Floor coverings

 

(57) Abstract:

The invention relates to sheet materials suitable for use in coating for floors or floor coverings. Describes a new sheet material suitable for use in flooring or floor covering in the form of a hard, wear-resistant material and containing a polymer resin in a homogeneous mixture of at least c one additive comprising an inorganic filler, these polymeric resin contains polyalkene resin having a relatively narrow limits of the molecular mass distribution (MMD), which is less than 3, a small degree of long chain branching and obtained by polymerization of at least one linear, branched or cyclic alkene having from 2 to 20 carbon atoms, with the use of one catalyst, and mentioned polyalkene also has the following properties: a) a melt index (IR) from 0.1 to 100; b) a density of from 0.86 to 0.97 in) measure the rheological properties (ORS) from 0.1 to 6.0, where ORS is an indicator of the long chain branching, as measured by comparing the shift to the right (due to the longer time relaxation the General dependence of the viscosity at zero shear on the relaxation time (both values from the equation of viscosity in the transverse direction). The technical result improved quality coatings for floors, the possibility of using graphic images. 5 C. and 23 C.p. f-crystals, 3 tab., 2 Il.

The invention relates to a sheet material suitable for use in floor covering, floor covering in the form of a hard, wear-resistant sheet material based on polymer resin, to a method for producing a sheet material suitable for use in the floor covering and the method of production of floor coverings.

More specifically, the invention relates to coatings for floors and, more particularly, to a floor in the form of a wear-resistant ceramic plate or sheet made of one or more layers of polymers, which are suitable, for example, for walking in the home and/or other conditions over an extended period of time.

Most floor of this type is based on polyvinylchloride (PVC) polymer. More specifically, the PVC polymer resin is mixed with a plasticizer, a solid or liquid (usually with other various additives, such as fillers, polymer stabilizers and excipients to improve Tehnologichesky to form sheets, using knife device or roller machine for coating, and then subjected to thermal curing, for example by heating in a furnace.

Known sheet material suitable for use in flooring or floor covering in the form of a hard, wear-resistant material and containing a polymer resin in a homogeneous mixture of at least c one additive comprising an inorganic filler (Handbook of plastic masses/Ed. by M. I. Garbara, ed. Chemistry, 1967, page 66, 73-74).

It is known to cover the floor in the form of a hard, wear-resistant sheet material based on polymer resin containing at least one layer of sheet material that contains a polymer resin in a homogeneous mixture of at least c one additive comprising an inorganic filler.with. The USSR 1789579, CL 06 D 1/00, 1993).

A method of obtaining a sheet material suitable for use in flooring or as a floor covering, comprising mixing in a mixer polymer of at least c one additive comprising an inorganic filler, when heated to melt the polymer, forming a homogeneous liquid smeester. 66, 73-74).

A known method of producing floor coverings, including multi-layer stacking of layers based polymer with at least one additive comprising an inorganic filler.

The use of polyvinyl chloride resulting from the application of chlorine leads, however, to problems concerning the environment and therefore, accordingly there is a need to create a floor-based alternative polymers. From the point of view of environmental protection are usually preferred polyalkene polymers, but the conventional polyalkene is associated with significant technological problems and, in addition, they are unsuitable for use in manufacturing equipment suitable for floorings, based on the use of technology to spread the coating and calendering technology. In addition, special issue, arising out of the use in coatings for floors usual polialcoolii polymers is that they do not provide the necessary physical properties required of the final product. More specifically, it is known that coatings for floors, obtained using the conventional polyalkene abrasion, resistance against stains and elastic recovery.

The aim of the present invention is to avoid or minimize one or more of the above disadvantages.

Currently, it is found that in the production of coatings for floors based on the use of more or less conventional application technology spread coating and calendering, can be successfully used special class polyalkenes that get through polymerization catalyzed one catalyst. In particular, polyalkene suitable in accordance with the present invention, are such polyalkene, which have a relatively narrow molecular mass distribution (MMD) and a small degree of branching with the formation of long side chain and which is produced by polymerization catalysed by a single center catalyst, however, they have the following properties:

a) a melt index (IR) from 0.1 to 100;

b) a density of from 0.86 to 0.97; and

C) measure the rheological properties (RPS) from 0.1 to 6.0, preferably from 0.4 to 5.5.

Used herein, the terms have the following specified values.

The melt index (IR) or I performance is measured in accordance with ASTM (American standard test method D-1238 (190/2.16).

Molecular mass distribution (MMD) is the ratio srednevekovoi molecular mass (MM) to srednekamennogo molecular weight (Mn) (i.e., MM/Mn).

Density is the mass (in grams) of 1 cm3resin, measured in accordance with ASTM D-792.

Figure rheological properties (ORS) is the index of branching with the formation of long side chain, measured in comparison with a shift to the right (due to the longer relaxation time) relative to the polymer resin with the zero degree of branching in the graph representing the dependence of the viscosity at zero shear on the relaxation time (both values from the equation of viscosity).

Other abbreviations used here, which are common in this area include R-side to 100 parts by weight of polymer resin (or the main component polymer resin).

Suitable polyalkene in accordance with the present invention may also include polyalkene having a relatively narrow molecular weight distribution and a low degree of branching with the formation of long side chain and is obtained by polymerization of at least one linear, resvinatrol. Polyalkene suitably includes a copolymer obtained by copolymerization of two or more alkenes, including the first linear or branched alkene having from 2 to 8 carbon atoms, and a second linear, branched or cyclic alkene having from 2 to 20 carbon atoms. This provides greater flexibility in obtaining sheet materials with specific desirable combinations of physical properties. In General can be used up to 15 mol.% this second monomer. Of course, it should be understood that when using cyclic alkenes, they may have more than one carbon ring and, thus, to include bicyclic and tetracyclic alkenes, such as norbornene and tetracyclinea.

The object of the invention is a sheet material suitable for use in the floor covering or floor covering in the form of a hard, wear-resistant material and containing a polymer resin in a homogeneous mixture of at least c one additive comprising an inorganic filler, these polymeric resin contains polyalkene resin having a relatively narrow limits of the molecular mass distribution (MMD), which is less than 3, neetling or cyclic alkene, having from 2 to 20 carbon atoms, with the use of one catalyst, and mentioned polyalkene also has the following properties:

a) a melt index (IR) from 0.1 to 100;

b) a density of from 0.86 to 0.97; and

C) measure the rheological properties (ORS) from 0.1 to 6.0, where ORS is an indicator of the long chain branching, as measured by comparing the shift to the right (due to a longer relaxation time) relative to the polymer resin with a zero degree of long chain branching (ACC) on the graph representing the dependence of the viscosity at zero shear on the relaxation time (both values from the equation of viscosity in the transverse direction).

Although regulation of specific technological characteristics, such as reduced energy consumption and/or increased speed of processing new materials of the present invention can be used excipients to improve the processing properties, feature polialcoolii resins used in the present invention, is that there is no need to use softener, resulting in greatly reduced problems in relation to the environment caused by migrates plasticizers.

Nevertheless, in such cases where it is desirable to increase the machinability, can be used a substance to improve the processing properties or plasticizer, and the advantage of the present invention in comparison with polymeric resins commonly used in coatings for floors, is that you can use a much smaller amount of plasticizer. Moreover, in a particularly preferred form of the invention to use a plasticizer or substance to improve the processing properties, including selectively curable liquid monomer system, which is essentially depolymerizing in the formation of the sheet, for example by extrusion, by spread coating or calendering used in the manufacturing process of sheet material used as a covering for floors, but then it essentially can be polimerizuet in order to obtain a material that does not contain liquid plasticizer. In General, the polymerized monomer can be used in the ratio of its number to the number of polyalkenoate resin is from 20:80 to 80:20. Additional details regarding suitable plasticizers, discussed next.

In this regard, it is in the Monomeric system together with the monomer. In such cases, it was important that there was such an initiator that can be activated selectively, i.e. in the conditions of formation of polyolefin product, the initiator is essentially inactive, but can then be activated under the appropriate conditions of polymerization or curing plasticized monomer.

In this area there are various polyalkene resin suitable for use in the materials of the present invention. In General, they are obtained by polymerization alkenovich monomers in the presence of specific catalysts, which restrict the flow of polymerization and which is known as metallocene (obtained polymers commonly referred to as the metallocene polyolefins, which for convenience also known as LRO). Such polyolefins and methods for their preparation are described in U.S. patent N 5272236.

Preferred polyalkene that may be mentioned include copolymers of ethylene-alkene having 4 to 20 carbon atoms, advantageously from 4 to 10 carbon atoms, such as butene-1 or hexene-1 or cyclic olefin such as norbornene; copolymers of propylene and-alkene having from 2 to 10 carbon atoms, such as butene-1, hexene-1 native atoms, for example butene-1, hexene-1 or cyclic olefin such as norbornene. It is preferable to use a copolymer containing up to 15 mol. % of co monomer. Moreover, it should be considered that can be used more than one monomer, i.e., can be used, for example, ternary copolymer, which use two different-alkene, each of which has 2 to 20 carbon atoms.

Suitable polyalkenoate resins, which are commercially available from Exxon Chemical Company (Exxon chemical company), USA and Dow Chemical Company (Dow chemical company), Michigan, USA, are listed in table. 1 and 2.

According to another aspect of the invention provides coverage in the form of a hard, wear-resistant sheet material based on polymer resin containing at least one layer of sheet material that contains a polymer resin in a homogeneous mixture of at least c one additive comprising an inorganic filler, these polymeric resin contains polyalkene resin having a relatively narrow limits of the molecular mass distribution (MMD), which is less than 3, a small degree of long chain branching and obtained by polymerization of at least one linear or zenaty polyalkene also has the following properties:

a) a melt index (IR) from 0.1 to 100;

b) a density of from 0.86 to 0.97; and

C) measure the rheological properties (ORS) from 0.1 to 6.0, where ORS is an indicator of the long chain branching, as measured by comparing the shift to the right (due to a longer relaxation time) relative to the polymer resin with a zero degree of long chain branching (ACC) on the graph representing the dependence of the viscosity at zero shear on the relaxation time (both values from the equation of viscosity in the transverse direction).

One of the very powerful characteristic properties of metallocene catalysts is the presence of a range of comonomers that may be incorporated into the polymer chain when using such catalysts for the polymerization of alkenes catalyzed one catalyst. Metallocene catalysts can, for example, for inclusion in the polymer chain of cyclic monomers, mainly polycyclic monomers, including cyclic monomers such as norbornene (C7H10). Thus, it is possible to include, for example, copolymers with ethylene materials such as norbornene, which will lead to the benefit of improving toughness E the present invention, have an additional advantage in their suitability for inclusion of the drawings. You can also include in the flooring graphical image in a way that gives the most profound of their perception. In this area is well known systems that use the technology of ion design. In these systems apply an electrostatic charge corresponding to a desired image. This image is deposited on the material using a drum or tape. Material bearing an electrostatic image, moves through the zone of the developer, where the material with the opposite charge, giving the color tone, stick to lighted areas of the dielectric surface with the formation of the visible image. On top it may be precipitated another polymer layer, and this layer is obtained another image. By adding successive layers, each of which has its own image, it is possible to build a structure with a deep perception of the image. This method, in which the use of conventional resins presented in U.S. patent N 5347296.

One advantage of using a polymer obtained using metallocene catalysts, Prowse the AET inclusion of boron-containing end groups and/or very high levels of ninasimone. These end groups to provide additional funds to facilitate image acquisition can be functionalized. Images can be created, or by using electrostatic systems design, or by functionalization of these end groups to the polymer chain is better connected with the toner or pigment.

Another object of the invention is a method of obtaining a sheet material suitable for use in flooring or as a floor covering, comprising mixing in a mixer polymer of at least c one additive comprising an inorganic filler, when heated to melt the polymer, forming a homogeneous liquid mixture in the form of a sheet, cooling and solidification, the polymer used polyalkene resin in accordance with the order, as described above, and mixing is carried out in a stirrer with great effort shift during the period of time equal to at least 10 minutes, at elevated temperature, component of at least 75oC.

Preferably stage of the process of formation of the sheet includes calendering.

More preferably stage of the process of education lowestcost at a temperature of from 100 to 250oC, most preferably from 130 to 200oC, to melt polyalkenes.

Another object of the invention is a method for coating for floors, including multi-layer stacking of layers based polymer with at least one additive comprising an inorganic filler, characterized in that use multiple layers containing a structural layer comprising hardening the carrier or substrate impregnated and/or coated with saturating composition; solid bottom covering layer, in which at least one of the layers receive the above method.

Preferably the method includes at least one layer, which is foamed, the method includes a step for the foam layer.

One preferred aspect of the invention uses a liquid mixture which essentially contains no plasticizer. However, as discussed above, the mixture can contain one or more plasticizers or excipients to improve the processing properties. When applied curable plasticizer, then the method includes additional processing of the cured sheet for curing to the same plasticizer. When S="ptx2">

The methods of producing a sheet material of the present invention have a significant advantage over methods that carry out using the usual polialcoolii or polyolefin resins. Not counting the excellent machinability, which provides the application of traditional existing production plant previously used for sheet materials based on PVC resin, with minimal modifications, due to the use of lower temperature curing in the methods of the present invention in comparison with the methods of production, based on the use of PVC resins for heat curing include fever, in the proposed methods is consumed less energy, resulting in lower energy consumption. Additional benefits that can be obtained in respect of the layers of the floor covering of this invention include higher impact strength of the outer transparent covering layer at higher impact strength due to the lower crystallinity associated with lower density; better recovery of cells in spenny the e MWD); and the high turnover of the saturated layer, obtained as a result of high M1 with a slight blocking of co monomer or in its absence.

With respect to the various aspects of the present invention should take into account that in order to "extend" the range of the specified polymer resins, with the aim of saving through the use of cheaper polialcoolii resins or to modify the final or other properties can be used other polymeric resins, which are outside specified. The number of such other polymer resins that can be used depends mainly on how it affects the fluidity and properties spread coating, consisting of materials of the invention. Thus, depending on the application and properties of the layers of the sheet can be used from about 50 to about 60 wt.% other polymeric resins (relative to the total weight of polymer resin). For example, a transparent covering layer, the amount of such other polymer resin is usually limited more a smaller amount constituting from about 15 to about 20 wt.%.

Additives that can be used in the materials of the present invention, and is neither depend on the particular resin used. Basic supplements and additional stages of processing, are generally well known in this field and are mentioned here include the following.

1. Inorganic fillers and reinforcers can enhance different layer or layers on the basis of the polyolefin in the coating material for floors, which is the subject of this invention. This amplification can be detected by improving the appearance, physical properties or chemical properties. To use a specific inorganic filler/hardener are important inorganic nature of the material, shape and material handling or surface coating. There are many important aspects of inorganic material. When applying density is an important and long-term usability of floor coverings. In this respect, can be very suitable highly filled upper layers (containing, for example, up to 85% by weight of the filler). Another important characteristic property of the material is hardness. For the final product is desirable increased hardness, but too solid filler (such as silica) can have a negative effect on the wear resistance proizvodyaschiesya fillers/reinforcers.

To increase opacity use whitening filler. Usually used less than 500 PHR, preferably from 20 to 120 PHR in saturating composition and foam cushioning materials and up to 200 PHR in solid substrate layers.

Optical properties of titanium dioxide make it particularly good pigment for white color with good opacity. This color is desired in the layer, which cause the printed image. It is located under the transparent wear-resistant layer. If this layer use a white filler such as calcium carbonate, at moderate levels, that can be used lower levels of titanium dioxide (from 2 to 6 PHR).

In compositions based polyolefin calcium carbonate has a specific value. It improves properties such as hardness, stiffness, heat distortion temperature, resistance to cracking due to stress, weldability, pacatuiesti and protivobloshinye properties. Reduced thermal shrinkage and elongation, as well as the permeability of water vapor and oxygen.

To strengthen the polyolefin composition used in coatings for floors, good another napolnitel layered structure. As for the increase in stiffness, heat distortion temperature and dimensional stability, the layered form of talc provides him with greater efficiency than calcium carbonate. The disadvantage of talc compared with calcium carbonate is lower impact strength, matte surface and a lower thermal-oxidative stability. These advantages and disadvantages is also mica, which also has a layered structure.

To increase the elastic modulus, ultimate tensile strength and heat distortion temperature systems based on the polyolefin has an even stronger impact than talc and mica, a high ratio of excipients to reinforcers, which are wollastonite (calcium silicate) and fiberglass.

Improvements provided by the high ratio of inorganic additives, will provide important assistance in coating system for floors made using the constant of the plasticizer and excipients to improve the processing properties, such as liquid paraffin. In these cases, the impact of such additives, which consists in giving rigidity to compensate for the loss of stiffness obtained tion and pacatuiesti, it may be useful silicon dioxide in the form of smoke or sludge at low concentrations (from 0.1 to 1.5%). In the system of flooring, it will be in a wear-resistant layer and in the layer, which cause the printed image. The same type of properties, which provides calcium carbonate, can provide aluminum trihydrate and magnesium hydroxide with the right particle size, which for most systems is less than 40 microns in diameter. In addition, they can provide high resistance and control the smoke. This will be discussed in more detail in the section concerning resistance to fire.

2. Polyolefin materials for coating systems for floors enhance by applying thermal and light stabilizers. The amount and type of thermal stabilizers used will vary with the change of method used for fabrication of the final structure. The approach, which consists in applying the melt, will provide a product that is less related to heating than the product obtained by means of calendering or extrusion of the melt. However, in all cases, which include foam system, polyolefin resin will be subjected to temperatures above 180oC during the time of the process.

When the protection of polyolefins from photooxidation particularly effective are the spatial employed amine light stabilizers (HALS). Particularly effective are rightly polymeric HALS, such as Luchem HA-B18 from Atochem (Atochem), which has the additional advantage that it does not show antagonism against other additives, such as DSTDP. The inclusion of 0.3% Luchem HA-B18 in an outer wear-resistant layer and 0.15% in the layer located under the transparent wear-resistant layer, will greatly enhance siteproject polyolefin coating systems for the sexes.

4. Depending on the cause, whether spread the floor or in the process of calendering (and conditions) may also be useful in enhancing the melt strength polyolefin system. To ensure a stronger and more elastic melt useful are graft copolymers of polyolefins and acrylic content in the range from 0.1 to 1.0%.

5. In coatings for floors based on the polyolefin, which are the subject of the invention, for most applications it is desirable to have the structure of one or more layers (this does not apply wear-resistant layer), which can be increased in volume (foam up) and give it the appearance of a foam with closely spaced cells. One effective way Polo in polyolefin systems are azo compounds. An example of this class of compounds is azodicarbonamide (Celogen AZ from Uniroyal). Particularly useful feature of this connection is that the temperature of its decomposition can be reduced from 220oC to less than 170oC due to the use of activators, such as zinc oxide. Such activated system through the use of inhibitors, such as benzotriazole, can be deactivated. If for printing on the surface of the polyolefin containing Celogen AZ and zinc oxide, are used benzothiazolesulfenamide inks for gravure printing, and the resulting structure having the above foamed layer of wear-resistant layer is heated to a temperature between the decomposition temperature of the activated and non-activated system, then the sample creates a convex pattern (chemical embossing).

In these structures can be used an additional blowing agent, such as aluminum trihydrate. Although its main purpose consists in the inhibition of inflammation and as an inorganic additive, he also plays other useful supporting role as the pore-forming substance, consisting in the fact that when heated above 200oC it produces water vapor. Beneficial effects as topolnicki properties or plasticizer.

In the case of azodicarbonamide it is usually used for the formation of foamed cushion, in the amount of from 2.0 to 4.5 PHR together with a suitable foaming activator, for example with zinc oxide.

Under appropriate conditions, some or all of the chemical pore-formers can be replaced by a mechanical foaming. Such conditions include the blend in the mixture based on the polyolefin, which is becoming one of the layers in the coating material for floors, air or other gas under conditions which give the desired number and desired size of the cells in the resulting foamed material. The system spread coating applied mixture should be foamy structure similar to the structure of the desired product. In the process of extrusion or calendering it is necessary that the gas was in the polymer in solution or in the system of the extruder in the form of small micro bubbles when the pressure of the melt. When the melt exits the extruder and passes from the high pressure (100 to 700 psi, or from 7,031 kg/cm2to 49,217 kg/cm2) to atmospheric pressure, swelling occurs. In both cases it is important that the cellular structure due to the rapid temperature drop in the sheet below that Neobee for floors, subject of the invention can be enhanced by using stitching usually using the organic peroxide used for increasing the toughness and/or stiffness of the layer of the sheet, in the amount of from 0.1 to 5.0 R. For such reactions are widely used reagent, as dicumylperoxide. This material becomes effective cross-linking agent at a temperature of 190oC. it is Known that the best foam cell structure will be created in the case of crosslinked foamed polyolefin systems when the crosslinking is carried out until foaming. In systems that include Celogen Z for foaming and dicumylperoxide for stitching, both processes will be held at the same temperature and for the same time period. If you use a peroxide with a lower activation temperature, such as 2,2-bis(tert-BUTYLPEROXY) butane, then it should be carried out at a temperature of 170oC stapling, and then at a temperature of 190oC foaming. Education durable stitched foam filled polyolefin systems can be enhanced by processing used inorganic filler vinylsilanes. In the formation of cross stitched mesh initiated posredstvennaia, become active.

In nesperennub layers dicumylperoxide is a good cross-linking agent. In layers, which are subject to foaming, it is preferable to use 2,2-bis(tert-BUTYLPEROXY) butane in combination with activated pore-forming system Celogen AZ. All filled with layers subject to foaming, the filler should be processed by the agent, such as vinylsilane specified will provide the filler particles center ninasimone.

7. For coating systems for floor-based polyolefin are also is the Flammability and smoke formation. Due to the use of a wide range of additives can be improved fire properties. As additives that act as fillers/flame retardants are suitable various inorganic compounds, such as aluminum trihydrate and magnesium hydroxide, which at elevated temperatures emit water. With improved fire properties of systems based on polyolefin useful role to play phosphorus compounds, borate and zinc oxide.

8. As noted above, as fillers or modifiers can be used with other polymer resins than the decree of the flax low density), EVA (ethylvinylacetate), ionomers, such as SURLYN (TM), available from Dupont Company (DuPont company) and VLDPE (polyethylene, very low density).

In addition, for specific combinations of desirable properties can be used a mixture of two or more polyolefins obtained using metallocene.

To improve impact properties using widespread known method can be used various types of elastomeric additives. They usually consist of small particles, the core of which consists of an elastomer, for example, is covered by an outer shell, which provides good adhesion to the matrix LRO polymer resin. An example of such an elastomeric additives, having a core and a shell, is Poraloid EXL-330 from Rohm and Haas Company (Rum and Haas company). This resin has a core of acrylic rubber and polymetylmetacrylate shell. Other types of modifiers that can be used to enhance impact properties include EPDM rubbers (ternary ethylene-propylene rubbers with diene co monomer), for example Polysar produced by the company Voeg (Bayer); A/B/A-block copolymers, for example Krafton, produced by Shell (shell); and numerous system di, which may be mentioned here include dyes, inks for gravure printing, antioxidants, etc. that are typically used in relatively small amounts, less than 50 PHR. In some applications, are also important antistatic properties.

In this case it would be appropriate to use in wear-resistant layer of various internal antistatics. Many antistatic additives are compounds with hydrophilic and hydrophobic parts. The usual material of this type is monoether polyol, such as glycerol and fatty acids with long chain, for example stereonova acid. Palilula part is very polar and comes to the surface of the polyolefin, while the fatty acid is similar to the polyolefin and will remain in the plastic. The hydrophobic part may be cationic, anionic or non-ionic. Suitable for the outer layer patterns are the amounts from 0.1 to 0.5 PHR.

10. Carriers or bases used in conjunction with the satiating compositions can have different forms, they can be in the form of, for example, woven or non-woven mesh or material or fabric, or less heat-resistant materials, for example glass fibers. Polyalkenoate or polilov, includes statistical bipolymer and ternary copolymers and block copolymers based on a variety of monomer units, including a lower alkene, preferably a 1-alkene having from 2 to 8 carbon atoms, such as propylene, but more preferably ethylene; dieny; cycloalkene and vinyl aromatic compounds.

Additional preferred characteristic features of the invention follow from the following detailed examples are described to illustrate, and the accompanying schematic drawings, in which:

Fig. 1 is a schematic side view showing the first part of the production line for the production of floor coverings;

Fig. 2 is the same side view of the second part of the production line shown in Fig. 1.

Fig. 1 shows the first cycle of the production line to obtain a three-layer sheet material 2 by applying a saturating foam gel and compounds 3, 4, 5 for applying a layer on a thin sheet of fiberglass cloth 6 (thickness of about 0.45 mm), delivered from the conveying drum 7 through the first drive 8. A thin sheet of fabric was passed through the first measurement system weight/surface 9 in the first unit 10 for applying promaznoy parryi shear effort 14 (approximately at the temperature of 90oC) was applied on one side 11 of the first roller 12 to a predetermined thickness equal to about 0.55 mm, adjustable using the first knife 13. On the other side 15 of the first roller 12 saturating composition was transferred to a thin sheet of fabric 6 in the gap 16 between the first roller 12 and located opposite the support is a thin sheet of cloth roller 17. Impregnated sheet of fabric 18 is then passed around a chilled drum 19 with a large diameter, the surface temperature of which was set equal to from about 25 to 40oC, and then through the cooling drums 20 for "curing the crystallization or solidification.

The coated cloth 18 is then sequentially applied formulations 4, 5 for the formation of a molten layer of foam and the bottom covering layer that had a thickness of ~0.2 and ~0.6 mm, the deposition was carried out in a similar fashion in the second and third units for applying spread coating 21 and 22, except that at the stage of applying the upper layer of chilled drum with a large diameter 19 is not used. The obtained three-layer sheet material 2 is then adopted to wind-up drum 23 that is located behind the second memory 24. Optionally, this sheet material is then about what about the picture for example, using paint designed for chemical embossing.

In Fig. 2 shows the second cycle of the production line 101, in which like parts corresponding to those of Fig. 1 denoted by the same positions as in Fig. 1, except that the added position 100. Three-layer sheet material 2 obtained in the first cycle of the production line 1, was delivered from the feed drum 107 via the memory 108 in the fourth unit for applying spread coating 110, in which the above mentioned sheet material 2 was applied composition for coating transparent layer 125 with a thickness of about 0.2 mm and utverjdali as before, except that in this case between the chilled drum 119 and heated mixer 114 to facilitate temperature control, etc. provided a heat shield to protect from heat.

Optionally, using another machine for applying spread coating (not shown) can be applied another foamed upper layer. In this case, you should take into account that in accordance with common practice in the industry, the order of application of different layers in a greater or lesser extent can be changed.

To what Itanium machines for applying striated coating roller.

The obtained multi-layer sheet material 140 is then passed through a multistage dryer, heated by hot air 141 to the maximum temperature of ~200C, mounted on a tape carrier 142, when the delay time of winding mechanism before the new cycle of winding, comprising about 1.5 min to ensure that the swelling of the foam layer (from about 0.2 to about 0.5 mm) at a polling control through chemical embossing in the case when it is used, after which it was carried out by cooling the final sheet material additional cooling drums 120, before taking on the receiving smatyvai drum.

To obtain coatings for floors that are the subject of the invention can also be used calendering of the melt. Although you can use as rolling of sheet and calendering of viscous workpiece when using Steklovolokno sheet, it is preferable to rolling.

Multilayer material was obtained by applying a series of melts on the basis of polialcoolii or polyolefin resins, which are described in the invention. All operations of the melt calendering can be performed continuously with the letters perform the operation of winding and then through separate operations cause additional layers. In addition, you can apply a combination of continuous and intermittent operations calendering. So, for example, fiberglass sheet can be applied saturating composition, then the base layer and the top foam layer. These three operations are carried out by sequentially before winding as passing the material through three different series calandria rolls. Between calendering operations you can perform additional processing stage. For example, a material obtained by applying the three polymer layers on glass fiber sheet, it is possible then to provide a decorative image and to facilitate chemical embossing skip through the installation of printing. After a single stage of printing can be followed by another stage calendering melt to Deposit wear-resistant layer on the coating for floors. After applying the wear-resistant layer can be accomplished stage heat treatment which is performed continuously or periodically. The heat treatment can foam up of different layers, resulting in layers containing a chemical blowing agent, is formed of foamed material. In addition, physical and chemical properties of polyolefin resins can improve the P CLASS="ptx2">

In the process of calendering melt on a series of two or more heated rolls is applied polymer melt thus, to obtain the polymer layer of the same thickness. Melt

obtained by mixing polymers and polimernyh components of the material under conditions of elevated temperature and shear forces. For this process can be applied to various devices, such as extruders or mixers. A more detailed description of the process of melt calendering can be found in Chapter 83 source Handbook of Plastic Materials and Technology, Irvin I. Rubin, published by John Wiley and Sons, Inc. (John Willy and sons., Inc.) (ISBN 0-471-09634-2).

The structure of the floor covering, which is the subject of the invention can also be obtained by extrusion from the melt. In such a process on a solid fiberglass sheet for single stage extrusion can be applied one or more layers of polymer. When to provide multiple layers in one pass through the system using a joint extrusion, to supply each of the melt in the block slotted heads for extrusion apply a separate extruder. The operation of the extrusion to obtain the final structure can be implemented together with other stages of processing. For example, steklopod co-extrusion, including transmission through three slotted head for the extrusion of the sheet from the melt. This structure can then be subjected to the printing process and the subsequent addition of one layer by extrusion. After applying the wear-resistant layer can be heat-treatment, which is carried out continuously or periodically. This processing can improve the final product due to foaming of the layer containing the chemical pore, and/or stitching layers containing systems stitching.

Originally described by way of creating desirable patterns of floor coverings, including the approach consisting in the use application of the melt, as shown in Fig. 1 and 2, can be expanded by use of fragile and/or unchanged excipients to improve the processing properties or plasticizers. Specified includes adding to a variety of polyolefin compositions used to obtain discrete layers of finite structures, fluids or liquids. This addition can be used to reduce the temperature required to obtain the viscosity required for a good treatment. So, for example, to obtain a homogeneous material having poobah, system polyolefin layer, you can mix white spirit, petroleum ether, gasoline or lacquer, using mixing heating or shear load. This fragile system in the form of white spirit or other plasticizer after the application of the system evaporates from the surface of the structure. Preferably, the evaporated white spirit or other plasticizer caught, are condensed and returned for recycling for recycling. Alternatively, you can use non-volatile liquid plasticizer, such as liquid paraffin (mineral oil). In this case, the resulting structure flooring will keep this material in the form of a constant component. You can also use a mixed system consisting of a volatile and changing fluids. The range of application of such additives can be extended from 200% to less than 5% relative to the weight of the polyolefin. However, the most desirable use of the polymerized plasticizer.

Monomers polymerized plasticizer that may be used in accordance with the present invention are those which are solvents for the principal(s) polymer(s) component(s) polyolefine other components, which themselves may also be polymers, such as impact resistance modifiers, auxiliary means for textures, pigments and other compatible substances. The monomers will in General be a long segment, which is similar to the polyolefin with an end group which is capable of free radical polymerization. Conventional structures, "such polyolefin are hydrocarbons with ten or more carbon atoms, and examples of such groups include lauryl (C12H25and stearyl (C18H37). Such structures are partially depending on the structure of the polyolefin can be linear, branched or cyclic. End of the polymerized group can be simple unsubstituted double bond, such as 1-dodecene or more complex elementary level, such as methacrylate, as in sterilisability.

For curing of the products obtained and to provide improved properties along with the monomer or monomers of the plasticizer can be used compounds which generate at elevated temperatures free radicals, and optionally the monomers, forming a cross connection. Can be used the peroxides, ketone-peroxide, perikaryon, PROXIFIER, cumene hydroperoxide, and peroxyketals. Useful are also several classes of azo compounds and many photoinitiators. Properties required for these compounds lies in the fact that the connections were essentially depolimerizuet, i.e. remained during the initial mixing, mixing, and method of production potential, but could be induced to receive free radicals at a rate that will initiate polymerization of the monomer, for example, when the overall temperature or when the connection is subjected to appropriate radiation. Such material as, for example, tert-butylperbenzoate, has a half-life of more than 1000 h at 100oC, while at 160oC the half-life is less than 2 minutes the System polymer/monomer containing such initiator, can be recycled in the form of the final product (i.e., the shape or configuration) at 100oC, and then by heating at 160oC such a system utverjdayut.

When the system includes a polyfunctional monomers, then from the monomer can be formed by a continuous system reticulated polymer. Optional could the second polyolefin system. When sew one together existing continuous systems (i.e., pre-existing polyolefin and the polymerized monomer plasticizer), get poluvsasavania reticular spatial structure (semi-1PN). When you sew the two systems, is formed vzaimopronikayut reticular spatial structure (1PN).

To prevent premature polymerization of the monomer plasticizer may be a suitable addition to the system of additional inhibitors. To prevent polymerization during handling and processing the majority of commercial monomers provide inhibitors. To compensate for the time spent in the conditions of formation of polyolefin polymer product, i.e. in the conditions used to convert the primary polyolefin polymer into a sheet or other shape or configuration, the level of such inhibitors should be increased. In this regard, the most significant factor is usually temperature, but can also be appropriate for other conditions. For example, sterilisability commercially provide 275 parts per million (ppm) nanometrology ether of hydroquinone (MEHQ). Depending on time and temperature may be the will be about the range of chemical families.

To receive plasticized material with low viscosity, which can be used for the manufacture of many kinds of products, using various methods of manufacture, the polymer system and the monomer system can be combined. The mixture of solid and liquid components can be accomplished in any suitable way, for example by use of a continuous mixer or mixer periodic operation, various types of mixing devices continuous or intermittent actions or various types of extruders. In all these types of equipment solid components are mixed together at a temperature and shear effort, sufficient to achieve both distributive and dispersive mixing. Fluid is injected at the required temperature and is subjected to shear force for dissolution of the basic polymer components and to obtain a good distributive and dispersive mixing of insoluble components from the obtained liquid. Then the liquid system is kept at a temperature that maintains the necessary fluidity for the manufacture of the final product form. This is usually carried out at a temperature from 80 to 120oArticle to create polymer chains, extending and mutually penetrate through pre-formed mesh spatial structure MPO polymer chains. When sew MPO polymer chain and polymerized plasticizer, then two polymer material mutually absorb each other, forming a so-called vzaimopronikayut polymer mesh (1PN), though if only one of these polymeric materials are made, then unstitched polymer chain can be removed. The last type of material suitably referred to poluvsasavania (semi-1PN). Such interpenetrating and poluvsasavania materials, although they are usually very similar physical properties physical properties of other materials provided with the present invention provide additional advantages from the point of view of increased resistance against stains and/or increased resistance against solvents as during placement and use of coatings for floors, secured by the present invention.

Example 1

Obtaining the multi-layer coating for floors using calendering

The structure of the floor coverings obtained by providing the first in the first cycle of the production line (the simulation gave a solid fiberglass Mat. Each zone has provided a separate mixers melt. In the first zone fiberglass Mat impregnated with the composition A. the following area struck composition B to create a layer of the substrate. In the third zone has caused the composition C to create a foaming layer. Then, the resulting system took on exhaust swath. On a separate stage of the process the system was applied to the print line, where the foam layer is caused decorative pattern. At the third stage of processing the material with a printed image is applied to the second cycle of the production line from one area of the melt calendering and then in the system dual-zone furnace (see Fig. 2). In the calendering zone inflicted composition D to create a transparent top layer. In the first zone of the furnace, the temperature of which was 160oC, has been a staple of each layer; in the second zone, the temperature of which was 190oC capable of swelling the layer of foam. Then the final product took on exhaust swath.

Composition to create different layers were as follows:

A. (Saturating layer) - PHR

MPO resin Exact 4038 - 100

Tieren - inorganic filler is magnesium hydroxide - 60

The source of free radicals for crosslinking - dicumylperoxide - 2

Teriba-Heidi - 0,1

The second antioxidant to prevent degradation of the polymer tiefer DSTDP (distearyldimethylammonium) - 0,1

The second antioxidant Ultranox 626 from Berg-Warner Chemicals (Berg-Warner Chemicals) - 0,05

B. Lower layer PHR

Exact 4038 - 100

Magnesium hydroxide - 150

The source of free radicals for the polymerization of the crosslinking - 2,2-bis(tert-BUTYLPEROXY)butane - 2

Irganox 1010 and 0.1

DSTDP - 0,1

Ultranox 626 - 0,05

C. (Foam layer) - PHR

Exact 5008 - 100

Reinforcing filler wollastonite with a high content of metasilicate calcium - 30

The flame retardant inorganic filler aluminium trihydrate - 30

The chemical blowing agent of azodicarbonamide (emit gas and nitrogen) - 2

Zinc oxide to reduce the temperature of decomposition of azodicarbonamide necessary to reduce the temperature of the foaming polymer - 0,8

2,2-bis(tert-BUTYLPEROXY)butane - 2

Irganox 1010 and 0.1

DSTDP - 0,1

Ultranox 626 - 0,05

Luchem HA-B18 - polymer light representing spatial hindered amine from Atochem (Atochem) and designed to prevent photochemical degradation of polymer - 0,15

D. (Wear-resistant top layer) - PHR

Exact 5008 - 100

Vinyltriethoxysilane providing additionally the Luchem HA-B18 - 0,3

Irganox 1010 and 0.1

DSTDP - 0,1

Ultranox 626 - 0,05

Example 2

Obtaining the multi-layer coating for floors using spread coating

Example 2 used the same sequence of stages and zones, which was used in example 1, except that in each zone the coating is preferably carried out smearing melt than calendering of the melt. The composition of all four layers were the same, except that each of the four formulations was added 80 parts Jayflex 215 and 20 parts of monomer G (monomer, forming a cross connection from Rohm and Haas) (Rum and Haas).

You should take into account that in the above described embodiment without deviating from the essence of the present invention can be made of various modifications. For example, alternative to chemically-initiated crosslinking of or in addition to the process of chemically initiated crosslinking can be used crosslinking initiated by the electron beam. Such crosslinking can be performed by exposure of the sample the electrons with high energy at a dose of from about 6 to about 8 megaregion over time from 30 s to 2 min To obtain a good result in this way is p the e from 2 to 5 parts.

Example 3

Individual characteristic compositions for coating

A. (Transparent covering layer) - PHR

MPO resin Engage EP 8500 (Dow Chemical To.) (5.0 MI; density of 0.87; DR1 0,5) - 100

The stabilizer protivootechenoe Irganox 1010 - 0,05

The stabilizer protivootechenoe EIT - 0,03

A crosslinking agent 2,5-TR1 - 0,1

B. Foaming gel layer PHR

MPO resin Engage EP 8500 (from Day Chemical To.) - 100

Whitening filler (typical for this class of substances) - 15

The pore-forming - uzasadnienie (typical for this class of substances) - 3

The blowing catalyst is zinc oxide and 1.5

Component for pigmentation - zinc oxide - 4

The stabilizer Irganox 1010 - 0,075

The stabilizer DSTDP - 0,05

Additive to improve the fluidity - calcium stearate - 0,10

Fire retardant Firebrake (TM) - 5

The flame retardant antimony oxide - 4

C. (Saturating layer) - PHR

LRO resin Engage EP 8500 (from Dow Chemical To.) - 100

Whitening filler (typical for this class of substances) - 50

The stabilizer Irganox 1010 and 0.1

Additive to improve the fluidity - stearate of zinc - 0,4

D. Solid upper-layer - PHR

MPO resin Engage EP 8500 (from Dow Chemical To.) - 100

Whitening filler (typical for this class of substances) - 200

It is Additive to improve the fluidity - calcium stearate - 0,10

Fire retardant Firebrake (TM) - 5

The flame retardant antimony oxide - 4

Example 4

Individual characteristic compositions for coating

Prepared another series of compositions based on polymeric resins, which are described above in example 1, but instead of resin EP 8500 from Dow Chemical company used the LRO resin from the Dow Chemical company brand SM 1250, which has an affinity to the above.

Example 5

Obtaining the multi-layer coating for floors using multiple spreading

By using the technique of multiple buttering received the material of the floor covering in the form of a four-layer structure. In the source area of the glass fiber sheet impregnated with A composition containing the resin, at a temperature of approximately 100oC. In a separate area on the lower side of the glass fiber sheet saturated with polymer, at a temperature of approximately 100oC from the composition B has caused the bottom layer. In another separate area on the upper part of the glass fiber sheet saturated with polymer, at a temperature of approximately 100oC struck composition C to obtain the foaming layer. Then on the foam layer using a continuous method of printing nab is a system of accelerated pricing and consequently be obtained by foaming the effect of chemical eliminate bulges. Another single stage coating on the foam layer at a temperature of approximately 100oC struck composition D for formation of a transparent wear-resistant layer. Then, the resulting structure pass through oven system at a temperature of approximately 170oC for stitching layers and then at a temperature of ~200C foaming layer increased in volume. At the end of the structure utverdili, was designed and has been profiled product, which amounted to a coating material for floors.

A. (Saturated layer) - PHR

MPO resin Exact 4038 - 100

Calcium carbonate - 66,7

Stealthkill (curable plasticizer) - 90

Trimethylolpropane (curable plasticizer) - 10

Lupersol 230 (initiator of radical polymerization from Atochem) - 5

Irganox 1010 and 0.1

DSTDP - 0,1

Ultranox 626 - 0,05

B. (upper layer) - PHR

Exact 4038 - 100

Calcium carbonate - 300

Sterilmatic - 90

Trimethylolpropane - 10

Lupersol 230 - 5

Irganox 1010 and 0.1

DSTDP - 0,1

Uetranox 626 - 0,05

C. (Foam layer) - PHR

Exact 5008 - 100

Calcium carbonate - 66,7

Sterilmatic - 90

Trimethylolpropane - 10

Irganox 1010 - 0,1

DSTDP - 0,1

Ultranox 626 - 0,05

D. (Wear layer) - PHR

Exact 3017 - 100

Sterilmatic - 70

Trimethylolpropane - 30

Lupersol 230 - 5

VINYLTRIMETHOXYSILANE - 4

Luchem HA-B18 - 0,3

Irganox 1010 and 0.1

DSTDP - 0,1

Ultranox 626 - 0,05 e

1. Sheet material suitable for use in flooring or floor covering in the form of a hard, wear-resistant material and containing a polymer resin in a homogeneous mixture with at least one additive comprising an inorganic filler, characterized in that the said polymer resin contains polyalkene resin having a relatively narrow limits of the molecular mass distribution (MMD), which is less than 3, a small degree of long chain branching and obtained by polymerization of at least one linear, branched or cyclic alkene having from 2 to 20 carbon atoms, using one catalyst, and mentioned polyalkene also has the following properties: a) a melt index (IR) from 0.1 to 100; b) a density of from 0.86 to 0.97 in) measure the rheological properties (ORS) from 0.1 to 6.0, where ORS is an indicator of the long chain branching, as measured SR with zero degree of long chain branching (RDP) on the graph, representing the dependence of the viscosity at zero shear on the relaxation time (both values from the equation of viscosity in the transverse direction).

2. The sheet material under item 1, characterized in that polyalkenoate resin has ORS from 0.4 to 5.5.

3. The sheet material under item 1, characterized in that it is suitable for use as a composite layer coating for floors, selected from the upper layer and the structural layer.

4. The sheet material under item 1, characterized in that it is used as a component in the coating layer for a floor other than the upper covering layer, and this layer is a foamed layer.

5. The sheet material under item 1, characterized in that it is virtually free of liquid plasticizer.

6. The sheet material according to any one of paragraphs.1-3, characterized in that polyalkene includes a copolymer obtained by copolymerization of at least two alkenes, including the first linear or branched alkene having from 2 to 8 carbon atoms, and at least one additional linear, branched or cyclic alkene having from 2 to 20 carbon atoms.

7. Sheet material p. 6, characterized in that the first womanuncensored.

8. The sheet material under item 6 or 7, characterized in that it contains up to 15 mol.% one additional(s) of monomer(s).

9. The sheet material according to any one of the preceding items, wherein the sheet material includes at least a floor, vzaimopronikayut polymer grid of polyalkene and polymer selectively curable liquid monomer system plasticizer, which, essentially, is depolymerizing in the formation of the sheet used in the manufacture of sheet material used as a covering for floors, although then, essentially, you can polimerizuet in order to obtain a material essentially containing no liquid plasticizer.

10. The sheet material under item 9, characterized in that the monomer plasticizer includes linear, branched or cyclic alkene having at least 10 carbon atoms and end of the polymerized functional group.

11. The floor covering in the form of a hard, wear-resistant sheet material based on polymer resin containing at least one layer of sheet material that contains a polymer resin in a homogeneous mixture with at least one of polyalkene resin, with a relatively narrow limits of the molecular mass distribution (MMD), which is less than 3, a small degree of long chain branching and obtained by polymerization of at least one linear, branched or cyclic alkene having from 2 to 20 carbon atoms, with the use of one catalyst, and mentioned polyalkene also has the following properties: a) a melt index (IR) from 0.1 to 100; b) density rheological properties (ORS) from 0.1 to 6.0, where ORS is an indicator of the long chain branching, measured by comparing the shift to the right (due to a longer relaxation time) relative to the polymer resin with a zero degree of long chain branching (ROC) graph representing the dependence of the viscosity at zero shear on the relaxation time (both values from the equation of viscosity in the transverse direction).

12. Flooring on p. 11, characterized in that it has at least these two layers mentioned sheet material containing a structural layer comprising hardening the carrier or substrate impregnated and/or coated with saturating composition and solid bottom covering layer, and the above-mentioned coating for the floor is different, however, the above-mentioned transparent protective or upper covering layer made of the above polyalkenes resin, essentially, does not contain filler.

14. The floor covering under item 12, characterized in that it includes a foamed layer.

15. The floor covering under item 12, characterized in that all layers except the top covering layer of foam.

16. The floor covering according to any one of paragraphs.11-15, characterized in that it is virtually free of liquid plasticizer.

17. The floor covering under item 16, characterized in that it comprises a curable plasticizer.

18. A method of obtaining a sheet material suitable for use in flooring or as a floor covering, comprising mixing in a mixer polymer with at least one additive comprising an inorganic filler, when heated to melt the polymer, forming a homogeneous liquid mixture in the form of a sheet, cooling and hardening, characterized in that the polymer used polyalkene resin according to any one of the preceding paragraphs and the mixing is carried out in a stirrer with great effort shift during the period of time, ravnos is 19. The method according to p. 18, characterized in that the mixture is injected auxiliary substance, contributing to the formation of the sheet.

20. The method according to p. 18, characterized in that stage of the process of formation of the sheet includes calendering.

21. The method according to PP. 18, 19, or 20, characterized in that stage of the process of formation of the sheet includes applying a spread coating.

22. The method according to p. 21, characterized in that the use of an auxiliary substance for applying spread coating, which is a liquid plasticizer.

23. The method according to p. 22, characterized in that as an excipient for application of spread coating using liquid paraffin.

24. The method according to any of paragraphs.19-21, characterized in that use is selectively curable liquid monomer system plasticizer, which, essentially, is depolymerizing in the formation of the sheet used in the manufacture of sheet material used as a covering for floors, but then it can essentially be polimerizuet in order to obtain a material essentially containing no liquid plasticizer.

25. The method according to p. 24, characterized in that it includes a step EA and consequently to receive sheet material, essentially, not containing liquid plasticizer.

26. The method according to p. 25, characterized in that the stage of formation of the sheet is carried out at a temperature of from 70 to 120oC, and stage polymerization is carried out at a temperature of from 150 to 250oC.

27. A method of producing a covering for floors, including a multi-layer stacking of layers based on polymer, of at least one additive comprising an inorganic filler, characterized in that use multiple layers containing a structural layer comprising hardening the carrier or substrate impregnated and/or coated with saturating compound, solid bottom opaque layer and a transparent or top covering layer, in which at least one of the layers produced by the method according to one of paragraphs.14-21.

28. A method of producing a covering for floors, including at least one layer, which churn, p. 27, characterized in that the method includes a step for the foam layer.

 

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