Moulding composition

FIELD: chemistry.

SUBSTANCE: invention relates to a polyethylene moulding composition intended for making pipes, conduits and cables, and a method of producing said composition. The composition has a multimodal molecular-weight distribution, density in the range of 920 to 960 kg/m3, melt flow index MFI190/2 in the range of 0.05 to 10 g/10 min and Shore hardness D, measured according to ASTM D2240-05 (15 s), of at least 56.0. The composition contains at least three ethylene polymer fractions having different molecular weight. Each of the fractions A, B and C is an ethylene homopolymer or a copolymer of ethylene with at least one C3-C10 comonomer. In the composition, one of the fractions A, B and C is an ethylene homopolymer and at least one of the other fractions is an ethylene copolymer with content of said C3-C10 comonomer of 1-15 wt %. Fraction A has weight-average molecular weight Mw in the range of 15 to 40 kg/mol, fraction B - in the range of 70 to 200 kg/mol and fraction C - in the range of 220 to 400 kg/mol.

EFFECT: obtained polyethylene moulding composition has excellent mechanical properties, hardness and wear resistance, and also has high impact resistance and slow crack growth.

13 cl, 6 dwg, 6 tbl

 

The invention relates to a polyethylene composition having excellent mechanical properties, hardness and abrasion resistance, as well as having high characteristics of the shock and the slow growth of cracks. In addition, the invention relates to a method for producing such compositions and to the use of such compositions for obtaining pipes for molding applications and for use in the manufacture of wires and cables.

The excellent behavior of the polymer in relation to the slow growth of cracks is important in many applications, including the reception of pipes and products produced by blow molding. Good resistance is also required for the finished products, so that they can withstand the impact without breaking. In addition, excellent mechanical properties in combination with good abrasion resistance and high hardness are essential properties for use in the manufacture of wires and cables.

The polyethylene composition according to the invention has a tri-modal molecular weight distribution, then there is a composition containing three fractions of the polymer of ethylene having a different molecular weight.

Injection molding under pressure can be used to manufacture a wide range of products, including the products view, having relatively complex shapes and a wide range of sizes. For example, injection molding is suitable for the manufacture of tubes and caps, as well as transport packaging, which often has a specific shape that corresponds to the subject that it is.

Examples of such products include boxes, cartons, trays, buckets, pallets and containers with cells. In addition, injection molding is widely used for the production of home textiles, such as plumbing sink and drain channels, bowls, food containers and buckets, as well as for thin-walled packaging products, such as open plastic containers for frozen or fresh food or non-food applications, for example for paints, adhesives, cosmetics and pharmaceutical materials.

As raw material rises in price, and consumers and producers become more demanding, traders polymers are seeking opportunities to provide cheaper, high-quality products for their customers.

Important properties of the polymer used for injection molding, are their mechanical properties, which, in turn, determine the properties of the final cast product. In particular, the polymer must have good impact resistance and, at the same time, a good balance between the control of the resistance to cracking under the influence of the environment (which, for example, to determine hoteleobrotowy samples or creep testing with a full cut (Full Notch Creep Test, FNCT) and stiffness (which, for example, determined by the modulus of tensile elasticity (E-modulus)). Of course, the polyethylene composition at the same time should possess good processability, such as good flow characteristics.

In order to reduce the size and to produce lighter products, there is increasing demand for more rigid polymeric materials.

Higher rigidity makes it possible to produce products with thinner walls and therefore allows the use of less raw material for the product than for a less rigid products. Thinner walls mean more light products and, consequently, lower transport costs. Lighter products also mean the reduction of the cycle time, which is also very important. Lighter items will be faster to cool, allowing you more likely to make the process of casting and producing more products for a specified period of time.

Unfortunately, the prior art it is known that increasing the stiffness of the polymer his other important properties such as impact strength and resistance to cracking under the influence of the environment, decrease, because these properties are at least partially mesowest the YMI, as, for example, resistance to cracking under the influence of the environment increases with a decrease in density, while the hardness increases with increasing density.

In General, the expert can increase the rigidity and resistance to cracking under the influence of the environment in a known manner, for example by increasing the molecular weight of the polymer. It is known that polymers with higher molecular weight have better mechanical properties compared to polymers with lower molecular weight. However, increasing the molecular weight polyethylene usually reduces manufacturability, and especially the flow properties of the polyethylene. Polymers with poor fluidity cannot easily ekstradiroval or to mold and, thus, they have limited value.

Also there is a relationship between hardness and toughness. More rigid materials tend to be the worst toughness, because they are more fragile. Materials with high toughness tend to be soft, to be able to absorb the shock. For cast products ability to withstand shock is an important property. However, the manufacture of products with high stiffness and good impact properties is a problem known in the prior art.

Thus, the La production of higher quality products from polyethylene molding compositions of matter to apply the composition had good or even excellent impact resistance, and good or even excellent balance of mechanical properties, particularly in terms of resistance to cracking under the influence of the environment and stiffness, measured in units of the modulus of tensile elasticity (E-modulus). At the same time the polyethylene moulding composition should exhibit good processability, such as good fluidity.

Although in the field of plastic molding compositions was performed a large number of developments, there is still a need for a polyethylene composition suitable for use in injection molding, blow molding and direct pressing, especially for use in the manufacture of wires and cables, plugs and caps, transport packaging and products for domestic applications, which provides a combination of, on the one hand, excellent mechanical properties, including excellent impact strength, crack resistance and stiffness as well as a good balance between mechanical properties and high hardness and abrasion resistance.

It was unexpectedly found that these objectives can be achieved by using a polyethylene molding composition containing at least one fraction of homopolymer and at the ore one fraction of copolymer in at least three-component system, in which these three fractions include one fraction with a low molecular weight, one fraction with an average molecular weight and one fraction with high molecular weight.

The INVENTION

Thus, in the proposed invention the polyethylene moulding composition having a multimodal molecular weight distribution, having a density according to ISO 1183 at 23°C in the range of 920 to 960 kg/m3and VKT190/2according to ISO 1133 in the range of from 0.05 to 10 g/10 min; however, the specified polyethylene moulding composition contains at least three fractions of the polymer of ethylene having different molecular weights:

A) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with a low molecular mass, with the mass-average molecular mass Mwin the range from 15 to 40 kg/mol;

(B) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with an average molecular mass, with the mass-average molecular mass Mwin the range from 70 to 200 kg/mol; and

C) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with a high molecular mass, with the mass-average molecular mass Mwin the range from 220 to 400 kg/mol;

provided that one of the fractions a, b, C is a homopolymer of ethylene, and at least one other component is a copolymer of ethylene with at least od is named C 3-C10the co monomer;

and the composition has:

- hardness shore D as measured by ASTM D2240-05 (15), at least 56,0.

In another aspect of the present invention proposed a molded article comprising the composition described above in the text of this specification.

In another aspect of the present invention proposed the use of a composition described above in the text of this specification, in the manufacture of molded products, especially products made by direct extrusion or injection molding.

It should be noted that at least a tri-modal polymer composition according to the invention is characterized not by any one of the above symptoms, but a combination of all the above defined characteristics. With this unique combination of characteristics can be obtained polyethylene moulding composition with excellent characteristics, particularly in terms of hardness, but also in respect of the balance of stiffness/resistance to cracking under the influence of the environment, and impact properties.

In another aspect of the present invention, a method for obtaining defined above composition, comprising mixing

A) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with a low molecular mass, with the mass-average molecular mass Mwin the range from 15 to 40 kg/mol;/p>

(B) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with an average molecular mass, with the mass-average molecular mass Mwin the range from 70 to 200 kg/mol; and

C) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with a high molecular mass, with the mass-average molecular mass Mwin the range from 220 to 400 kg/mol;

provided that one of the fractions A, B, C is a homopolymer of ethylene, and at least one other component is a copolymer of ethylene with at least one C3-C10the co monomer;

and the composition has:

- multimodal molecular mass distribution;

the density according to ISO 1183 at 23°C in the range 920-960 kg/m3;

- PTR/2 according to ISO 1133 in the range of from 0.05 to 10 g/10 min, and

- hardness shore D as measured by ASTM D2240-05 (15), at least 56,0.

In another aspect of the present invention proposed a polyethylene moulding composition having a multimodal molecular weight distribution, a density according to ISO 1183 at 23°C in the range of 920 to 960 kg/m3and VKT190/2according to ISO 1133 in the range of from 0.05 to 10 g/10 min, with the specified polyethylene moulding composition contains at least three fractions of the polymer of ethylene having different molecular weights:

A) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with low molecular weight, with the TPP190/2according to ISO 1133 of from 50 to 1000 g/10 min;

(B) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with an average molecular weight, MFR:190/2less than 10 g/10 min; and

C) 15-50% of the mass. fraction homopolymer or copolymer of ethylene with a higher molecular weight, with the TPP190/21less than factions, and in the range from 0.05 to 5 g/10 min,

provided that one of the fractions A, B, C is a homopolymer of ethylene, and at least one other component is a copolymer of ethylene with at least one C3-C10the co monomer;

and the composition has:

- hardness shore D as measured by ASTM D2240-05 (15), at least 56,0.

DETAILED description of the INVENTION

Wherever in the text of this specification is not met, the term "molecular weight" is meant the mass-average molecular mass.

Typically a polyethylene composition comprising at least two fractions of polyethylene, which were obtained under various conditions of polymerization, resulting in different (mass-average) molecular weights and different molecular weight distributions of these fractions, referred to as "multimodal". Accordingly, in this sense, the compositions according to the invention is a multimodal polyethylene. The prefix "multi" refers to the number of different faction the polymers, composed the song. Thus, in this case, the composition consisting of the three factions, called "tri-modal".

Polyethylene molding composition according to the invention preferably is a tri-modal polymer and consists of a faction And homopolymer (NMG) or copolymer (NMS) ethylene with a low molecular weight; fraction of homopolymer (SMG) or copolymer (SMMS) ethylene with an average molecular weight and the fraction of homopolymer (VMG) or copolymer (VMS) ethylene to high molecular weight, as described in detail below, where one of a, b and C represents a homopolymer, while the other two components are the copolymers.

Found that the polyethylene molding composition according to the invention allows to obtain products with the ideal balance of properties. They have excellent mechanical properties and good processibility. In particular, the products show excellent balance of stiffness/resistance to cracking under the influence of the environment, as well as excellent impact strength. In particular, this composition shows the ideal hardness.

As noted above, the composition has a density according to ISO 1183 at 23°C in the range of 920 to 960 kg/m3more preferably from 925 to 940 kg/m3.

PTR/2 according to ISO 1133 of the composition is di the range from 0.05 to 10 g/10 min Preferably, the polyethylene composition has an MFR of 0.1 to 5 g/10 min, more preferably from 0.3 to 2 g/10 minutes

The modulus of tensile elasticity (E-modulus) measured on samples obtained by direct pressing of the multimodal polyethylene molding composition, is preferably at least 300 MPa, preferably at least 400 MPa, more preferably at least 500 MPa and most preferably at least 550 MPa or more.

The composition according to the invention has the impact strength Charpy CIS (0°C), measured on samples with a V-shaped incision, obtained by direct pressing, at least 90 kJ/m2preferably at least 110 kJ/m2. Preferably the composition according to the invention has the impact strength Charpy (-20°C), measured on the received direct pressing of the samples with a V-shaped incision at least 30 kJ/m2preferably at least 50 kJ/m2more preferably at least 80 kJ/m2.

In addition, the composition according to the invention preferably has a resistance to cracking under the influence of the environment measured during tests on creep with a full cut on the ISO/DIS 16770.3 at 50°C and 9 MPa, at least 20 h, preferably at least 40 hours, especially at least 60 hours

p> In addition, the composition according to the invention has a hardness of shore D, measured according to ASTM D2240-05 (15), at least 56,0, preferably at least 56,5 and more preferably at least 57,0. The composition according to the invention preferably has a hardness of shore D, measured according to ASTM D2240-05 (3) at least 58,0, preferably at least 59,0 and more preferably at least 57,0.

The composition according to the invention can be abrasion by the Taber ASTM D4060-07 (roller CS-10) less than 8 mg/1000 cycles, preferably less than 7 mg/1000 cycles.

In addition, the composition according to the invention preferably has a voltage of plastic deformation (yield strength) of at least 12 MPa, preferably at least 13 MPa.

In addition, the composition according to the invention preferably has a stress at break (tensile strength) of at least 20 MPa, preferably at least 25 MPa.

In addition, the composition according to the invention has an elongation at break of at least 450%, preferably at least 500%.

Of course, the composition according to the invention can have any combination of these parameters.

As mentioned above, the polyethylene molding composition according to the invention includes three different fractions of the polymer of ethylene, have their different molecular weight.

Fraction And

Fraction And represents a low-molecular (MMO) fraction homopolymer or copolymer of ethylene (NMG or NMS, respectively). The molecular weight of A fraction is in the range from 15 to 40 kg/mol, preferably from 20 to 30 kg/mol.

PTR190/2according to ISO 1133 of A fraction is preferably at least 50 g/10 min, more preferably at least 100 g/10 min, the Upper limit for PTR/2 MMOs fraction is preferably 1000 g/10 minutes

Density according to ISO 1183 at 23°C homopolymer NMG fraction is preferably in the range from 960 to 980 kg/m3preferably from 965 to 975 kg/m3. Density according to ISO 1183 at 23°C copolymer MMOwiththe fraction is preferably in the range from 915 to 935 kg/m3preferably from 920 to 930 kg/m3.

Fraction In

Fraction represents a fraction of average molecular mass (hmm) homopolymer or copolymer of ethylene (SMMgor hmmwith, respectively). Hmm fraction has a molecular weight higher than that of hmm-fraction, and a lower value PTR190/2than MMO-faction.

Preferably, the TPP190/2Hmm-fraction is less than 10 g/10 min, preferably less than 5 g/10 min, and more preferably less than 1 g/10 min. in Addition, SMG fraction preferably has a MFR190/2in the range from 5 to 50 g/10 min, Ave is doctitle from 10 to 20 g/10 minutes

Thus, the hmm fraction has a molecular weight preferably in the range of from 100 to 200 kg/mol, more preferably from 110 to 180 kg/mol. Density homopolymer SMG fractions according to ISO 1183 at 23°C is preferably in the range from 950 to 965 kg/m3preferably from 952 to 957 kg/m3. The density of the copolymer hmmwithfractions according to ISO 1183 at 23°C is preferably in the range from 905 to 925 kg/m3preferably from 910 to 920 kg/m3.

Fraction With

The cut is a high molecular weight (AMM) fraction homopolymer or copolymer of ethylene (AMMgor TIMwith, respectively). TIM fraction has a molecular weight higher than that of hmm-faction and SMM-fraction, and a lower value PTR190/2than SMM-faction.

Thus, TIM fraction has a molecular weight in the range from 220 to 400 kg/mol, preferably from 250 to 350 kg/mol, more preferably from 270 to 295 kg/mol. In one example embodiment TIM faction has MB less than 300 kg/mol. Density homopolymer TIMgfractions according to ISO 1183 at 23°C is preferably in the range of 930 to 950 kg/m3preferably from 940 to 950 kg/m3. The density of the copolymer TIMWithfractions according to ISO 1183 at 23°C, preferably less than 910 kg/m3.

In addition, TIMwiththe fraction is preferably who meet the TPP 190/21in the range from 0.05 to 5 g/10 minutes

Preferably, two factions represented copolymers, and one fraction of the homopolymer.

In the preferred example embodiment of Fraction A (low molecular weight fraction) represents a homopolymer of ethylene, while Faction b and C are copolymers of ethylene. Also preferably, if the faction is a homopolymer, and fractions a and C - copolymers. Preferably also, if the cut is a homopolymer, and fractions a and b copolymers.

When used in the text of this patent description, it is assumed that the term "homopolymer of ethylene comprises a polymer consisting essentially of repeating units derived from ethylene. For example, the homopolymers may contain at least 99.8% of the mass, and preferably at least 99.9% of the mass. recurring units derived from ethylene. In the preferred example embodiment the fraction of homopolymer only detect blocks of ethylene.

When used in the text of this patent description, it is assumed that the term "ethylene copolymer" includes polymers that consist of repeating units derived from ethylene and at least one C3-C10the co monomer. Preferred copolymers are binary and thus contain this the len and the only comonomer.

The comonomers that can be used include C3-C10alpha-olefins, preferably selected from but-1-ene, Gex-1-ene, 4-methyl-1-Penta-1-ene, hept-1-ene, Oct-1-ene and Oct-1-ene, more preferably - but-1-ene and Gex-1-ene. Preferably use hexene or butene, or a mixture of hexene and butene. In one example embodiment of the present invention use only one comonomer. This comonomer represents, for example, hexene or butene, preferably hexene.

Preferably copolymers of ethylene containing from 1 to 15% of the mass. the co monomer, based on the high molecular weight fraction of ethylene, preferably from 2 to 12% of the mass. and more preferably from 5 to 10% of the mass.

Any fraction can be present in a mass ratio of from 15 to 50 wt. -%, preferably from 20 to 40% of the mass. Polyethylene molding composition according to the invention contains a fraction, and preferably in an amount of from 18 to 45% of the mass. for each fraction, especially from 20 to 40% of the mass. for each fraction. Preferably the fractions a, b and C are present in equal quantities, about 33.3% of the mass, for each fraction.

In one example embodiment of the present invention proposed a mixture of fractions a, b and C, i.e. the sum of the fractions a, b and C is 100%. Thus, highly preferred composition according to the image is the shadow of this mixture. Moreover, preferably the fractions a, b and C was the only polyolefin components in the composition so that the composition consisted essentially of these components and standard polymer additives.

If in the text of this description lists the characteristics of the fractions (A), (b) and (C) the composition according to the invention, typically, these values are for cases when they can be measured directly on the appropriate fractions, for example, if the fraction is obtained separately or get the first stage of the multistage process.

However, the base polymer can also be obtained (and preferably to be in a multistage process in which, for example, fraction (A), (b) and (C) receive on successive stages. In this case, the properties of the fractions obtained at the second and third stage (or in a later stage) multistage process, you can either infer from the properties of the polymers, which separately receive on a separate stage, employing the same conditions of polymerization (for example, an identical temperature, partial pressure of reagents/solvents, suspension medium, reaction time), relative to the stage of a multistage process, which receives a given fraction, and using a catalyst, which is not present in any of the pre-obtained polymers. In Alt rnative case, the properties of the fractions obtained at a later stage of the multistage process, can also be calculated, for example, by the method of C. Hagstrom, Conference on Polymer Processing The Polymer Processing Society), Extended Abstracts and Final Programme, Gothenburg, August 19-21, 1997, 4:13.

Thus, although the properties of the fractions obtained in the later stages of the multistage process, and cannot be directly measured on the products of such a multistage process, you can define them using one of the above ways or both ways. Suitable method can be selected by the technician.

The method by which the polyethylene molding composition according to the invention, is not critical to this invention. The composition can be obtained by mechanical mixing of the individual fractions, by mixing in the reactor or in situ mixing by combining these two processes, or in other ways, which is achieved by the corresponding homogenization. For example, the composition can be obtained by mechanical mixing of the three factions in the desired quantity, for example, using conventional equipment for compounding or mixing, such as a Bunbury mixer, double-roll rollers for elastomers, elasticator bass (Buss) or twin screw extruder.

Fractions A, B and C used for mechanical mixing, get the CTD is a major using any conventional method of homopolymerization or copolymerization of ethylene, accordingly, for example, in the gas phase, slurry phase, liquid phase polymerization in mass), using conventional reactors, such as a loop reactor, gas-phase reactor, the reactor properities or periodic operation, in the presence of a catalyst of polymerization.

Preferably the fractions get carrying out the reaction in suspension, preferably in a loop reactor, or in gas-phase reactor.

This composition can also be obtained by in-situ mixing of at least two of the three factions, or all three factions.

Under in-situ mixing imply obtaining a multimodal polymer, in which faction or simultaneously receive, at one stage of the reaction (for example, when using different catalysts), and/or get them in a multistage process.

Multistage process is defined as the process of polymerization in which a polymer consisting of two or more fractions, produce receiving each faction or at least two polymer fractions on a separate reaction stage, usually under different reaction conditions at each stage, in the presence of the reaction product of the previous step, which contains a polymerization catalyst. The polymerization reaction used at each stage may include a normal reaction homopolymerization or copolym the polarization of ethylene, for example, the polymerization in the gas phase, slurry phase, in the liquid phase, using conventional reactors, e.g. loop reactors, gas phase reactors, reactors with a mixing tank reactors, batch and so on (see, for example, WO 97/44371 and WO 96/18662).

Thus, the multimodal polyethylene molding composition according to the invention can be obtained by using multi-stage sequence of reactions involving successive stages of polymerization, carried out at given various reaction conditions in the respective reactors arranged in series, to obtain the corresponding fractions of polyethylene having different molecular weight. A process of this type can be made in suspension medium: in this case, the monomers in the presence of a molecular weight regulator, preferably hydrogen, first polymerized in the first reactor under first reaction conditions, in the presence of a suspension medium and a suitable catalyst; then the obtained product is transferred to the second reactor and conduct further polymerization under second reaction conditions and then transferred to the third reactor and conduct further polymerization when the third reaction conditions, the first reaction conditions differ from the second and third is aukcionnyh conditions so to obtain three fractions of polyethylene having different molecular weight.

Each method of obtaining a used catalyst polymerization. Polymerization catalysts include catalysts, which represents a coordination compound of a transition metal, such as catalysts of the Ziegler-Natta (TSN), metallocene catalysts, nepetalactone catalysts, chromium catalysts, etc. Catalysts can be supported on a carrier, for example on conventional substrates, including silicon dioxide, Al-containing substrate and the substrate on the basis of magnesium dichloride.

Preferably the catalyst is a metallocene catalyst. Getting a metallocene catalyst can be performed in accordance with methods known from the literature, or similar, and it is within the competence of the professionals.

These metallocene contain at least one organic ligand, generally 1, 2 or 3, for example 1 or 2, which is connected with the metal η connection, for example η2-6-ligand, such as η5the ligand. Preferably metallocene represents a connection 4-6 transition metal group, you can Titanian, zirconocene or garretsen, which contains at least one η5the ligand, which, for example, represents a possibly substituted cyclopentadienyl, vozmojnostey indenyl, possibly substituted tetrahydroindene or possibly substituted fluorenyl.

The metallocene compound may have the formula I:

(Cp)mTnMAq(1),

in which:

each Cp independently is an unsubstituted or substituted and/or condensed Homo - or heterosynaptically ligand, for example a substituted or unsubstituted cyclopentadienyl, substituted or unsubstituted indenyl or substituted or unsubstituted fluorenyl; one or more substituents preferably selected from halogen, hydrocarbide (for example, C1-C20of alkyl, C2-C20-alkenyl, C2-C20-quinil, C3-C12-cycloalkyl, C6-C20-aryl or C7-C20-arylalkyl); C3-C12-Cycloalkyl, which contains in ring 1, 2, 3 or 4 heteroatom (heteroatoms); C6-C20-haloalkyl, -SiR"3, -OSiR", -SR", -PR"2or-NR2; each R" independently represents hydrogen or hydrocarbon, for example, C1-C20-alkyl, C2-C20alkenyl, C2-C20-quinil, C3-C12-cycloalkyl or C6-C202two Deputy R" can form a ring, e.g. five - or six-membered ring together with the nitrogen atom to which they are attached.

T is a bridge of 1-7 atoms, e.g. a bridge of 1-4 C-atoms and 0-4 heteroatoms, in which the heteroatom (heteroatoms) can be, for example, atoms of Si, Ge and/or O, each of the atoms of the bridge may independently have substituents such as C2-C20-alkyl, three(C1-C20-alkyl)silyl, three(C1-C20-alkyl)siloxy or C6-C20-aryl; or a bridge of 1-3, e.g. one or two, heteroatoms, such as silicon atoms, germanium and/or oxygen, for example,-SiR21in which each R1independently represents a group as C1-C20-alkyl, C6-C20-aryl or three(C1-C20-alkyl)silyl, for example the trimethylsilyl group.

M represents a transition metal of groups 4-6, for example, group 4, such as Ti, Zr or Hf.

Each And independently represents a Sigma-ligand, for example, H, halogen, C1-C20-alkyl, C1-C20-alkoxy, C2-C20alkenyl, C2-C20-quinil, C3-C12-cycloalkyl, C6-C20-aryl,C 6-C20-aryloxy, C7-C20-arylalkyl, C7-C20-arylalkyl, -CH2-Y, where Y represents a C6-C20-aryl, C6-20-heteroaryl, C1-20-alkoxy, C6-20-aryloxy, -NR2, -SiR"3or OSiR", -SR", -PR"3, -SiR"3, -OSiR"3or-NR2; each R" independently represents hydrogen or hydrocarbon, for example, C1-C20-alkyl, C2-C20alkenyl, C2-C20-quinil, C3-C12-cycloalkyl or C6-C20-aryl; or e.g. in case of-NR2two Deputy R" can form a ring, e.g. five - or six-membered ring together with the nitrogen atom to which they are attached.

Each of the above cyclic structures, by itself or as part of a molecule, as a substitute for Cp, A, R or R1may be optionally substituted, for example, C1-C20-alkyl which may contain Si atoms and/or;

n is 0,1 or 2, for example 0 or 1,

m is 1, 2 or 3, for example 1 or 2,

q is 1, 2 or 3, for example 2 or 3, when m+q is equal to the valency M

More preferred is a metallocene compound of formula II

(Cp)2MX2(1) ,

in which both Cp may be substituted, or may be a condensed Homo - or heterosynaptically ligand;

M is Zr or Hf;

and both X represents-CH2-Y, in which Y represents C6-20-aryl, C6-20-heteroaryl, C1-20-alkoxy, C6-20-aryloxy, -NR2, -SiR"3or OSiR"3,

R represents a C1-20hydrocarbon or, in the case of-NR2two of the substituent R may form a ring together with the nitrogen atom to which they are attached.

In the formula (II) both Cf are possibly substituted, or possibly condensed Homo - or heterosynaptically ligand, for example a substituted or unsubstituted cyclopentadienyl, substituted or unsubstituted indenyl or substituted or unsubstituted fluorenyl.

Specified Deputy (deputies) present in the Cp group, which are selected from halogen, hydrocarbide (for example, C1-20-alkyl, C2-20-alkenyl, C2-20-quinil, C3-20-cycloalkyl, C6-60-aryl or C7-20-arylalkyl), C3-12-geterotsiklicheskie, C5-20-heteroaryl, C1-20-haloalkyl, -NR'2, -SiR'3or OSiR'3while R' represents a C1-20-hydrocarbon (for example, C1-20-alkyl, C2-20alkenyl, C2-0 -quinil, C3-12-Cycloalkyl or C6-20-aryl), or, in the case of-NR'2two of the substituent R' may form a ring together with the nitrogen atom to which they are attached.

Cp preferably represents cyclopentadienyl, indenyl, tetrahydroindene or fluorenyl, possibly substituted, as defined above. More preferably, Cp denotes a cyclopentadienyl or tetrahydroindene.

In a preferred example embodiment, the two groups Cp remain unsubstituted or both are replaced by the same number and type of substituents.

Preferred substituents include C1-20-alkyl, C6-20-aryl or C7-20-arylalkyl.

In a particularly preferred case, the Cp group are unsubstituted or both have C1-6-alkyl substituent, such as methyl, ethyl, isopropyl or n-butyl.

M represents Zr or Hf, particularly preferred is Hf.

Preferably both Y are selected from C6-20-aryl, -NRn"2, -SiR"3or OSiR"3in which R" is as defined above.

More preferably, -CH2-Y represents a benzyl or-CH2-SiR"3while R represents a C1-6-alkyl or C6-10-aryl.

Especially preferred are the following compounds:

Dibenzyl-bis(n-butylcyclopentadienyl)Hf,

Dibenzyl-bis(metaltitlepane dienyl)Hf,

Dibenzyl-bis(1,2-dimethylcyclopentane)Hf,

Dibenzyl-bis(n-propylcyclopentanol)Hf,

Dibenzyl-bis(ISO-propylcyclopentanol)Hf,

Dibenzyl-bis(1,2,4-trimethylcyclopentanone)Zr,

Dibenzyl-bis(tetrahydroindene)Zr,

Bis(n-butylcyclopentadienyl)Hf(CH2SiMe3)2,

Bis(n-propylcyclopentanol)Hf(CH2SiMe3)2,

Bis(ISO-propylcyclopentanol)Hf(CH2SiMe3)2,

Bis(1,2,4-trimethylcyclopentanone)Hf(CH2SiMe3)2.

The most preferred compound is dibenzyl-bis(n-butylcyclopentadienyl)Hf.

Getting metallocenes used in accordance with this invention can be carried out in accordance with (or similar to) the methods known from the literature, which are in the competence of specialists in this field.

Metallocene compounds of the formula I can be obtained, for example as described in EP 1462464.

The catalytic composition is preferably used in this invention, additionally includes impregnated (saturated) alumoxane media obtained by bringing alumoxane or modified alumoxane in contact with silicon dioxide as the inert material of the carrier.

There are various ways to get alumoxane and modified alumoxanes, neogranichinymi the examples of which are described in U.S. patents 4665208, 4952540, 5091352, 5206199, 5204419, 4874734, 4924018, 4908463, 4968827, 5308815, 5329032, 5248801, 5235081, 5157137, 5103031, 5391793, 5391529, 5693838, 5731253, 5731451, 5744656, in European publications EP-A-0561476, EP-B1-0279586 and EP-A-0594218 and in WO 94/10180, which are all fully included in the text of this description by reference.

Preferably for impregnating media use alumoxane, especially methylalumoxane or modified methylalumoxane, isobutyryloxy, for example, TIBAO

(tetraisostearate) or GIBO (examsolutions). It is more preferable to use methylalumoxane (MAO).

The molar ratio of Al alumoxane component to the metal catalyst with the same type of active centers of polymerization is in the range from 0.3:1 to 2000:1, preferably from 20:1 to 800:1 and most preferably from 50:1 to 500:1.

Preferred as the inert carrier used silicon dioxide. Surface area, pore volume and particle size of the silica can be selected in accordance with the requirements of the particular polymerization process, which will use these catalysts. It is usually possible to use particles of silicon dioxide having a surface area in the range of from about 10 to 700 m2/g (BET method), pore volume in the range of from about 0.1 to 6.0 cm3/g and average particle size in the range of from about 10 to 500 microns.

Silicon dioxide mo is et to be in the form of pellets, agglomerates, in colloidal form or another.

Additionally, it is preferred that the material of the carrier was calcined, that is heat-treated in air and then in directionspanel gas, for example nitrogen. This processing is preferably carried out at a temperature above 100°C, more preferably 200°C. or higher, for example at 200-800°C, especially about 600°C. the annealing Treatment is preferably carried out in a few hours, for example from 2 to 30 hours, more preferably about 10 hours.

Soaked alumoxanes media is obtained by bringing alumoxane in contact with the silicon dioxide and heating to a temperature from 50°C to 100°C. containing Such alumoxane silicon dioxide is used as a carrier for metallocene formula (I) or (II). Preferably impregnated alumoxanes media contains less than 15% of the mass. aluminum, more preferably from 9.0 to 14.5% of the mass. and most preferably from 10.0 to 14.0% of the mass. aluminum, based on the total weight of the material of the carrier and alumoxane.

The catalyst is preferably applied to the material of the carrier in an amount of from 0.05 to 4%, preferably from 0.1 to 3.0%, especially from 0.2 to 2.0 wt%. the active metal is relatively dry mass of the material medium.

The polyethylene composition according to the invention may also contain small amounts of additives, that is as pigments, the nucleating, antistatic agents, fillers, antioxidants, processing AIDS, and so on, generally in amounts up to 10 wt. -%, preferably up to 5% of the mass.

If the composition contains additives, the properties according to the invention is measured on the compositions with additives present.

This invention also relates to the product obtained injection molding or direct pressing, containing the above polyethylene composition, method of producing the product obtained injection molding or direct pressing, which includes forming this composition injection molding or direct pressing of obtaining products, and to the use of a polyethylene composition for injection molding or direct compression.

Description of the DRAWINGS

Fig.1 depicts the dependence of the modulus of tensile elasticity of the density for the compositions according to the invention.

Fig.2 depicts the voltage dependence of plastic deformation density for the compositions according to the invention.

Fig.3 depicts the dependence of hardness shore D (ASTM D2240-05) at 15 with density for the compositions according to the invention.

Fig.4 depicts the dependence of hardness shore D (ASTM D2240-05) if 3) is the density for the compositions according to the invention.

Fig.5 depicts the dependence of the viscous shock is t and a cut on the Sharpie at -20°C impact strength notched at Sharpie at 0°C for compositions according to the invention.

Fig.6 depicts the dependence of creep, when tested with a full notch in at 9.0 MPa and 50°C, density of the compositions according to the invention.

INFORMATION ON TESTS

Gel permeation chromatography (GPC): Average molecular mass, molecular mass distribution and the index polydispersity (Mn, Mw, MWD, PDI).

Average molecular weight (Mw, Mn), molecular mass distribution (MMD, MWD) and its width described by the index polydispersity, PDI=Mw/Mn where Mn is srednekamennogo molecular weight, a Mw represents a mass-average molecular mass) was determined by using gel permeation chromatography (GPC) according to ISO 16014-4:2003 and ASTM D 6474-99. The instrument Waters GPCV2000 equipped with differential refractometric detector and on-line viscometer, used with TSK-gel columns 2xGMHXL-HT and 1xG7000HXL from Tosoh Bioscience and 1,2,4-trichlorobenzene (TCB, stabilized with 250 mg/l 2,6-di tert-butyl-4-METHYLPHENOL) as solvent at 140°C and at a constant flow rate of 1 ml/min For analysis of 209.5 introduced ál of the sample solution. Set the columns were calibrated using universal calibration (ISO 16014-2:2003), at least 15 of polystyrene (PS) standard samples with narrow molecular weight distributions in the range from 1 kg/mol to 12000 kg/mol. Used constants Brand-Hovinga the La cops, PE and PP are consistent with ASTM D6474-99. All samples were prepared by dissolving 0.5 to 4.0 mg of polymer in 4 ml (140°C) stabilized TCB (the same was used as mobile phase), maintaining the solution within a maximum of 3 hours maximum at 160°C with constant gentle shaking, before the introduction of the sample into the GPC instrument.

Density

The density of the polymer was determined according to ISO 1183-1987, method D, the samples obtained by the method of direct compression.

The melt flow index of

The melt flow index (MFR) determined according to ISO 1133; his lead in g/10 min MFR is an indicator of the ability of the polymer to flow and, consequently, its maintainability. The higher the melt flow index, the lower the viscosity of the polymer. MFR is determined at 190°C and it can be defined at different loads, for example when 2,16 kg (MFR190/2), 5 kg (MFR190/5) or 21.6 kg (MFR190/21).

Impact strength Charpy

Impact strength Charpy determined according to ISO 179:2000 samples with a V-shaped incision, the size of 80×10×4 mm3if (0°C impact strength Charpy (0°C) and at -20°C (impact strength Charpy (-20°C)). Samples were cut from the plates 4 mm thick, obtained by the method of direct compression, ISO 293-2004, using the conditions specified in section 3.3 ISO 1872-2:2007.

Elastic properties

The modulus of tensile elasticity

<> As a measure of hardness was measured modulus of tensile elasticity (E-modulus) of the songs at 23°C on samples obtained by the method of direct compression, according to ISO 527-2:1993. Samples obtained by direct pressing, cut out from a plate thickness of 4 mm, obtained by the method of direct compression ISO 293:2004, using the conditions defined in section 3.3 ISO 1872-2:2007. The module was measured at a speed of 1 mm/min

Voltage plastic deformation (yield strength)

Voltage plastic deformation (MPa) was determined on the same samples according to ISO 527-2. The measurements were carried out at 23°C, with a speed of strain 50 mm/min

The voltage of destruction and destructive deformation

Stress fracture, or the tensile strength (in MPa) and destructive deformation or elongation at break (%) was determined on the same samples according to ISO 527-2. The measurements were carried out at 23°C, with a speed of strain 50 mm/min

Creep testing with full cut

Resistance to cracking under the influence of the environment was measured in accordance with test method for creep with a full cut on the ISO/DIS 16770.3, at 50°C and a stress of 9 MPa, with a depth of cut of 1 mm and dimensions of the sample 123 mm ×6 mm × 20 mm, solvent Used was a 10% about. Igepal CO-630 in deionized water. Used samples, the floor is obtained by direct pressing. Samples were cut out of the plate thickness of 6 mm, obtained by the method of direct compression ISO 293:2004, using the conditions specified in section 3.3 of ISO 1872-2:2007.

The shore hardness

Hardness shore D measured according to ASTM D2240-05 at 3 or 15 (rod of hardened steel with a diameter of 1.1-1.4 mm, with conical narrowing of 30° and end with a radius of 0.1 mm, the force pushing 44,64 N). Samples were cut from the plates 4 mm thick, obtained by the method of direct compression ISO 293:2004, using the conditions defined in section 3.3 ISO 1872-2:2007.

Resistance to abrasion to Taber

The deterioration rate was calculated as the mass loss (mg) 1000 cycles ASTM D4060-07 (roller CS-10). Samples were cut from the plates with a thickness of 2 mm obtained by the method of direct compression ISO 293:2004, using the conditions defined in section 3.3 ISO 1872-2:2007.

The content of the co monomer

The content of the co monomer in the obtained products were measured in a known manner, on the basis of infrared spectroscopy with Fourier transform (FTIR), with calibration13C-NMR, IR spectrometer Nicolet Magna 550, together with software Nicolet Omnic FTIR.

Of the samples by direct extrusion films were obtained, having a thickness of from about 220 to 250 μm. Similar films were prepared from the calibration samples with known content of co monomer. The thickness change is Yali at least five points of the film. Then the films were made roughened with sandpaper to avoid reflections. To avoid contamination, the film does not touch the hands. For each sample and the calibration sample were obtained at least two films. The films were pressed from the pellet using the press to film Graceby Specac, at 150°C, using the preheat time 3+2 min, the pressing time of 1 min and a cooling time of 4-5 minutes For samples with very high molecular weight preheating time can be increased or to increase the temperature.

The content of the co monomer was determined from the optical density at a wavelength of about 1378 cm-1. Comonomer used in the calibration samples was the same as comonomer present in the samples. Analysis was performed by using a resolution of 2 cm-1, the wavelength range from 4000 to 400 cm-1and the number of scans 128. For each film was shot at least two spectra.

The content of the co monomer was determined from the spectrum recorded in the wavelength range from 1430 to 1100 cm-1. The optical density was measured as the peak height, choosing the so-called short or long base line, or both. Short baseline spend approximately in the area 1410-1320 cm-1through the points of minima, and the long baseline is between about 1410 and 1220 cm-1 . Must be calibrated separately for each type of baseline. In addition, the content of co monomer in an unknown sample must be within the range of concentrations of the co monomer in the calibration samples.

EXAMPLES

Preparation of catalyst

Preparation of metallocene complex:

The catalytic complex used in the examples of polymerization, represented dibenzyl-bis(n-butylcyclopentadienyl)hafnium, (n-BuCp)2Hf(CH2Ph)2and it was produced in accordance with Example 2 preparation of the catalyst" WO 2005/002744, on the basis of the dichloride bis(n-butylcyclopentadienyl)hafnium (coming from Witco).

The preparation of the catalyst was performed in a 160 l reactor batch, which was added a solution of metallocene complex. During the reaction, the stirring speed was 40 rpm, and at drying - 20 Rev/min Before the reaction, the reactor was thoroughly washed with toluene and, after addition of silicon dioxide in it was created by an inert atmosphere using nitrogen.

Preparation of a catalytic composition

10,0 kg of activated silica (commercial carrier is silicon dioxide, XP02485F having an average particle size of 20 μm; supplier: Grace) first suspended 21.7 kg of dry toluene at room temperature. Then the suspension of silicon dioxide to allali to 14,8 kg 30% of the mass. methylalumoxane in toluene (MAO, supplied by Albemarle) for 3 hours. After that, the mixture MAO/silica was heated to 79°C for 6 hours, and then cooled to room temperature.

The resulting solution was reacted with 0.33 kg (n-BuCp)2Hf(CH2Ph)2in toluene (67.9% of the mass.) within 8 hours at room temperature. The catalyst was dried by blowing with nitrogen for 5.5 hours at 50°C. the resulting catalyst had a molar ratio Al/Hf equal to 200; the Hf concentration of 0.44% of the mass. and the Al concentration of 13.2% of the mass.

Molding a plastic composition Obtaining Fractions a, b and C

Fraction homopolymer or copolymer of ethylene with a low molecular weight (NMG or NMS fraction) fraction B homopolymer or copolymer of ethylene with an average molecular mass (hmmgor hmmwithfraction) and a fraction With homopolymer or copolymer of ethylene to high molecular weight (VMG or VMS fraction) were obtained separately in the plant with the reactor prior to polymerization (terpolymerization) (reactor prior to polymerization loop type, with a capacity of 50 DM3and a loop reactor with a volume of 500 DM3. In the reactor prior to polymerization downloaded previously obtained a catalyst in the form of 15% of the mass. suspension in oil (primol 352).

Other parameters of the reaction are shown in Table 1.

Table 1
The preliminary polymerization
A18A17A28
(MMOg)(Hmmg)TIMwith)
T [°C]606060
Pressure [MPa (bar)]6(60)6(60)6(60)
The feed rate of the catalyst [g/h]3529,715,2
Submission of antistatic [million hours] Octastat 3000550
The feed rate of ethylene [kg/h]020
The feed rate of H2[g/h]010
Speed under the Chi propane [kg/h] 474734
Loop reactor
T [°C]858580
Pressure [MPa (bar)]5,7 (57)5,7 (57)5,7 (57)
The feed rate of ethylene [kg/h]373730
The feed rate of H2[g/h]81,80
Feed rate hexene [kg/h]005
The flow rate of propane [kg/h]828282
The concentration of C2[% mole.]7,66,26,2
The ratio of [H2/C2mol/KMOL]0,480,07 0,06

The ratio of C6/C2[mol/KMOL]--207
Capacity [kg/h]32,334,029,1
Properties
Irganox V [million hours]200020002000
PTR190/2[g/10 min]3400,93-
PTR190/21[g/10 min]-170,89
Density [kg/m3]972,4954,5907,4
Mw[kg/mol]24129272
Content6[wt. -%]--8,6
Pre the preliminary polymerization
A22A25A15
(MMOwith)(Hmmwith)TIMg)
T[°C]606060
Pressure [MPa (bar)]5,8 (58)5,9 (59)6,0 (60)
The feed rate of the catalyst [g/h]to 19.928,230,9
Submission of antistatic Octastat 3000 [million hours]005,0
The feed rate of ethylene [kg/h]002,0
The feed rate of H2[g/h]000,7
The flow rate of propane [kg/h]34,334,247,4
Loop reactor
T[°C]748585
Pressure [MPa (bar)]5,7 (57)5,7 (57)5,6 (56)
The feed rate of ethylene (C2) [kg/h]353834
The feed rate of H2[g/h]121,20
The feed rate of hexene (C6) [kg/h]5,24,20
The flow rate of propane [kg/h]676782
The concentration of C2[% mole.]6,25,35,9
The relation of H2/C2[mol/KMOL]0,50,120,02
The ratio of C6/C2[mol/KMOL]219 111-
Capacity [kg/h]the 33.436,931,0
Properties
Irganox V [million hours]200020002000
PTR190/2[g/10 min]3700,5-
PTR190/21[g/10 min]--0,88
Density [kg/m3]922915,4944
Mw[kg/mol]24138294
The contents of C6[wt. -%]8,36,9-

The basic properties of the obtained polymers are shown in Table 2. Party A15, A17 and A18 are homopolymers; party A22, A25 and A 28 are copolymers of hexene.

Table 2
The basic properties of each of the unimodal fractions
A15 (AMMg)A17 (SMMg)A18 (MMOg)A22 (MMOwith)A25 (SMMwith)A28 (AMMwith)
d, kg/m3944,0954,5972,4922,7915,4907,4
PTR190/2Not ODA.0,933403700,5Not ODA.
PTR190/210,8817Not ODA.Not ODA.Not ODA.0,89
MM, kg/mol2941292424 138272
HEXEN, % of the mass.0008,36,98,3

With the help of extrusion mixing of melts were prepared 12 different plastic compositions.

Preparation of polyethylene mixture

Three fractions were mixed and homogenized in the molten state in the extruder.

Compounding was carried out by stirring the extruder simultaneously with rotating and coming into engagement with two screws Prism TSE 16 having a screw diameter D of 16 mm and a ratio L/D of 25, using high-intensity mixing augers equipped with kneading blocks. Was installed following the temperature profile along the length of the screw: 210°C/215°C/220°C/215°C/210°C, using speed production of 1-1,5 kg/h and the speed of screw rotation of 200 rpm Each composition was extrudible twice to ensure proper homogenization. Each mixture consists of three factions, and one of them is homopolymer. The exact composition of each mixture is given in Table 3.

Table 3
Composition to the positions of the examples according to the invention (mass fraction)
A15A17A18A22A25A28
TIMg)(Hmmg)(MMOg)(MMOwith)(Hmmwith)TIMwith)
Example-133,333,333,3
Example-233,333,333,3
Example 333,333,333,3
Example 440,020,0 40,0
Example 540,040,020,0
Example 620,040,040,0
Example 720,040,040,0
Example 840,020,040,0
Example 940,020,040,0
Example-1040,040,020,0
Example 1120,040,040,0
Example 1240,040,020,0

Mechanical properties

The mechanical properties of the mixtures are presented in Table 4. As the material for comparison was tested commercial polymer Borstar brand ME.

Comparison of mechanical properties graphically shown in Fig.1-2. As can be seen from these graphs, when similar density described mixtures exhibit superior mechanical properties compared to polymer comparison Borstar ME.

Table 4
Density, MFR and mechanical properties of mixtures (comparison test conducted on ME).
dPTR190/2,ModuleVoltageVoltageDestroyed
kg/m3g/10elasticplasticdestructionBoost
minguestsdeformationMPaA deformation
MPaMPation, %
Example 1931,10,6050715,533,5595,5
Example 2931,90,4749515,723,9685
Example 3931,60,7648215,224645
Example 4934,00,455816,431,9547
Example 5935,40,3957217,124800
Example 6927,40,3539213,6of 21.9565
Example 7923,50,1634812,525,8478
Example 8931,70,1449215,826,6700
Example 9930,60,2148215,326,6618
Example 10935,90,69597of 17.532,6597
Example 11929,50,6642714.4V20,4602
Example 12936,20,9658817,222,9697
ME936,30,6754816,113,8356

The hardness and abrasion

The results of measuring the hardness shore D (ASTM D2240-05, measured at 3 and 15 seconds) and resistance to abrasion to Taber (coefficient abrasion resistance, ASTM D4060-07, roller CS-10) are shown in Table 5. The same data in graphical form shown in Fig.3 and 4.

Table 5
Hardness shore D (ASTM D2240-05) and the resistance to abrasion is aniu on a Taber (ASTM D4060-07, roller CS-10) for examples according to the invention for the polymer comparison (ME)
Shore D (15)Shore D (3)Wear index
Example 156,5to 58.13,7
Example 256,558,45,1
Example 356,058,06,6
Example 457,959,75,3
Example 557,759,76,8
Example 1058,660,15,9
Example 1257,759,39
ME55,857,98,9

As can be seen from Fig.3 and 4, the examples according to the image the structure shows significantly better hardness and abrasion resistance as compared with the polymer comparison Borstar VT6053 (with similar density). This means that in the case of compositions according to the invention the same firm and the same abrasion resistance can be obtained at a lower density (up to 5 units below, with benefits in terms of lower modulus of bending, which are the consequence). Alternatively, at the same density can be increased hardness and abrasion resistance.

The data presented in Table 5, clearly show that the proposed polymeric compositions exhibit better abrasion resistance compared to polymer comparison ME.

The impact resistance and resistance to cracking under the influence of the environment

The samples of examples 1, 4, 7 and 10 were tested for impact strength and resistance to cracking under the influence of the environment, in comparison with ME.

The impact toughness (impact strength Charpy notched, according to ISO 179) at 0°C and -20°C and creep testing with a full notch in at 9.0 MPa and 50°C (according to ISO 166770:E) were conducted on samples obtained by direct pressing. The remaining results are shown in Table 6; the same information in graphical form shown in Fig.5 and 6.

As can be seen from Fig.5, for examples according to the invention are observed significantly higher toughness values compared to the polymer of the comparison. This difference is particularly noticeable for the shock viscosity at low temperature.

Not surprisingly, the magnitude of the creep test will be conducted with the cut decreases with increasing density (Fig.6). However, you can see that the trend line for the examples according to the invention lies significantly above the values for material comparison (ME).

Table 6
Impact strength Charpy (at 0°C and -20°C) and creep when tested with a full cut (9,0 MPa and 50°C) for mixtures according to the invention and polymer comparison ME
Impact strength Charpy at 0°C, kJ/m2Impact strength Charpy at -20°C, kJ/m2Creep (9,0 MPa, 50°C), h
Example 112490135
Example 41245693
Example 7115118Not ODA.
Example 10933660
ME791725

Therefore, we can conclude that the described polymer compositions show a slower crack growth and improved toughness as compared with the material comparison ME.

1. Polyethylene moulding composition having a multimodal molecular weight distribution, a density according to ISO 1183 at 23°C in the range of 920 to 960 kg/m3and the melt flow index, determined according to ISO 1133 at 190°C and a load of 2.16 kg, PTR190/2in the range from 0.05 to 10 g/10 min; however, the specified polyethylene moulding composition contains at least three fractions of polymers of ethylene having different molecular weights:
A) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene with a low molecular mass, with the mass-average molecular mass Mwin the range from 15 to 40 kg/mol;
B) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene with an average molecular mass, with the mass-average molecular mass Mwin the range from 70 to 200 kg/mol; and
C) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene with a high molecular mass, with the mass-average molecular mass Mwin the range from 220 to 400 kg/mol,
provided that one of the fra the Nations And B and C is a homopolymer of ethylene and at least one other component is a copolymer of ethylene with at least one C3-C10the co monomer;
and the composition has
- hardness shore D as measured by ASTM D2240-05 (15), at least 56,0;
- each faction copolymer contains comonomer C3-C10and the content of the co monomer is from 1 to 15% of the mass.

2. The composition according to p. 1 with resistance to abrasion by the Taber, measured according to ASTM D4060 with roller CS-10, less than 8 mg/1000 cycles, preferably less than 7 mg/1000 cycles.

3. Composition under item 1, in which the fractions a, b and C are present in amounts from 20 to 40 wt. -%, for example, 33.3% of the mass. for each fraction.

4. Composition under item 1, in which the Fraction And represents a fraction of homopolymer, having a density in the range from 965 to 980 kg/m3preferably from 970 to 975 kg/m3; any fraction of a copolymer, having a density in the range from 920 to 930 kg/m3preferably from 920 to 925 kg/m3.

5. Composition under item 1, in which the Faction is either the fraction of homopolymer, having a density in the range from 950 to 965 kg/m3preferably from 952 to 957 kg/m3; any fraction of a copolymer, having a density in the range from 910 to 920 kg/m3preferably from 912 to 917 kg/m3.

6. HDMI is the information under item 1, in which the cut is either the fraction of homopolymer, having a density in the range from 935 to 950 kg/m3preferably from 942 to 947 kg/m3; any fraction of a copolymer, having a density of less than 910 kg/m3.

7. Composition under item 1, in which the Fraction And represents a homopolymer of ethylene, and fractions b and C are copolymers of ethylene.

8. Composition under item 1, in which each copolymer comprises ethylene and hexene.

9. The composition according to p. 1, having a density according to ISO 1183 at 23°C in the range from 920 to 940 kg/m3preferably from 925 to 935 kg/m3.

10. Polyethylene moulding composition having a multimodal molecular weight distribution, a density according to ISO 1183 at 23°C in the range of 920 to 960 kg/m3and VKT190/2according to ISO 1133 in the range of from 0.05 to 10 g/10 min, with the specified polyethylene molding composition comprises at least three fractions of the polymer of ethylene having different molecular weights:
A) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene with a low molecular weight, MFR:190/2according to ISO 1133 of from 50 to 1000 g/10 min;
B) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene with an average molecular weight, MFR:190/2less than 10 g/10 min; and
C) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene to high molecular weight, while the motor melt, defined according to ISO 1133 at 190°C and a load of 21.6 kg, PTR190/21less than the value of the fraction, in the range from 0.05 to 5 g/10 min,
provided that one of the fractions a, b and C is a homopolymer of ethylene, and at least one other component is a copolymer of ethylene with at least one C3-C10the co monomer;
and the composition has
- hardness shore D as measured by ASTM D2240-05 (15), at least 56,0;
- each faction copolymer contains comonomer C3-C10and the content of the co monomer is from 1 to 15% of the mass.

11. Composition according to any one of the preceding paragraphs.1-10, in which each fraction is obtained using a catalyst with the same type of active centers of polymerization.

12. The product, obtained by injection molding, blow molding or direct pressing, or the wire or cable containing a polyethylene composition according to any one of the preceding paragraphs.1-11.

13. A method of obtaining a composition according to any of the preceding paragraphs.1-11, comprising mixing
A) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene with a low molecular mass, with the mass-average molecular mass Mwin the range from 15 to 40 kg/mol;
B) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene with an average molecular weight, average the mass of molecular mass M win the range from 70 to 200 kg/mol; and
C) from 15 to 50 wt%. fraction homopolymer or copolymer of ethylene with a high molecular mass, with the mass-average molecular mass Mwin the range from 220 to 400 kg/mol,
provided that one of the fractions a, b and C is a homopolymer of ethylene and at least one other component is a copolymer of ethylene with at least one C3-C10the co monomer;
this composition has:
- multimodal molecular mass distribution;
the density according to ISO 1183 at 23°C in the range of 920 to 960 kg/m3;
- PTR190/2according to ISO 1133 in the range of from 0.05 to 10 g/10 min, and
- hardness shore D as measured by ASTM D2240-05 (15), at least 56,0;
- each faction copolymer contains comonomer C3-C10and the content of the co monomer is from 1 to 15% of the mass.



 

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18 cl, 5 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a PVC-free floor or wall covering comprising at least one layer of a thermoplastic composition. The composition contains a polymer matrix comprising at least two polymers and at least 100 pts.wt of least one filler per 100 pts.wt of the polymer(s). Said matrix contains 10-40 pts.wt of a polymer with carboxylic acid anhydride groups in amount of 0.5-3.1 wt %, and the other polymer of the matrix is selected from a group comprising EVA, EMA, EBA, EEA, EPM, EPDM, VLDPE, LLDPE, POE, POP and mixtures thereof, and has melt flow index between 0.6 and 3 g/10 min at 190°C and mass of 2.16 kg. The total amount of combined polymers in the composition is 100 pts.wt.

EFFECT: floor or wall covering obtained according to the invention preferably in form of rolls or tiles has improved residual indentation properties and is also suitable for recycling.

14 cl, 7 dwg, 9 tbl

FIELD: chemistry.

SUBSTANCE: coating comprises an adhesive sublayer of a thermoplastic adhesive and a functional layer of a nanostructured composite material based on polyethylene. The composite material of the functional layer has a polyethylene matrix and montmorillonite particles dispersed in the matrix in amount of 0.1-2 wt %.

EFFECT: improved physical and mechanical properties of the coating.

12 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a low-density ethylene polymer with a multimodal comonomer distribution, a method for production thereof and moulded articles, including films, made from said polymer. The multimodal polyethylene has a wide molecular weight distribution MWD in the range from 3 to 8 and contains two polymer components. The first polymer component is 70-95 wt % copolymer of ethylene with at least one C3-C20-α-olefin comonomer, having MWD less than 5, CDBI greater than 60% and high-load melt index (@21.6 kg, 190°C) of 10-100 g/10 min. The second polymer component is 5-30 wt % substantially homopolymeric polyethylene, having MWD greater than 10, CDBI greater than 80% and high-load melt index (@21.6 kg, 190°C) of 0.2-20 g/10 min. Said multimodal polyethylene is obtained in a single reactor using a catalyst system containing at least two catalysts in form of transition metal complexes.

EFFECT: polyethylene disclosed herein has considerably improved resistance to mechanical factors and excellent processing properties, which enable to avoid use of process additives when processing films.

13 cl, 4 dwg, 3 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to method of obtaining cross-linked pipe and to cross-linked pipe, which contains cross-linked polymer composition, containing cross-linked ethylene polymer. method of manufacturing cross-linked pipe includes: (i) polymerisation of ethylene non-obligatorily with one or several comonomers (comonomer) in presence of Ziegler-Natta catalyst with obtaining ethylene polymer, which contains carbon-carbon double bonds; ethylene polymer has: (A) linkability, expressed through the level of gel content, equal, at least, 50 wt %, according to the measurement of disc-shaped sample of cross-linked ethylene polymer (ASTMD 2765-01, Method A, extraction in decalin); or/and (B) content of carbon-carbon double bonds in a number higher than 0.2 carbon-carbon double bond/1000 carbon atoms, according to the measurement by FTIR method; and (ii) obtaining polymer composition, including, at least, 50% wt % of ethylene polymer; (iii) formation of pipe from composition, obtained at stage (ii); (iv) cross-linking pipe, obtained at stage (iii). Ethylene polymer represents ethylene homopolymer or ethylene copolymer with one or several comonomers, and is selected from elastomers (POE), plastomers (OPO) or very low density ethylene copolymers of (VLDPE), which cover the density range from 855 to 909 kg/m3, linear low density ethylene copolymers (LLDPE), which have density in the range from 910 to 930 kg/m3 (ISO 1183), medium density ethylene copolymers (MDPE), which have density in the range from 931 to 945 kg/m3, or high density polyethylenes (HDPE), which are selected from homo- or copolymers of ethylene, and which have density higher than 946 kg/m3. Cross-linked pipe consists of cross-linked polymer composition. Polymer composition before cross-linking includes, at least, 50 wt % of ethylene polymer, where ethylene polymer is obtained by polymerisation of ethylene optionally together with one or several comonomers (comonomer) in presence of Ziegler-Natta catalyst, where ethylene polymer contains carbon-carbon double bonds in a number higher than 0.4 carbon-carbon double bond/1000 carbon atoms, according to the measurement by FTIR method, where ethylene polymer has linkability, expressed through the level of gel content, equal, at least, 50 wt %, according to the measurement for disc-shaped sample of cross-linked ethylene polymer (ASTMD 2765-01, Method A, extraction in decalin) and has MFR2 from 0.01 to 5.0 g/10 min, Mn/Mw from 0.1 to 20.0 g/10 min, and where ethylene polymer represents ethylene homopolymer or ethylene copolymer with one or several copolymers, and is selected from linear low density ethylene copolymers (LLDPE), which have density in the range from 910 to 930 kg/m3 (ISO 1183), medium density ethylene copolymers (MDPE), which have density in the range from 931 to 945 kg/m3, or high density polyethylenes (HDPE), which are selected from ethylene homo- or copolymers and which have density higher than 946 kg/m3.

EFFECT: improvement of material properties.

18 cl, 5 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to composition of polymodal polyethylene, which has improved resistance to cracking under impact of environment and higher rate of crystallisation. Composition contains ethylene homopolymer, two ethylene copolymers and nucleating agent in amount from 20 to 5000 ppm in terms of entire polyethylene composition. Second ethylene copolymer has higher molecular weight than first ethylene copolymer, and first ethylene copolymer has higher molecular weight than ethylene homopolymer.

EFFECT: obtained polyethylene composition possesses resistance to cracking under impact of environment (ASTM D1693, Conditions B, in 100% Igepal) more than or equal 40 days, and half time of crystallisation lower than or equal 70% of half time of crystallisation of polymodal polyethylene without nucleating agent.

12 cl, 1 tbl, 12 ex

FIELD: chemistry.

SUBSTANCE: claimed invention relates to method of obtaining copolymers of ethylene and α-olefin and to copolymers, obtained by claimed method, which can be adapted to wide number of various applications, including film, electric wires and thermomelting glues. Copolymers have content of (C3-C18) α-olefin from 10 wt % to 45 wt % of copolymer, molecular-weight distribution (Mw/Mn) from 1.5 to 3.0 and density 0.850-0.900 g/cm3. Method of obtaining copolymers of ethylene and (C3-C18) α-olefin is realised in solution at temperature of copolymerisation from 80°C to 140°C in single reactor or in continuous reactors, connected successively or in parallel way for 2-stage reactions. Catalytic composition contains activator and catalyst, composition of which includes compound with transition metal, represented by chemical formula (1) , where X2 represents and the remaining values of radicals are given in the invention formula.

EFFECT: method of copolymerisation of ethylene with α-olefin makes it possible to obtain copolymer, which has strict value of molecular-weight distribution and homogeneous distribution of density, with density not higher than 0,910 g/cm3, with high activity and excellent reaction activity on highly molecular α-olefin.

11 cl, 2 tbl, 2 dwg, 12 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a thermoplastic polyolefin composition for pressure moulding painted and flame pretreated articles. The composition contains a continuous phase (matrix) (M) of a propylene homopolymer or a propylene copolymer with weight content of the comonomer of not more than 20%, which form a dispersion phase (E) with characteristic viscosity of at least 2.2 dl/g, a first elastomer which is copolymer rubber based on ethylene-C3-C8-alpha-olefin, and a second elastomer, and inorganic filler. The second elastomer is different from the first elastomer and is a random copolymer based on ethylene/alpha-olefins, the composition of which includes ethylene and up to 45% of one or more C3-C8 alpha-olefins.

EFFECT: articles pressure moulded from the disclosed composition have low or no sensitivity to flame treatment during flame pretreatment before depositing a clean paint layer and also demonstrate high heat conductivity.

10 cl, 4 tbl, 15 ex

FIELD: chemistry.

SUBSTANCE: at the first stage a polymer material to be recycled is loaded into a cutting-compacting device, equipped with a mixing or crushing device, after which the polymer particles are continuously moved and heated in the cutting-compacting device. In order to neutralise the formed products of destruction or decomposition into the softened but not yet melted polymer added is a solid, powder-like, preferably mineral, filling agent, usually used for dilution or as a diluting agent, for instance chalk, diatomaceous earth, zinc oxide, talc, activated coal and/or carbonate, in particular calcium carbonate, in an amount, at least, corresponding to the expected acidic or basic impact. The mixture is continuously mixed, moved, if necessary, crushed and supported in the form of separate pieces or freely flowing for a definite time.

EFFECT: method makes it possible to effectively neutralise acidic and basic compounds, which results in the reduction of corrosion and increase of the service term of machines.

30 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a bimodal polyethylene high-density composition for obtaining products by pressure moulding, in particular caps and plugging means. The composition includes bimodal high-density polyethylene, a composition of an inorganic alpha-nucleating agent, a composition of a friction-reducing agent, representing amide of primary fatty acid, and a composition with one or more additives, selected from antioxidants, acid acceptors, pigments and UV-stabilisers. The application of bimodal polyethylene in a combination with the inorganic alpha-nucleating agent, in particular, with talc and behenamide, as the friction-reducing agent, makes it possible to obtain the moulding composition with an unexpected and synergic impact on crystallisation temperature, and the composition friction coefficient.

EFFECT: composition by the invention demonstrates higher crystallisation temperature and lower friction coefficient.

14 cl, 5 tbl

FIELD: chemistry.

SUBSTANCE: claimed invention relates to a solvent-free polyethylene film, which can be applied, for instance, in membranes, packing, and ballistics. The polyethylene film has a ratio between the strength in the first direction in the film plane and the strength in the second direction in the film plane, perpendicular to the first direction, in the range of 0.1-10:1. The strength in, at least, one direction in the film plane constitutes not less than 0.2 GPa. The weight-average molecular weight of polyethylene constitutes not less than 500000 g/mol, and a value of ratio Mw/Mn does not exceed 6. The method of the said film manufacturing is performed by processing an initial polymer of polyethylene UHMWPE with the weight-average molecular weight of not less than 500000 g/mol by elastic shear modulus, determined immediately after melting at 160°C, not higher than 1.4 MPa, and a value of Mw/Mn ratio not higher than 6. Processing is carried out by pressing in the absence of a solvent. A stage of extraction is performed in such conditions that the temperature of the polymer film half-product does not exceed the temperature of the polymer melting at any time moment. During extraction the force is applied to the polymer film half-product in the first direction and in the second direction, which is perpendicular to the first direction.

EFFECT: film, possessing high strength more than in one direction in the film plane, is obtained.

15 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to use of a stabilised composition based on an ethylene homo- or copolymer containing a combination of at least two sterically hindered amine compounds for making plastic articles for transportation and storage of esters of vegetable oil, preferably plastic fuel tanks for motor vehicles, including single-layer or multi-layer articles. At least one of the sterically hindered amine compounds is selected from compounds having the chemical formula:

and a chemical formula:

, where n is an integer ranging from 2 to 20. The invention also describes a plastic article and components for transportation and storage of liquid fuels, including biodiesel fuel.

EFFECT: high resistance to thermal oxidative decomposition caused by presence of liquid fuels, such as biodiesel fuel, including esters of vegetable oils, together with oxygen.

7 cl, 3 tbl, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to heat sealable films, laminated materials, membranes or other polymer articles based on cross-linked polymers, having rubber-like heat resistance (heat deformation) and dimensional stability at temperature higher than the melting point of the polymer, while maintaining properties of the compound obtained by heat sealing (heat-adhesive compound). The heat sealable film contains at least one layer formed from a composition containing A) at least one polymer selected from a group comprising i) an ethylene-based polymer, ii) an ethylene/α-olefin/diene interpolymer and iii) a polymer based on a C4-C10 olefin, and B) at least one polymer selected from a group consisting of a propylene/ethylene interpolymer and a propylene/α-olefin interpolymer. Said film is cross-linked using radiation and/or chemical reagents.

EFFECT: polymer films and articles disclosed herein have improved mechanical properties and improved puncture resistance and can be used for high-temperature filling and processing in thermal or radiation sterilisation conditions, and as stretch films and shrink films.

13 cl, 9 dwg, 8 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to method of obtaining cross-linked pipe and to cross-linked pipe, which contains cross-linked polymer composition, containing cross-linked ethylene polymer. method of manufacturing cross-linked pipe includes: (i) polymerisation of ethylene non-obligatorily with one or several comonomers (comonomer) in presence of Ziegler-Natta catalyst with obtaining ethylene polymer, which contains carbon-carbon double bonds; ethylene polymer has: (A) linkability, expressed through the level of gel content, equal, at least, 50 wt %, according to the measurement of disc-shaped sample of cross-linked ethylene polymer (ASTMD 2765-01, Method A, extraction in decalin); or/and (B) content of carbon-carbon double bonds in a number higher than 0.2 carbon-carbon double bond/1000 carbon atoms, according to the measurement by FTIR method; and (ii) obtaining polymer composition, including, at least, 50% wt % of ethylene polymer; (iii) formation of pipe from composition, obtained at stage (ii); (iv) cross-linking pipe, obtained at stage (iii). Ethylene polymer represents ethylene homopolymer or ethylene copolymer with one or several comonomers, and is selected from elastomers (POE), plastomers (OPO) or very low density ethylene copolymers of (VLDPE), which cover the density range from 855 to 909 kg/m3, linear low density ethylene copolymers (LLDPE), which have density in the range from 910 to 930 kg/m3 (ISO 1183), medium density ethylene copolymers (MDPE), which have density in the range from 931 to 945 kg/m3, or high density polyethylenes (HDPE), which are selected from homo- or copolymers of ethylene, and which have density higher than 946 kg/m3. Cross-linked pipe consists of cross-linked polymer composition. Polymer composition before cross-linking includes, at least, 50 wt % of ethylene polymer, where ethylene polymer is obtained by polymerisation of ethylene optionally together with one or several comonomers (comonomer) in presence of Ziegler-Natta catalyst, where ethylene polymer contains carbon-carbon double bonds in a number higher than 0.4 carbon-carbon double bond/1000 carbon atoms, according to the measurement by FTIR method, where ethylene polymer has linkability, expressed through the level of gel content, equal, at least, 50 wt %, according to the measurement for disc-shaped sample of cross-linked ethylene polymer (ASTMD 2765-01, Method A, extraction in decalin) and has MFR2 from 0.01 to 5.0 g/10 min, Mn/Mw from 0.1 to 20.0 g/10 min, and where ethylene polymer represents ethylene homopolymer or ethylene copolymer with one or several copolymers, and is selected from linear low density ethylene copolymers (LLDPE), which have density in the range from 910 to 930 kg/m3 (ISO 1183), medium density ethylene copolymers (MDPE), which have density in the range from 931 to 945 kg/m3, or high density polyethylenes (HDPE), which are selected from ethylene homo- or copolymers and which have density higher than 946 kg/m3.

EFFECT: improvement of material properties.

18 cl, 5 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to crosslinkable compositions based on polyolefins and copolymers thereof and modifiers for producing silanol-crosslinkable polymer compositions which can be used to produce film coatings, insulation and sheaths for cables and conductors for different purposes. The silanol-crosslinkable composition contains polyolefin, vinyl alkoxysilane, organic peroxide and a sheet silicate which is modified with resorcinol resin with ratio of the resorcinol resin to the sheet silicate of 6:10 pts.wt.

EFFECT: improved operational characteristics, shorter crosslinking time and longer property retention time.

6 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to a heterophase propylene composition for making articles by injection moulding, as well as a composition for improving strength of polypropylene at low temperatures. The composition contains a polypropylene matrix, an elastomer copolymer containing ethylene links, at least one C3-C20 α-olefin and optionally an unconjugated diene, high-density polyethylene which is bimodal or multimodal polyethylene and inorganic filler.

EFFECT: disclosed heterophase polypropylene has acceptable impact characteristics at -40°C without loss of hardness.

14 cl, 3 tbl, 14 ex

Multimodal polymer // 2496794

FIELD: chemistry.

SUBSTANCE: invention relates to cross-linked polyethylene, a method of producing cross-linked polyethylene, as well as cross-linked polyethylene and articles, preferably pipes, made therefrom. The cross-linked polyethylene contains a multimodal ethylene polymer with density lower than 950 kg/m3, which is obtained via polymerisation in the presence of a catalyst with one active centre and having STR21 from 2 to 15 g/10 min and shear thinning index PSV2.7/210 from 5 to 10.

EFFECT: providing a polymer composition with improved cross-linking capacity, eg with cross-linking degree of at least 70%, flexibility and good processability.

14 cl, 3 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: composition contains a high-molecular weight polyethylene component and a low-molecular weight polyethylene component, and has density of 0.940 g/cm3 or higher and melt strength of 18 cN or higher. The ratio of the weight-average molecular weight of the high-molecular weight component to the weight-average molecular weight of the low-molecular weight component in the composition is greater than 15:1 and less than 28:1, the high- and low-molecular weight polyethylene components being formed by polymerisation in one reactor. The composition is classified as PE 100 material and has the appropriate balance of properties. A tube made from the composition, subjected to an internal strength test, has extrapolated stress of 10 MPa or higher, when the internal strength curve of the tube is extrapolated to 50 or 100 years according to ISO 9080:2003(E).

EFFECT: improved operational characteristics.

22 cl, 3 dwg, 6 tbl

FIELD: rubber materials, polymers.

SUBSTANCE: invention relates to composition based on ethylene-propylene or ethylene-propylenediene rubber and copolymer of ethylene and octyne that is used as an inter-strand filling agent in cables. Method involves preparing the composition containing the following components, mas. p. p.: rubber, 100; copolymer of ethylene and octyne, 25-55; paraffin, 50-170; stearic acid, 4-30; dibutyl phthalate, 4-25; chalk, 500-1600. The composition can comprise aluminum trihydrate additionally, 180-270 mas. p. p. per 100 mas. p. p. of rubber. Invention provides enhancing electric, physical and technological indices of materials used for filling cable articles.

EFFECT: improved and valuable properties of composition.

1 ex

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