the adhesive composition will be between PVP and the substrate.

The prior art and the technical problem.

In the patent GB 1578517 described ABS, covered with a film of PVF, the polyurethane layer may be between PVP the ABS.

In the patent US 4226904 described PMMA coated film of PVF. To improve the adhesion to the film of PVF put a solution of PMMA in dimethylformamide and, after evaporation of the solution film of PVF pressed on PMMA.

In the patent US 4415519 described substrate of ABS or PVC-coated film of PVF, when the adhesive is located between PVP and substrate. As the adhesive, you can use the mixture, expressed in weight percent: 40% PMMA, 30% PVP and 30% ABS, or a mixture, expressed in weight percent: 30% PMMA, 40% polyacrylic derivative and 30% ABS.

In the patent US 4364886 described substrate of ABS or unsaturated polyester, covered with a film of PVF, when this adhesive composition is located between PVP and substrate. As the adhesive composition, a mixture, expressed in weight percent: 30% PMMA, 40% acrylic elastomer and 30% ABS.

In the patent US 5242976 described composition, together extrudable with PVP designed for adhesion to the substrates. As the composition of a mixture, expressed in weight percent: from 27 to 50% PMMA, from 17.5 to 36.5% PVP and from 25 to 47,45% acrylic elastomer.

None of the above none mentions the presence in the adhesive composition additives against ultraviolet radiation (UV).

In the patent EP 733475 B1 described substrates covered PVF; sequentially consists of a substrate, clease what about the layer, layer PVP protected from UV and visible radiation, and a layer of PVF. To protect the layer PVP in PVP injected substance selected from metal oxides, pigments and benzophenone. In the examples we are talking only about PVP containing 15 weight % of zinc oxide.

In the patent US 5256472 described two-layer film containing a first layer composed mainly of PVP and fewer PMMA, and a second layer providing adhesion to the substrate. Specified adhesive layer consists expressed in parts by weight: from 50 to 95, preferably from 70 to 90) parts of PMMA, from 5 to 50 (preferably 10 to 30) parts PVF and from 0.1 to 15 parts material that absorbs UV. It is clarified that the presence of substances absorbing UV, is necessary because this adhesive layer is sensitive to radiation and in the absence of a material that absorbs UV glue is destroyed, and a layer composed mainly of PVP, unstuck from the substrate. PMMA denotes homopolymers of methyl methacrylate or copolymers of methyl methacrylate with copolymerization monomer, and a mixture with kucukkale (acrylate rubber), but does not specify the ratio of PMMA and rubber. It is clarified that if the amount of PMMA is less than 50 parts, substances that absorb UV, come to the surface. It was found, although in this paper it is not specified that such withdrawal on the surface of adverse what about the effect on transparency film and cause peeling. In addition, such films do not have mechanical resistance, so they are difficult to use. Necessary is the presence of the elastomer in the adhesive layer, because in the absence of elastomer bonding is not quality, and the film has no mechanical strength. According to the above-mentioned document US 5242976 his number should be from 25 to 47,45%, but these amounts can cause insufficient resistance to radiation.

The applicant was created composition extrudable together with PVP, in which there is an exit to the surface of substances that absorb UV, in which a two-layer film of PVF/together extrudable composition has a high mechanical strength, which provides high adhesion layer PVF to the substrate and is resistant to radiation.

Brief description of the invention

The present invention relates to a composition extrudable together with PVP containing:

20-40 parts PVF,

40-60 parts of PMMA,

5-18 parts of acrylic elastomer,

1-4 part material that absorbs UV,

the total amount is 100 parts.

The invention concerns also co-extrudable films, consisting of:

layer together extrudable compositions mentioned above (also referred to as an adhesive layer) and with it connected the th,

layer-based PVP containing as main components from 50 to 100 parts PVF and correspondingly from 50 to 0 parts of PMMA (more briefly this layer is also referred to as "layer PWF").

In accordance with a second embodiment of the invention, the layer PVP consists of 2 layers:

one is jointly extrudable layer and contains as main components, from 50 to 90 parts PVF and correspondingly from 50 to 10 parts of PMMA,

another (also called outer layer) contains as main components from 75 to 100 parts PVF and correspondingly from 25 to 0 parts of PMMA.

These films have mechanical properties sufficient that they are easy to handle, apply and use them as cover, transparent for visible light, but protects from ultraviolet radiation.

The invention also applies to substrates coated with such a film, and together extrudable composition (adhesive composition) is located on the substrate.

Detailed description of the invention.

PVP denotes homopolymers of vinylidenefluoride (VF) and copolymers of vinylidenefluoride (VF), preferably containing at least 50 weight % VF and at least one other polymerized together with VP monomer. Mainly comonomer is fluoridated, it can be selected, for example the EP, from winifrida; trichoroethylene (WHF); chlorotrifluoroethylene (HTFA); 1,2-defloration; tetrafluoroethylene (TPV); HEXAFLUOROPROPYLENE (HFP); simple PERFLUORO(alkylvinyl) esters, such as Perfora(metilidinovy)ether (PMVE); Perfora(ethylenically)ether (PAVE), perfluro(propylvinyl)ether (PPVE); PERFLUORO(1,3-dioxide); Perfora(2,2-dimethyl-1,3-dioxide) (SDA). Preferably possible comonomer choose from chlorotrifluoroethylene (HCFA), HEXAFLUOROPROPYLENE (HFP), trichoroethylene (WHF) and tetrafluoroethylene (TPV).

Mainly PVP has a viscosity of 100 PA·s to 2000 PA·s, and the viscosity is measured at 230°when the gradient of the shear stress equal to 100 sec-1using a capillary rheometer.

PMMA denotes homopolymers of methyl methacrylate and copolymers containing at least 50 mass % of methyl methacrylate. As an example of co monomer include, for example, alkyl(meth)acrylates, Acrylonitrile, butadiene, styrene, isoprene. Examples of the alkyl(meth)acrylates described in KIRKOTHMER, Encyclopedia of chemical technology, edition 4, volume 1, str-293 and volume 16, str-478. Mainly PMMA may contain from 0 to 20 mass % and preferably from 5 to 15% of methyl acrylate and/or ethyl acrylate. PMMA can be functionalized, i.e. it may contain, for example, acid groups, acid chloride acid, alcohol, anhydride. These gruppioni be administered by graft copolymerization or copolymerization. Mainly it is an acid group introduced with the co monomer is acrylic acid. Two neighboring acrylic acid groups can degidratirutego obtaining anhydride. The number of groups can be from 0 to 15 mass % PMMA containing possible groups.

MVI (melt volume index or the volume ratio of fluidity in the molten state) PMMA can be from 2 to 15 cm3/10 min, measured at 230°under load, equal to 3.8 kg

Acrylic elastomer means elastomers on the basis of at least one monomer selected from Acrylonitrile, alkyl(meth)acrylate and copolymers core shell (core-surface layer). Copolymer type core-surface layer has the form of fine particles consisting of a core consisting of elastomer and at least one thermoplastic surface layer, the particle size, usually less than one micron and is preferably from 50 to 300 nm.

As an example, the kernel can be called the homopolymers of isoprene or butadiene, copolymers of isoprene, containing not more than 30 molar % of vinyl monomer, and copolymers of butadiene containing not more than 30 molar % of vinyl monomer. The vinyl monomer may be styrene, alkylthiol, Acrylonitrile or alkyl(meth)acrylate. To another family, forming the core include homopolymers of alkyl(meth)acrylate and copolym the market alkyl(meth)acrylate, containing not more than 30 molar % of a monomer selected from another alkyl(meth)acrylate and a vinyl monomer. The alkyl(meth)acrylate mainly is butyl acrylate. As the vinyl monomer may be used styrene, alkylthiol, Acrylonitrile, butadiene or isoprene. The core copolymer type core-surface layer can be made fully or partially. Just enter at least bifunctional monomers in the process of obtaining the kernel, these monomers can be selected from poly(meth)acrylic esters of polyols, such as butylene(meth)acrylate and trimethylolpropane. Other bifunctional monomers are, for example, divinylbenzene, trivinylbenzene, vinylacetat and vanillacream. You can also sew the kernel by entering it using the graft copolymerization or copolymerization of unsaturated functional monomers such as unsaturated anhydrides of carboxylic acids, unsaturated carboxylic acids and unsaturated epoxides. As example can be mentioned maleic anhydride, (meth)acrylic acid and glycidylmethacrylate.

The surface layer or layers are homopolymers of styrene, alkylthiol or methyl methacrylate or copolymers containing at least 70 molar % of one of the above monomers and at least one of SOMO of the Omer, selected from the other of the above monomers, other alkyl(meth)acrylate, vinyl acetate and Acrylonitrile. The surface layer can be functionalitywith introduction to him through graft copolymerization or as co monomer during the polymerization of unsaturated functional monomers such as unsaturated carboxylic acids and unsaturated epoxides. As example can be mentioned maleic anhydride, (meth)acrylic acid and glycidylmethacrylate. As example can be mentioned copolymers of the type a core-surface layer, the surface layer which consists of polystyrene and copolymers of the type a core-surface layer, the surface layer which consists of PMMA. There are also copolymers of the type a core, the surface layer having two surface layers, one made of polystyrene and the other, external, from PMMA. Examples of the copolymer and the method of their derivation are described in the following patents: US 4180494, US 3808180, US 4096202, US 4260693, US 3287443, US 3657391, US 4299928, US 3985704, US 5773520.

Mainly the core ranges from 70 to 90 mass % of a copolymer type core-surface layer and the surface layer is from 30 to 10%.

As an example, the copolymer can be called the copolymer (i) the core of which is between 75 and 80 parts and is in molar percent of at least 93% of butadiene, 5% styrene and 0.5 to 1% divinylbenzene, and (ii) two surface with the OYA which, having basically the same mass range from 25 to 20 parts, one internal layer is made of polystyrene and the other external, PMMA.

As other examples are copolymers having a core of poly(butyl acrylate) or of a copolymer of butyl acrylate and butadiene and the surface layer of PMMA.

All of these copolymers type a core, the surface layer is sometimes referred to as soft/hard, because their core is made of elastomer.

There are other types of copolymers type core-surface layer, such as a hard/soft/hard, this means that they are in the order specified, solid core, soft surface layer and the solid surface layer. The solid part can consist of a polymer surface layer of the above polymers such as a soft-hard and soft part can consist of a polymer core of the above polymers such as a soft-solid.

As example can be mentioned the copolymers formed in the following order:

the core of a copolymer of methyl methacrylate and ethyl acrylate,

the surface layer of a copolymer of butyl acrylate and styrene,

the surface layer of a copolymer of methyl methacrylate and ethyl acrylate.

There are also other types of copolymers type core-surface layer, such as a hard (core)/soft/semi-solid. They differ from the previous one lies in the external "on utorda" layer, which consists of two surface layers: one intermediate and the other external. The intermediate layer consists of a copolymer of methyl methacrylate, styrene and at least one monomer selected from alkylacrylate, butadiene and isoprene. The outer surface layer consists of homopolymer or copolymer PMMA.

As example can be mentioned the copolymers formed in the following order:

the core of a copolymer of methyl methacrylate and ethyl acrylate,

the surface layer of a copolymer of butyl acrylate and styrene,

the surface layer of a copolymer of methyl methacrylate, butyl acrylate and styrene,

the surface layer of a copolymer of methyl methacrylate and ethyl acrylate.

When choosing the number of the acrylic elastomer should be aware that in PMMA may already contain acrylic elastomer. Indeed, there are commercial brands of PMMA, called "shock proof", which contain high-impact acrylic modifiers, the most common type of core-surface layer. These modifiers may be present in PMMA, as they are in the process of polymerization or receive simultaneously in the process of polymerization.

Substance, absorbing UV, refers to well-known products. Such products are referred to in the patent US 526472. Mainly use benzotriazole and benzophenone. For example, you can use the Tinuvin® 213 or Tinuvin®109 and preferably Tinuvin®234 company Ciba Speciality Chemicals.

Mainly the composition extrudable together with PVP, consists of:

25-35 parts PVF,

45-55 parts of PMMA,

8-18 parts of acrylic elastomer,

2-3 pieces of material that absorbs UV,

the total amount is 100 parts.

Preferably the composition extrudable together with PVP, consists of:

30-35 parts PVF,

50-55 parts of PMMA,

8-12 pieces of acrylic elastomer,

2-3 pieces of material that absorbs UV,

the total amount is 100 parts.

Together extrudable composition can be obtained by mixing PVP, PMMA and acrylic elastomer in the molten state with the addition of substances absorbing UV. Mainly used the devices used for mixing thermoplastic substances.

In conjunction extrudable film consisting of a jointly extrudable compositions and layer PVF, the thickness of the layer PVF is preferably from 2 to 50 μm and the thickness together extrudable composition is from 10 to 100 microns.

Predominantly layer-based PVP includes as main components from 70 to 100 parts PVF and correspondingly from 30 to 0 parts of PMMA and preferably from 75 to 85 parts PVF and correspondingly from 25 to 15 parts of PMMA.

In accordance with the second is the embodiment of the invention the layer PVP consists of 2 layers:

one is jointly extrudable layer and includes as main components from 50 to 90 parts PVF and correspondingly from 50 to 10 parts of PMMA,

another (also called outer layer) includes as main components from 75 to 100 parts PVF and correspondingly from 25 to 0 parts of PMMA.

Thus, the film according to the invention are in the order of:

together extrudable layer composition according to the invention (adhesive layer),

layer located on jointly extrudable layer comprising as the main components, from 50 to 90 parts PVF and correspondingly from 50 to 10 parts of PMMA,

layer (also called outer layer)comprising as main components from 75 to 100 parts PVF and correspondingly from 25 to 0 parts of PMMA.

Mainly the outer layer contains as main components from 85 to 100 parts PVF and respectively from 15 to 0 parts of PMMA and preferably from 90 to 100 parts PVF and correspondingly from 10 to 0 parts of PMMA.

The thickness of the layer together extrudable composition is preferably from 10 to 100 μm and the thickness of each of the other layers is preferably from 2 to 50 microns.

The invention also applies to substrates coated with such a film, and together extrudable composition is on the substrate.

As examples of the substrate include:

chlorinated polymers: PVC, plasticized PVC, chlorinated PE,

polymers and copolymers containing styrene, such as ABS, SAN, PS,

saturated polyesters (PET, PBT,...) and copolymers of esters or unsaturated polyester resin(NPS),

epoxy and phenol-formaldehyde resin,

copolymers of ethylene and alkylacrylate or vinyl acetate (EMA, EVA), functionalityand or defunctionalization,

PA (polyamide) and Sopa (copolyamids), PEBA, complex polyetherimide and TPU (thermoplastic polyurethane, an abbreviation of the term Thermoplastic polyurethane),

EMU (copolymer of ethylene and vinyl alcohol),

aluminum, steel or a mixture of metals,

composite materials based on lignin,

acrylic composition (PMMA),

glass,

foam PVC, PU.

Examples.

Used the following products:

Kynar® 720: a homopolymer PVP company ATOFINA and MVI (Melt Volume Index or the volume ratio of fluidity in the molten state) 10 cm3/10 min (230°C, 5 kg)

Kynar® 740: homopolymer PVP company ATOFINA and MVI (Melt Volume Index or the volume ratio of fluidity in the molten state) 1.1 cm3/10 min (230°C, 5 kg)

OROGLAS® BS8: PMMA company ATOGLAS MVI 4.5 cm3/10 min (230°C, 3.8 kg) in granular form, containing comonomer of methyl acrylate in amounts is up to 12%.

OROGLAS® V 825 T: PMMA company ATOGLAS MVI 2.5 cm3/10 min (230°C, 3.8 kg).

Tinuvin® 109: substance, absorbing UV, type benzotriazole company Ciba Speciality Chemicals.

Tinuvin® 213: substance, absorbing UV, type hydroxyphenylacetate company Ciba Speciality Chemicals.

Tinuvin® 234: substance, absorbing UV, type hydroxyphenylacetate company Ciba Speciality Chemicals.

D320: abbreviation Durastrengh® D320 denotes the elastomer type core-surface layer of soft/hard, the core of which is a copolymer of butyl acrylate and butadiene and the surface layer consists of PMMA, the size of 80 nm, manufactured by the SES.

Paraloid® 355 KM: indicates the elastomer type core-surface layer of soft/hard, the core of which is a homopolymer of butyl acrylate and the surface layer consists of PMMA size of 150 nm, manufactured by Rhom Haas et.

In the examples, the compositions expressed in weight %.

Example 1 (according to the invention).

Two-layer film containing a layer consisting of 80% PVP COPAG 720 and 20% altuglas BS8, of a thickness of 15 μm and a binder, the thickness of 35 μm, having the following composition: COPAG 720 to 31.8%, 50.7% of altuglas BS8, 2.5% of Tinuvin 234 and 15% D320, this film has an elongation at break equal to 197%, index turbidity 14 and then after finding within 7 days in the drying chamber no outcrops were observed. This film has a property to absorb UV, eno is Noah for use on the external surfaces.

Example 2 (according to the invention).

Two-layer film containing a layer consisting of 80% PVP COPAG 720 and 20% altuglas BS8, thickness 15 μm, and a binder, the thickness of 35 μm, having the following composition: COPAG 740 - 33,6%, 53.9% of altuglas BS8, 2.5% of Tinuvin 234 and 10% D320, this film has an elongation at break equal to 210%, the index turbidity 11 and then after finding within 7 days in the drying chamber no outcrops were observed. This film has a property to absorb UV sufficient for use on the external surfaces.

Example 3 (according to the invention).

Two-layer film containing a layer consisting of 80% PVP COPAG 740 and 20% altuglas BS8, thickness 15 μm, and a binder, the thickness of 35 μm, having the following composition: COPAG 740 - 33,6%, 53.9% of altuglas BS8, 2.5% of Tinuvin 109 and 10% D320, this film has an elongation at break of 150%of the index turbidity 8 and then after finding within 7 days in the drying chamber no outcrops were observed. This film has a property to absorb UV sufficient for use on the external surfaces.

Example 4 (according to the invention).

Two-layer film containing a layer consisting of 80% PVP COPAG 740 and 20% altuglas BS8, thickness 15 μm, and a binder, the thickness of 35 μm, having the following composition: COPAG 740 - 33,6%, 53.9% of altuglas BS8, 2.5% of Tinuvin 213 and 10% D320, this film has an elongation at break of 150%of the index turbidity 6.5 and then after finding during the 7 days in the drying chamber no outcrops were observed. This film has a property to absorb UV sufficient for use on the external surfaces.

Example 5 (according to the invention).

Two-layer film containing a layer consisting of 80% PVP COPAG 740 and 20% altuglas BS8, thickness 15 μm, and a binder, the thickness of 35 μm, having the following composition: COPAG 740 - 33,6%, 53.9% of altuglas BS8, 2.5% of Tinuvin 234 and 10% D320, this film has an elongation at break of 150%of the index turbidity 6.5 and then after finding within 7 days in the drying chamber no outcrops were observed. This film has a property to absorb UV sufficient for use on the external surfaces.

Example 6 (comparative).

Two-layer film containing a layer consisting of 80% PVP COPAG 720 and 20% oroglas V825T, thickness 15 μm, and a binder, the thickness of 35 μm, having the following composition: COPAG 720 with 32.5%, 32.5 per cent of oroglas V825T, 2.5% of Tinuvin 234 and 32.5% Polaroid KM355, this film has an elongation at break of 150%of the index turbidity 15 and then after finding out within 1 day in the drying chamber was observed release to the surface. The property to absorb UV this film is insufficient for use on the external surfaces.

Example 7 (comparative).

Two-layer film containing a layer consisting of 80% PVP COPAG 720 and 20% oroglas V825T, thickness 15 μm, and a binder, the thickness of 35 μm, having the following composition: COPAG 720 with 32.5%, 32.5 per cent of oroglas V825T, 2.5% of Tinuvin 234 and 32.5% Durastrength D320, this captivity is and has elongation at break, equal to 150%, the index turbidity 15, and then after finding out within 1 day in the drying chamber was observed release to the surface. The property to absorb UV this film is insufficient for use on the external surfaces.

1. Composition extrudable together with the poly (vinylidene fluoride), consisting of

20-40 parts of poly (vinylidene fluoride),

40-60 parts polymetylmetacrylate of homopolymer or copolymer,

5-18 parts of acrylic elastomer,

1-4 parts substances absorbing UV,

the total amount is 100 parts.

2. The composition according to claim 1, containing mainly the following amounts:

25-35 parts of poly (vinylidene fluoride),

45-55 parts polymetylmetacrylate of homopolymer or copolymer,

8-18 parts of acrylic elastomer,

2-3 pieces of material that absorbs UV,

the total amount is 100 parts.

3. The composition according to claim 2, containing mainly the following amounts:

30-35 parts of poly (vinylidene fluoride),

50-55 parts polymetylmetacrylate of homopolymer or copolymer,

8-12 pieces of acrylic elastomer,

2-3 pieces of material that absorbs UV,

the total amount is 100 parts.

4. Composition according to any one of the preceding paragraphs, which is a quality acrylic elastomer used is a copolymer type core - the surface layer.

5. The composition according to claim 4 in which the copolymer type core - surface layer are selected from copolymers such as a soft/hard, hard/soft/hard and hard/soft/semi-solid.

6. Together extrudable film consisting of a layer together extrudable composition according to any one of the preceding paragraphs, directly associated with it, a layer based PVP comprising as main components from 50 to 100 parts of polyvinylidene fluoride and correspondingly from 50 to 0 parts polymetylmetacrylate of homopolymer or copolymer.

7. The film according to claim 6, in which the layer on the basis of polyvinylidene fluoride includes as main components from 70 to 100 parts of polyvinylidene fluoride and correspondingly from 30 to 0 parts polymetylmetacrylate of homopolymer or copolymer.

8. The film according to claim 7, in which the layer on the basis of polyvinylidene fluoride includes as main components from 75 to 85 parts of polyvinylidene fluoride and correspondingly from 25 to 15 parts polymetylmetacrylate of homopolymer or copolymer.

9. The film according to any one of p-8, in which the thickness of a layer of polyvinylidene fluoride is preferably from 2 to 50 μm and the thickness together extrudable composition is from 10 to 100 microns.

10. The film according to any one of p-8, in which the thickness of the layer together extrudable whom is osili is preferably from 10 to 100 μm and the thickness of each of the other layers is preferably from 2 to 50 microns.

11. Together extrudable film comprising in order from

together extrudable layer composition according to one of claims 1 to 5 (adhesive layer),

layer located on jointly extrudable layer comprising as the main components, from 50 to 90 parts of poly (vinylidene fluoride) and correspondingly from 50 to 10 parts polymetylmetacrylate of homopolymer or copolymer,

layer (also called outer layer)comprising as main components from 75 to 100 parts of polyvinylidene fluoride and correspondingly from 25 to 0 parts polymetylmetacrylate of homopolymer or copolymer.

12. The film according to claim 11, in which the outer layer comprises as main components from 85 to 100 parts of polyvinylidene fluoride and respectively from 15 to 0 parts polymetylmetacrylate of homopolymer or copolymer.

13. The film according to any one of claim 11 or 12, in which the thickness of the layer together extrudable composition is preferably from 10 to 100 μm and the thickness of each of the other layers is preferably from 2 to 50 microns.

14. Substrates, coated with a membrane on one PP-13, together with the extrudable composition is placed on the substrate.



 

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