Method of producing polyolefin films

FIELD: process engineering.

SUBSTANCE: invention relates to production of films from superhigh-molecular polyolefin. Proposed method comprises affecting initial superhigh-molecular polyolefin with weighted mean molecular weight of, at leas 500000 g/mol in the form of compacted powder by isobaric press. Besides, compacted polyolefin of rolling stage is subjected to definite processing. Also, it is stretched at such conditions whereat polymer processing temperature does no up to magnitude exceeding its fusion point at no point whatsoever.

EFFECT: high-quality films from superhigh-molecular polyolefin.

15 cl, 2 dwg

 

The present invention relates to a method for producing films of ultrahigh molecular weight polyolefin.

US patent # US 5091133 describes a method of producing sheets of ultra-high molecular weight polyolefin with the stages of the introduction of the polyolefin powder between a combination of endless belts located in the ratio of reciprocating motion in opposite directions, forming the extrusion of polyolefin powder at a temperature lower than the melting point of the polyolefin powder, by means of a device for pressing, holding, at the same time polyolefin powder between the endless conveyor belts, then rolling and stretching the obtained polyolefin, molded by pressing.

European patent EP 0467323 describes a method of obtaining a colored films of ultrahigh molecular weight polyethylene, where the powdery ultrahigh molecular weight polyethylene, which is then subjected to compaction-spinning and stretching, add dye.

U.S. patent No. 4879076 describes a method of obtaining a plastic material by using a method including compression and tension, where the seal is carried out in an extruder or in an indefinite press.

Although the method described in U.S. patent No. 5091133 above, gives a product with acceptable properties is, discovered that there are still room for improvements. In particular, upon receipt of the films with a very high ratio stretching method, as described in U.S. patent No. 5091133, can lead to products with heterogeneous quality. Irregularities will, among other things, limit the strength of the film to tear.

Accordingly, there is a need for a method of producing films of ultrahigh molecular weight polyolefin, which yields a product with a higher homogeneity, higher tensile strength and other desirable physical properties. The method in accordance with the present invention also provides a wider tape.

The present invention provides such a method. Thus, the present invention is directed to a method of obtaining a film of ultra-high molecular weight polyethylene, which includes stages

- exposure to the original ultra-high molecular weight polyolefin with srednevekovoi molecular weight of at least 500,000 grams/mole in powdered form under seal using Isobaric press

- impact on compacted polyolefin stage of rolling and at least one stage stretching under such conditions, during processing of the polymer in either single point temperature does not rise to the meant is I above its melting temperature.

The method in accordance with the present invention allows to obtain a polymer film high quality, with high uniformity. The resulting product is of consistent quality, high strength, high uniformity in width and a uniform density distribution. Other advantages of the present method will become apparent from the additional description below.

It is noted that U.S. patent No. 4353855 describes a method of obtaining plastic products, not having the stress, through the seal of the polymer powder in the form of using a pressure exceeding the yield strength. However, the stage of pressing is carried out at a temperature above the melting temperature of the polymer, and the subsequent stage stretching is carried out.

The present invention will be described in more detail below.

A number of embodiments of the present invention is described in detail and as only examples with reference to the accompanying drawings.

Figure 1 results the first version of the implementation of the configuration Isobaric press suitable for use in the present invention.

Figure 2 results of the second variant of implementation of the configuration Isobaric press suitable for use in the present invention.

In the first stage of the method in accordance with the present invention the polyolefin powder upl is Taeda in Isobaric press. Isobaric press is a press where pressure is applied to the material that needs to be compacted, is a constant, independent of the thickness of the material which shall be compacted. It is the opposite of isochoric presses, where the thickness of the final product is constant and applied pressure varies with the thickness of the material which shall be compacted. Isobaric press known in the field, and are commercially available, for example, from Hymmen GmbH, Germany. However, the use of Isobaric press in the method of producing films of ultrahigh molecular weight polyolefin has not previously been described.

In one of the embodiments of the present invention used Isobaric press has such a pressure distribution that the ratio of pressure to density of the sealing material is constant at each point of the material which shall be compacted. It should be noted that the press can contain multiple zones of compression that can operate at different pressures.

Isobaric press suitable for use in the present invention, will now be described with reference to Figure 1. It is noted that, as will be obvious to the person skilled in the art, various preferential options for implementation, discussed below, are not limited to competitive advantage is to maintain the device. In figure 1 the device comprises two pairs of rolls 1, 2, and 3, 4 and a pair of endless conveyor belts 12, 13 located in the state of tension in the ratio of reciprocating movement in opposite directions with rolls 1-4. Pairs of opposite cushions 5, 6, 7 and 8 of the pressing installed inside the conveyor belts 12, 13, and the polyolefin is placed between the conveyor belts 12, 13, and conveyor belts 12, 13 carry the pressure on the polyolefin. Cushions 5, 6, 7 and 8 of the pressing preferably contain (inside) gaseous and/or liquid medium for exerting pressure on the polyolefin. As the environment can be used, for example, oil and/or air. You can use one pair of pillows pressing or many pairs of pillows pressing. Due to the fact that the environment can be heated, the temperature of the polyolefin during pressing can be controlled very precisely. Actually, to obtain the advantages associated with the present invention, good temperature control is essential, as will be discussed below. Alternatively, the heated environment inside the cushions 5, 6, 7 and 8 of the pressing cushion 5, 6, 7 and 8, the pressing can be heated using an external heating device (for example, microwave or infrared). It is also possible cooling of the compacted material pore the STV active or inactive cooling with additional pillows (16, 17 figure 2) pressing to prevent build-up on the endless conveyor belts 12, 13. Using Isobaric press fitted pillows 1-4 pressing for the application of pressure to the polyolefin, ensures uniform pressure across the width and length of the pressing zone and for this reason represents a preferred implementation of the present invention, as will be explained in more detail below.

In figure 1 of the original polyolefin powder can be entered from the bunker on the endless conveyor belt 12, as a rule, before the blade unit 11. At the stage of pressing the original polyolefin 20 on the conveyor belt is preheated to improve the ductility at (hot) pressing using a plate 9 for preheating. Pre-heating the polyolefin powder causes an increase in the static charge of the powder particles, which will have a negative effect on the uniformity of the layer of polyolefin powder. To overcome this static charge powder dispense cold endless conveyor belt 12. This endless conveyor belt 12 is heated in the nip, which means that before dosing polyolefin powder is necessary cooling conveyor belt 12. Continuous heating and cooling of the pipeline, the first tape 12 will cause high internal tension in the conveyor belt and cause frequent failures of conveyor belt 12. In a preferred embodiment of the present invention to eliminate the cycle of heating and cooling conveyor belt 12, the polyolefin powder is metered directly onto the conveyor belt 12, but on a secondary conveyor belt 10 passing between the conveyor belts 12, 13. Auxiliary conveyor belt 10 is heated by means of a heating plate 9 and the temperature of the conveyor belts 12, 13 to increase the temperature of the polyolefin above the softening temperature before entering into the press area. The heated polyolefin on the auxiliary conveyor belt 10 to be introduced into the gap of the press with double conveyor belt. When the polyolefin is compressed, thus formed sheet compacted polyolefin is fed to the roller 14. Auxiliary conveyor belt 10 is wound on the roller 15.

Figure 2 shows another variant of implementation of the Isobaric press suitable for use in the present invention. In this embodiment, in addition to heated cushions 5, 6, 7 and 8, the press contains extra pillows 16, 17, which can be used for cooling the compacted polyolefin through active or inactive cooling to prevent build-up on the endless conveyor belt. In one embodiment, implementation Figure 2 heating the plate 9 is missing. Instead, the temperature of the polyolefin determines the temperature of the conveyor belts 12, 13. In this embodiment, the blade unit 11 is located higher than the figure 1, so you get a thicker layer of powder than in the first case. Two additional guide roll 18 and 19 are applied to polyolefin 20 in the gap of the press area.

In a preferred embodiment of the present invention, in order to make easier the release of trapped air from the layer of polyolefin powder into the gap, the input angle support at 4.5°, preferably 3°, more preferably in the range between 2.5° and 0.5°, in particular about 1.5°.

Caught in the gap layer polyolefin powder is compressed between the endless conveyor belts in the zone (or zones) pressing. Depending on the bulk density polyolefin powder, stage of pressing can take place in one area of the Isobaric pressing the press, or can be used in several areas of pressing, the pressure at each nip is higher than in the previous nip. In a specific embodiment, the present invention Isobaric press contains two zones of compaction, where the first pressing zone operates at a pressure of at most 10 bar, for example, between 2 and 10 bar, more specifically, between the 3 is 8 bar, while the second pressing zone operates at a pressure higher than 10 bar, for example, up to 80 bar. It should be noted that this represents the use of Isobaric press, which allows the use of such high pressure in combination with good temperature control. This implementation is a particular interest, when the polyolefin powder has a low bulk density, as will be explained in more detail below.

In one embodiment of the method in accordance with the present invention, use of the press with an effective width of at least 250 mm, in particular, of a width of at least 400 mm, more specifically at least 1100 mm wide press allows obtaining a relatively wide film, at the same time, using high-ratio stretching.

Applied pressure is determined by the density of the sealing material, which must be achieved. To allow appropriate further processing of the material, as a rule, it is necessary to compact the material to a density equal to at least 95% of theoretical density of the polymer, in particular at least 97%, more particularly at least 98%.

Found that if the material is compacted to a density of less than 95% of theoretical density of the polymer material is ial group may be too fragile to allow stretching of the material. In addition, the cohesion and strength of the raw material may be too low to allow for appropriate further processing.

For example, when the polyolefin is a polyethylene, theoretical density of the polymer 0.97 g/cm3. Accordingly, the applied pressure is generally selected so that the density of the compacted material, at least, is 0.92 g/cm3. More specifically, the applied pressure is chosen so that the density of the compacted material, at least, is 0.93 g/cm3. More specifically, the applied pressure is chosen so that the density of the compacted material is at least 0,94 g/cm3.

As a rule, apply pressure on the under seal is at least 5 bar, in particular at least 10 bar, more specifically at least 20 bar. Depending on the properties of the polymer, the pressure required to obtain the specified density may be relatively high. In some embodiments, the implementation of the applied pressure under seal is at least 25 bar, in particular at least 30 bar, more specifically, at least 35 bar, more particularly of at least 40 bar, more particularly of at least 45 the ar or at least 50 bar. Values greater than 80 bar, as a rule, are not required.

Allowing obtaining the required density, compaction takes place at elevated temperature, specifically at a temperature above the softening temperature of the polymer on Vicat and below the temperature of unlimited melting of the polymer. For reasons of processing efficiency, as a rule, it is preferable to carry out stage seal relatively close to the temperature of unlimited melting of the polymer. This will simplify the seal and will result in a material with a higher cohesion. Material with higher cohesion will, in turn, have better tensile properties that will produce films with improved properties, like tensile strength. However, an important feature of the present invention is that the polymeric material with high strength and high modulus temperature during sealing is maintained below the natural temperature of the polymer melt. This material will not be obtained when the product melts during compaction.

In the method in accordance with the present invention stage seal, as a rule, carried out at a temperature at least 1°C below the temperature of unlimited melting of the polymer. Depending on riroda polymer may be possible the implementation stage of compaction temperature, at least 3°C below the natural temperature of unlimited melting of the polymer, more specifically at least 5°C below the melting temperature of the polymer. When possible the implementation of the seal at a temperature more than 1°C below the temperature of the natural melting of the polymer, it is preferred for reasons connected with the efficiency of the method. As a rule, the stage of compaction is carried out at a temperature of at most 40°C below the natural temperature of the polymer melt, in particular at most 30°C below the natural melting point of the polymer, more particularly at most 10°C below.

In a preferred embodiment of the method in accordance with the present invention the temperature under seal support standing in the window of temperatures 2°C, in particular, in the window of the temperature 1°C. This results in a product with improved final properties. As shown above, that can be obtained such a narrow window of temperatures, is one of the characteristics associated with the use of Isobaric press.

The polymer is provided in powder form. The respective powders contain particles may have a particle size of up to 1000 microns, preferably up to 500 microns, more specifically, up to 250 microns. The particles preferably they shall have the particle size, at least 1 micron, more specifically at least 10 microns. The distribution of particle sizes can be determined using laser diffraction (PSD, Sympatec Quixel) as follows. The sample was dispersed in water containing a surfactant, and treated with ultrasound for 30 seconds to remove agglomerates/weaves. The sample is pumped through the laser beam and detects the scattered light. The amount of diffraction of light is a measure for the particle size.

Depending on the nature of the initial polymer polymer powder typically has a bulk density in the range between 0.08 and 0.6 g/cm3. Bulk density can be determined according to ASTM-D1895. Approximation of average quality for this value can be obtained as follows. A sample of UHMWPE powder is poured into the beaker with a volume of exactly 100 ml After removal of the excess material defining the weight of the contents of the Cup and calculate the bulk density.

Thus, the bulk density is a measure of the percentage of air present in the polymer powder. The percentage of air present in the polymer powder can be calculated by the bulk density and the density of the polymer using the following formula:

The percentage of air=100% (1-bulk density/density polymer)

As a rule, the percentage of air in the polymer powder, used in the method in accordance with the present invention, is in the range between 30 and 90%. In one of the embodiments of the present invention, the source powder is the percentage of air in the range between 60%and 40%. In another embodiment of the method in accordance with the present invention, the source powder is the percentage of air more than 60%, in particular more than 65%, more specifically, more than 70%. Typically, the powders with such a high percentage of air, as it is considered difficult to process in the form of polymer films, and discovered that the present invention allows the processing of such materials with a low density.

For example, when the polymer is a high molecular weight polyethylene, bulk density will typically be between 0.08 and 0.6 g/cm3. In one of the embodiments is used, the polyolefin, in particular, high molecular weight polyethylene, which has a relatively low bulk density compared to the bulk density of conventional polyolefins, particularly high molecular weight polyethylene. More specifically, the polyolefin used in the method in accordance with the present invention may have a bulk density below 0.50 g/cm3in particular, below 0.25 g/cm3more specifically, below 0.18 g/cm3more specifically, below 0,13 g/cm3. This item is igodit, for example, to obtain nepetalactone ultra-high molecular weight, which will be discussed in more detail below.

In the method according to the present invention stage of compaction is carried out for the Association of polymer particles in one object, for example, in the form of uterine sheet. Uterine sheet is exposed to the stage of rolling, and then, under tension. Stage stretching is carried out for imparting orientation to the polymer and to obtain the final product. Stage seals and stage stretching is carried out in directions perpendicular to each other. At the stage of rolling, compaction combined with some stretching in the direction perpendicular to the seal.

Stage stretching in the method in accordance with the present invention carried out to obtain a polymer film. Stage stretching can be performed at one or more stages of method common to this area. The corresponding method includes conducting film on one or several stages on a set of rolls, which both are rolling in direction along the way, while the second roller rolls faster than the first roller. Stretching can take place over a hot stove or in an air circulating oven.

Typically, in the method in accordance with the present invention stage stretching the deposits will be carried out under such conditions, what is the General attitude of stretching, at least 30, particularly at least 50. Depending on the nature of the polymer, it may be possible and/or desirable to use higher relations sprains, more specifically at least 80, even more specifically at least 100, even more specifically, at least 120, even more specifically, at least 140, even more specifically at least 160. Found in particular that if these high relations stretching of the advantages of the present invention will be more pronounced.

The General attitude of the strain is defined as the cross-sectional area compacted sheet, divided by the cross-section of the laminated film obtained from this compacted sheet.

In the method in accordance with the present invention stage stretching, as a rule, carried out at a temperature at least 1°C below the melting temperature of the polymer under the conditions of the method. As is well known to specialists in this field, the melting point of the polymer may depend on the constraints under which they are. This means that the melting temperature under the conditions of method may vary from case to case. It can easily be determined as the temperature where the tension stress in the way drops sharply. Depending on the nature of the polymer is, may be possible the implementation stage stretching at a temperature at least 3°C below the melting temperature of the polymer under the conditions of the method, more specifically at least 5°C below the melting temperature of the polymer under the conditions of the method. Generally, stage stretching is carried out at a temperature of at most 30°C below the melting temperature of the polymer under the conditions, in particular at most 20°C below the melting temperature of the polymer under the conditions of the method, more specifically, at most 15°C below.

In one of the embodiments, the polymer is an ultra-high molecular weight polyethylene (UHMWPE) with srednevekovoi molecular weight (Mw)equal to at least 500,000 grams/mole, in particular within between 1,106g/mol and 1,108grams/mol. The distribution of molecular masses and average molecular weight (Mw, Mn, Mz) of the polymer can be determined according to ASTM D 6474-99 at a temperature of 160°C using 1,2,4-trichlorobenzene (TCB) as solvent. Can be used corresponding chromatographic equipment (PL-GPC220 from Polymer Laboratories), including a device for high-temperature sample preparation (PL-SP260). The system is calibrated using sixteen polystyrene standards (Mw/Mn <1,1) in the range of molecular masses from 5·103up to 8·10 grams/mole.

The distribution of molecular mass can also be determined using the rheology of the melt. Before measurement, the sample of polyethylene, to which is added 0.5 wt% of an antioxidant, such as IRGANOX 1010, to prevent thermo-oxidative degradation must first specalist at 50°C and 200 bar. Disks with a diameter of 8 mm and a thickness of 1 mm obtained from sintered polyethylene, fast heat up (~30°C/min) to a temperature much higher than the equilibrium melting temperature in the rheometer, in nitrogen atmosphere. For example, the disk is maintained at 180°C for two hours or more. Slippage between the sample and the disk rheometer can be monitored with an oscilloscope. During the dynamic experiments two output signals from the rheometer, i.e. one signal corresponding to a sinusoidal deformation, and another signal corresponding to the result from the response voltage, continuously monitored with an oscilloscope. Excellent sinusoidal feedback voltage, which can be obtained at low strain values, is indicative of the absence of slippage between the sample and the disk.

The rheometric can be performed using a parallel-plate rheometer, such as a Rheometrics RMS 800 from TA Instruments. Software Orchestrator Software supplied by TA Instruments, kotoryjraspolagaet algorithm Mead, can be used to determine the molar mass and distribution of molar masses of data on the dependence of shear modulus on frequency defined for the polymer melt. Data are obtained under isothermal conditions in the range between 160 and 220°C. To obtain a good fit should be selected angular region of frequencies in the range between 0.001 and 100 rad/sec and area of permanent deformation in the linear viscoelastic region between 0.5 and 2%. The superposition of the time-temperature is applied at the reference temperature of 190°C. To determine the shear modulus lower than the frequency of 0.001 (rad/sec) can be carried out experiments with stress relaxation. In experiments with stress relaxation, applied and recorded one non-stationary deformation (warp speed) for polymer melt at a fixed temperature on the sample, and record the time-dependent attenuation of the voltage.

The temperature of the natural melting of the original polymer is in the range between 138 and 142°C and can be easily determined by the person skilled in the art. Using the values shown above, this allows the calculation of the appropriate working temperature.

Determination of the melting temperature can be carried out using a DSC (differential scanning calorimetry) nitrogen in the temperature range from +30 to +180°C the rate of temperature increase of 10°C/minute. The maximum of the largest endothermic peak in the region from 80 to 170°C is estimated to herein as the melting temperature.

UHMWPE, which is used in the preferred embodiment of the method in accordance with the present invention may be a homopolymer of ethylene or copolymer of ethylene with co monomer that is another alpha-olefin or cyclic olefin, both, as a rule, with the number of carbon atoms between 3 and 20. Examples include propene, 1-butene, 1-penten, 1-hexene, 1-hepten, 1-octene, cyclohexene, and the like. The use of dienes having up to 20 carbon atoms, is also possible, for example, butadiene or 1-4 hexadiene. Number (other than ethylene) alpha-olefin in the ethylene homopolymer or copolymer used in the method in accordance with the present invention, is preferably at most 10 mole%, preferably at most 5 mole%, more preferably at most 1 mole%. If use (other than ethylene) alpha-olefin he usually present in amounts of at least about 0.001 mole%, in particular at least 0.01 mole%, more particularly at least 0.1% mol. Obviously, the ranges given above for the source material, also belong to the final polymer film.

Pic is b in accordance with the present invention is carried out in the solid state. The final polymer film has a polymer content of the solvent is less than 0.05 wt%, in particular less than 0.025% mass, more specifically, less than 0.01% of the mass.

The film in accordance with the present invention is a three-dimensional object, which is characterized by the fact that two of its size is much larger than the third. More specifically, the relationship between the second smallest size, the width of the film, and the smallest size, film thickness, is at least 50.

In one of its embodiments, the method in accordance with the present invention is suitable for fabricating films of UHMWPE with a tensile strength of at least 1.0 GPA, a strain energy at break of at least 15 j/g and a Mw of at least 500,000 grams/mole.

Tensile strength is determined according to ASTM D882-00. Depending on the relationship stretching temperature and the stretching can be obtained tensile strength of at least 1.3 HPa at least a 1.5 GPA, or at least a 1.7 GPA. In some embodiments, the implementation can be derived materials with a tensile strength of at least a 2.0 GPA. Sometimes there can be obtained a tensile strength of at least a 2.5 GPA, in particular at least a 3.0 GPA, more specifically, at least a 3.5 GPA. Can also be obtained tensile strength, at m is re, 4 HPa.

The strain energy at break is determined in accordance with ASTM D882-00 using strain rate 50%/min It is calculated by integrating the energy per unit mass under the curve tension-deformation. Depending on the relationship of strain can be obtained film in accordance with the present invention, which have the strain energy at break of at least 15 j/g or strain energy at break of at least 25 j/g, In some embodiments, the implementation can be derived material with strain energy at break of at least 30 j/g, in particular at least 40 j/g HPa, more specifically at least 50 j/g HPa.

The elastic modulus of the UHMWPE film manufactured using the method in accordance with the present invention typically is at least 75 GPA. The module is determined according to ASTM D822-00. Depending on the relationship of strain can be obtained module, at least 85 GPA. In some embodiments, the implementation can be obtained modulus of at least 100 GPA, more specifically, at least 120 GPA. It is possible to obtain the elastic modulus of at least 140 GPA, or at least 150 GPA.

It may be preferable to ultra-high molecular weight polyethylene used in the present invention, had a relatively narrow distribution of mo is cularly masses. It is expressed by a ratio Mw (srednevekovoi molecular weight) to Mn (srednekamennogo molecular weight), which is at most 8. More specifically, the ratio Mw/Mn is at most 6, more specifically at most 4, more particularly at most 2.

In one embodiment, the implementation uses ultra-high molecular weight polyethylene, which has an elastic modulus shiftGN0determined directly after melting at 160°C, at most 1.4 MPa, in particular, 1.0 MPa, more specifically at most 0.9 MPa, still more particularly at most 0.8 MPa, more specifically at most 0.7 MPa. The expression "directly after melting" means that the elastic modulus shear determined immediately after the melting of the polymer, in particular, within 15 seconds after melting of the polymer. For this polymer meltGN0as a rule, increases from 0.6 to 2.0 MPa in one, two or more hours, depending on the molar mass of the polymer.GN0represents the elastic modulus of shear in the field of elastomeric cards is. It is associated with an average molecular weight between weaves Me, which, in turn, is inversely proportional to the density of the weave. In thermodynamically stable melt having a homogeneous distribution of binding is Me can be calculated from theGN0using the formulaGN0=gNρRT/Me,where gNis a numerical coefficient, defined as 1, is the density in g/cm3, R is the universal gas constant and T represents the absolute temperature in degrees K. the Low modulus of elasticity shear directly after melting corresponds to a large stretching of the polymer between the weaves and, thus, a low level of weaves. A recognized method for studies of changesGN0during the formation of the weave is the same as described in the publications (Rastogi, S., Lippits, D., Peters, G., Graf, R., Yefeng, Y. and Spiess, H., "Heterogeneity in Polymer Melts from Melting of Polymer Crystals", Nature Materials, 4(8), 1st August 2005, 635-641 and PhD thesis Lippits, D. R., "Controlling the elting kinetics of polymers; a route to a new melt state", Eindhoven University of Technology, dated 6th March 2007, ISBN 978-90-386-0895-2). Found that the polymer of this type is attractive for ballistic purposes.

In a specific embodiment of the present invention, polyethylene is seperately UHMWPE. In the present description, seperately UHMWPE different srednevekovoi molecular weight (Mw)of at least 500,000 g/mol, Mw/Mn, at most 8, and the elastic modulus shiftGN0determined directly after melting at 160°C, at most 1.4 MPa. The preferred ranges given above for these parameters also apply for this option implementation.

When the polymer is a polymer with a modulus shiftGN0determined directly after melting at 160°C, at most 1.4 MPa, it can be obtained by using method of polymerization, where ethylene, optionally, in the presence of other monomers, as discussed above, is polymerized in the presence of one of the catalyst for polymerization at a temperature below the crystallization temperature of the polymer so that the polymer crystallizes direct what about after education. In particular, reaction conditions are chosen so that the rate of polymerization is lower than the rate of crystallization. These synthesis conditions cause the molecular chains to crystallize immediately upon their formation, leading rather to the emergence of a unique morphology, which is essentially different from that obtained from a solution or melt. Crystalline morphology that is created on the surface of the catalyst will depend largely on the relationship between the crystallization rate and the growth rate of the polymer. In addition, the temperature of the synthesis, which in this case represents the crystallization temperature, will strongly affect the morphology of the obtained powder of UHMWPE. In one of the embodiments the reaction temperature is in the range between -50 and +50°C, more specifically, between -15 and +30°C. the Ability to determine through routine trial and error what the temperature of the reaction corresponds to the combination with this type of catalyst, concentration of polymer and other parameters that affect the reaction, is within the knowledge of experts in this field.

To obtain neprednamerennogo UHMWPE is important that the centers of polymerization were far enough removed from each other to prevent the weave of polymer chains during synthesis. This can be done with used the eat one catalyst, which is homogeneous dispersed in the environment of crystallization at low concentrations. More specifically, the corresponding can be concentrations of less than 1·10-4mol catalyst per liter, in particular, less than 1·10-5mol of catalyst per liter of reaction medium. Single center catalyst media can also be used, as long as measures are taken to ensure that the active centers were far enough removed from each other to prevent substantial weave polymer during formation.

Appropriate methods of obtaining the original UHMWPE used in the present invention, well-known in this field. You can refer to, for example, in WO 01/21668 and US 20060142521.

(Seperately) UHMWPE used in the method in accordance with the present invention, preferably has a crystallinity according to DSC of at least 74%, more specifically at least 80%. The morphology of the films can be determined using differential scanning calorimetry (DSC), for example, on a Perkin Elmer DSC7. Thus, a sample with a known weight (2 mg) were heated from 30 to 180°C at 10°C / minute, maintained at 180°C for 5 minutes, then cooled at 10°C per minute. The results of this scan DSC can be depicted on the graph of dependence of the heat flux (mW or MJ/s; y-axis)against temperature (x-axis). The degree of crystallinity is measured using data from the heating part of the scan. The latent enthalpy of fusion ΔH (j/g) for the transition of the crystal in the melt is calculated by determining the area under the graph of temperature defined directly below the start of the main melting transition (endotherm), to a temperature just above the temperature where there is complete fusion. Then the calculated ΔH is compared with theoretical latent enthalpy of the phase transition (ΔHCequal to 293 j/g)determined for 100% crystalline PE with a melting point of approximately 140°C. the crystallinity Index according to DSC is expressed as a percentage of 100 (ΔH/ΔHC).

When the present invention is used seperately UHMWPE, the stage of compaction and rolling, as a rule, carried out at a temperature at least 1°C below the temperature of unlimited polymer melt, in particular at least 3°C below the temperature of unlimited melting polymer, still more specifically at least 5°C below the temperature of unlimited melting of the polymer. As a rule, the stage of compaction is carried out at a temperature of at most 40°C below the temperature of unlimited polymer melt, in particular at most 30°C below the temperature of unlimited melting p is limera, more specifically, at most 10°C. In the method of this variant implementation stage stretching, as a rule, carried out at a temperature at least 1°C below the melting temperature of the polymer under the conditions, in particular at least 3°C below the melting temperature of the polymer under the conditions of the method, more specifically at least 5°C below the melting temperature of the polymer under the conditions of the method. As is well known to specialists in this field, the melting point of the polymers may depend on constraints in which they are located. This means that the melting temperature under the conditions of method may vary from case to case. It can easily be defined as the temperature at which the tension stresses in the way drops sharply. Generally, stage stretching is carried out at a temperature of at most 30°C below the melting temperature of the polymer under the conditions, in particular at most 20°C below the melting temperature of the polymer under the conditions of the method, more specifically, at most 15°C below.

In one of the embodiments of the present invention, in particular, for neprednamerennogo polyethylene, stage of stretching comprises at least two individual stages of stretching, where the first stage stretching is carried out at a temperature lower than the second, which is optional, additional stages of stretching. In one embodiment, the implementation stage of stretching comprises at least two individual stages of stretching, where each next stage stretching is carried out at a temperature that is higher than the temperature of the previous stage stretching. As will be obvious to the person skilled in the art, this method can be carried out in such a way that the individual phases can be identified, for example, in the form of films, which impose on individual hot plates with a given temperature. The method can also be carried out in a continuous manner, where the film is exposed to a lower temperature at the beginning of the method, the stretching and the impact of higher temperature at the end of a way of stretching, the temperature gradient is applied between stages. This alternative implementation may, for example, be carried out by conducting film on a hot plate, which is provided with a temperature zones, where zone at the end of the hot plate closest to the sealing device has a lower temperature than the zone on the edge of the hot plate, the farthest from the sealing device. In one of the embodiments, the difference between the lowest temperature applied during the stage of stretching, and the highest temperature applied in EMA stage stretching, is at least 3°C, in particular at least 7°C, more particularly at least 10°C. generally, the difference between the lowest temperature applied during the stage of stretching, and the highest temperature applied during stage stretching is at most 30°C, in particular at most 25°C.

When polyethylene is seperately polyethylene, found that compared with the conventional processing of UHMWPE materials with a strength of at least 2 GPA can be obtained at higher strain rates. The rate of deformation is directly related to the performance of the equipment. For economic reasons it is important to produce the product at a deformation speed, as high as possible without adversely affecting the mechanical properties of the film. In particular, we discovered that it is possible to produce a material with strength at least 2 GPA by using method, where stage stretching, which is required to increase the strength of the product from 1.5 GPA, at least up to 2 HPa, is carried out at a speed of at least 4% per second. In the processing of conventional polyethylene impossible to carry out this stage of stretching at this speed. While in the processing of conventional UHMWPE, the initial stage of stretching, before coloring strength and, for example, 1 or 1.5 HPa, can be carried out at speeds above 4% in the second, final stage, necessary to increase the strength of the film to a value of 2 GPA or above must be carried out at speeds much below 4% in the second, because otherwise the film would collapse. In contrast, in the method in accordance with the present invention found that it is possible to stretch the intermediate film with a strength of 1.5 GPA at a speed of at least 4% per second, to obtain a material with strength at least 2 GPA. Other preferred values of strength refers to the fact that all that is stated above. Found that the rate applied at this stage, may be at least 5% per second, at least 7% per second, at least 10% per second, or even at least 15% in the second.

The strength of the film is linked to applied ratio of stretching. For this reason, this impact can also be expressed as follows. In one of the embodiments of the present invention, stage stretching method in accordance with the present invention may be carried out such that the phase of the stretching ratio, the stretching 80 to stretch at least 100, in particular at least 120, more specifically, at least 140, more specifically, at the ore, 160 at a speed of stretching of the above.

In another embodiment, stage stretching method in accordance with the present invention can be carried out in such a way that stage stretching from a material with modulus of 60 GPA to a material with a modulus of elasticity of at least 80 GPA, in particular at least 100 GPA, more specifically, at least 120 GPA of at least 140 GPA, or at least 150 GPA, is performed at the speed indicated above.

The person skilled in the art it is obvious that intermediate products with a strength of 1.5 GPA, with respect to the stretching 80 and/or modulus of 60 GPA, respectively, are used as a starting point for calculating that when you begin the stage of stretching at a high speed. This does not mean that is separately identifiable stage stretching, where the source is specified strength, the ratio of the strain or the elastic modulus. A product with these properties can be formed as an intermediate product during the stage of stretching. Then the ratio of the strain will be calculated back to product with the specified initial properties. Note that high speed stretching described above, depends on the requirements that all stages of stretching, including stage or a hundred the AI stretching at high speed, carried out at a temperature below the melting temperature of the polymer under the conditions of the method.

When used in the present invention seperately polyethylene, the resulting film may have a flat orientation f 200/110 at least 3. The flat orientation 200/110 Φ is defined as the ratio between the peak areas 200 and 110 in the picture of the x-ray diffraction (XRD) pattern of the tape, as defined in the geometry of reflection.

X-ray scattering at large angles (WAXS) is a technology that gives information about the crystal structure of the material. Methodology refers specifically to the analysis of the Bragg peaks in the scattering at large angles. The Bragg peaks arise from long-range structural ordering. The WAXS measurement gives the diffraction pattern, i.e., intensity as a function of diffraction angle 2θ (it represents the angle between the beam after diffraction and the primary beam). The flat orientation 200/110 gives information on the degree of orientation of crystal planes 200 and 110 with respect to the tape surface. For sample tape with high flat orientation 200/110 crystal plane 200 are strongly oriented parallel to the tape surface. Found that strong flat landmarks is the as a rule, is accompanied by high tensile strength and high strain energy at break. The ratio between the peak areas 200 and 110 for sample with disordered oriented crystallites is approximately 0.4. However, in strips, which are preferably used in one of the embodiments of the present invention, the crystallites index 200 preferably oriented parallel to the film surface, resulting in a higher value of the ratio of the peak areas 200/110 and, consequently, to a higher value of the parameter plane orientation.

The value of the parameter plane orientation 200/110 can be determined using x-ray diffractometer. Diffractometer Bruker-AXS D8, equipped with a focusing multilayer x-ray optics (mirror Goebel), giving radiation Cu-Kα (wavelength K=1,5418 Å), is suitable for use. Measuring conditions: 2 mm protivorechivaya slit 0.2 mm detector slit and generator settings of 40 kV, 35 mA. The sample tape is mounted on the sample holder, for example, with the help of some double sided tape for mounting. The preferred dimensions of the sample tape is 15 mm ×15 mm (length × width). Must be careful that the sample was aged completely flat and combined with the sample holder. The holder is of brazza sample tape then placed in D8 diffractometer in reflection geometry (with normal belt, perpendicular to the goniometer and perpendicular to the sample holder). The scanning range for the diffraction pattern is from 5° to 40° (2θ) with a step of 0.02° (2θ) and a counting time of 2 seconds per step. During the measurement, the sample holder rotates at a speed of 15 revolutions per minute around the normal to the ribbon, so that further alignment of the sample is not necessary. Then the intensity is measured as a function of diffraction angle 2θ. The area of the peaks of reflections for 200 and 110 define using standard software fit the profile, for example, Topas from Bruker-AXS. Because reflection for 200 and 110 represent individual peaks, the fitting process is simple and the selection and implementation of appropriate procedures fit is within the knowledge of the person skilled in the art. The flat orientation 200/110 is defined as the ratio between the peak areas 200 and 110. This parameter is a quantitative measure flat orientation 200/110.

As indicated above, in one of the embodiments of the films have the option of a flat orientation 200/110 at least 3. It may be preferable that this value was at least 4, more specifically, at least 5, or at least 7. Higher values, such as values, at least 10 or even at least 15 can the be particularly preferred. theoretical maximum value for this parameter is infinity, if the peak area 110 is equal to zero. High values for the parameter plane orientation 200/110 often accompanied by high values of strength and strain energy at break.

In one of the embodiments the width of the film, as a rule, is at least 5 mm, in particular at least 10 mm, more specifically at least 20 mm, more particularly at least 40 mm. film Width, as a rule, is at most 200 mm, film Thickness, as a rule, is at least 8 μm, in particular at least 10 microns. The film thickness, as a rule, is at most 150 μm, more particularly at most 100 microns. In one of the embodiments of the films receive high strength as described above, in combination with a high linear density. In this application the linear density is expressed in units decitex. They represents the weight in grams of 10,000 meters of film. In one of the embodiments, the film in accordance with the present invention, has a denier of at least 3000 dtex, in particular at least 5000 dtex, more specifically, at least 10000 dtex, even more specifically at least 15,000 dtex, or even at least 20,000 decitex, combined with the strength of the, as indicated above, at least a 2.0 GPA, in particular at least a 2.5 GPA, more specifically, at least a 3.0 GPA, still more specifically at least a 3.5 GPA, and still more specifically at least 4.

The present invention will be explained using the following further Examples, without being limited to them, or with his help.

Example 1

Polyolefin powder with a bulk density 453 g/l condense on Isobaric press with double conveyor belt at different pressures. The density after compaction determined by cutting a sample of 0.5 m2of the sheet and weighing the sample. The results are presented in the following table:

Pressure (bar)Density (g/cm3)
300,90
400,92
500,94
600,95
700,95

The table shows that the increase in pressure leads to an increase in density. The higher the density of the compacted sheet gives the best source strength. Higher density is also the prerequisite for higher tensile strength, higher shear modulus and higher strain energy at break for the tape of the compacted sheet.

The table also shows that there can be obtained a very high pressure. It is noted that the pressure which can be obtained using izobaricheskogo press, limited to 40 bar mechanical structure of the press with a crawler belt. Also the width of the isochoric press limits pressure: the more you press, the lower maximum pressure. For this reason it is difficult and may be impossible to obtain density in the specified range using izobaricheskogo press.

1. A method of obtaining a film of ultra-high molecular weight polyolefin, which includes stages
- exposure to the original ultra-high molecular weight polyolefin with srednevekovoi molecular weight of at least 500000 g/mol in powdered form under seal using Isobaric press,
- impact on compacted polyolefin stage of rolling and at least one stage stretching under such conditions that at no point during the processing of the polymer its temperature is not increased to a value above its melting point.

2. The method according to claim 1, in which Isobaric press is a press with a continuous double conveyor belt.

3. The method according to claim 1 or 2, in which the polyolefin powder is exposed to the pre-heating stage before sealing.

4. The method according to claim 1 or 2, in which Isobaric press is supplied with a cushion pressing for the application of pressure to the polyolefin.

5. The method according to claim 1 or 2, wherein a material of the carrier is used to support a polyolefin powder under seal and all previous stages.

6. The method according to claim 1, in which Isobaric press is supplied with a gap, this gap has an input angle is less than 4.5°.

7. The method according to claim 1 or 2, in which Isobaric press provided with at least two zones of compaction, each pressing zone operates at a pressure higher than the previous nip.

8. The method according to claim 6, in which the first pressing zone operates at a pressure of at most 10 bar and at least one subsequent pressing zone operates at a pressure above 10 bar.

9. The method according to claim 1 or 2, in which the pressure under seal is at least 25 bar, in particular at least 30 bar, preferably at least 35 bar, more preferably at least 40 bar, most preferably at least 45 bar or at least 50 bar.

10. The method according to claim 1 or 2, in which stage stretching is carried out at such conditions that receive the General attitude of stretching, at least 30, particularly at least 50, preferably at least 80, more preferably, less than the least 100, most preferably at least 120, preferably at least 140, preferably at least 160.

11. The method according to claim 1 or 2, in which the source material is an ultra-high molecular weight polyethylene (UHMWPE) with srednevekovoi molecular weight of at least 500000 g/mol.

12. The method according to claim 1 or 2, in which stage of compaction is carried out at a temperature at least 1°C below the temperature of the natural polymer melt, in particular at least 3°C, preferably at least 5°C below.

13. The method according to claim 1 or 2, in which stage stretching is carried out at a temperature at least 1°C below the melting temperature of the polymer under the conditions, in particular at least 3°C, preferably at least 5°C below.

14. The method according to claim 1 or 2, in which the original polyolefin powder has a bulk density below 0.50 g/cm3in particular below 0.25 g/cm3preferably below 0.18 g/cm3, more preferably below 0,13 g/cm3.

15. The method according to claim 1 or 2, in which the temperature under seal support standing in the window of temperatures 2°C.



 

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FIELD: process engineering.

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23 cl, 7 dwg, 1 ex

FIELD: wood-working industry.

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19 cl, 2 dwg, 6 tbl, 2 ex

FIELD: chemistry.

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48 cl, 3 dwg, 3 tbl, 3 ex

FIELD: chemistry.

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22 cl, 3 tbl

FIELD: chemistry.

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41 cl, 3 tbl, 2 dwg, 2 ex

FIELD: chemistry.

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13 cl, 1 tbl, 13 ex

Aircraft window // 2475414

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9 cl, 6 tbl, 24 ex

FIELD: chemistry.

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EFFECT: films with said glass-transition temperature have high specific resistance.

10 cl, 2 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: copolymer of ethylene and a (C3-C18) α-olefin comonomer has density of 0.900-0.940 g/cm3, falling dart impact strength (F) satisfying the correlation with Vicat softening point as expressed by formulae (1) and (2), where V is Vicat softening point measured according to ASTM D 1525; and F is falling dart impact strength. The ethylene copolymer having improved impact properties is applicable to film, injection, compound, sheet, rotational, pipe or blow moulding.

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13 cl, 4 dwg, 3 tbl, 14 ex

FIELD: chemistry.

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14 cl, 3 dwg 4 tbl, 11 ex

Rotary pelletiser // 2487017

FIELD: process engineering.

SUBSTANCE: invention relates to machine building, particularly, to pelletisers to be used in chemical and pharmaceutical, electrochemical and other industries. Rotary pelletiser comprises rotor with female dies, aligned top and bottom male dies, and feeder. Said feeder has casing its inner space being formed by communicated chambers of turners. Said casing has a grove communicated with rotor female dies in rotation. Collector of excess material being pelletised is arranged at casing bottom. Said collector is communicated with turner chambers. Collector intake is composed of channel directed toward rotor rotation and communicated with aforesaid groove.

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Extrusion toolage // 2484966

FIELD: process engineering.

SUBSTANCE: invention relates to extruders of energy-bearing materials and may be used for making pyrotechnical cords from pre-compacted pellets. Proposed device comprises container with central guide channel and blind spline. Male die is arranged coaxially in said container. Reducing female die with through forming orifice adjoins the container end. Detachable ring is provided for geometrical closure of container with female die. Replaceable cardboard tube is fitted coaxially in container blind axial groove for gapless fitting of preformed pellet in press toolage axis.

EFFECT: higher quality of extruded articles and safety in extruding energy-bearing pyrotechnical materials.

1 dwg

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Pelletising press // 2481193

FIELD: process engineering.

SUBSTANCE: invention to material forming and may be used for making pellets from coal fines, peat grit, chips, etc. Proposed press comprises casing to house shaft with forming wheel mounted off-center. Said wheel is arranged between top and bottom flanges. Top flange has offloading opening and check opening arranged there above in bottom flange. Forming wheel is rigidly fitted on shaft, its axis being offset relative to casing axis. Said shaft is installed at plates with bearings, adjustment links and oval holes. Said plates are secured by means of studs and nuts at top and bottom flanges. Flanges are secured to casing. Plate teeth are regularly located on forming wheel outer side. Teeth side surfaces are inclined toward pellet exit through a definite angle to interact with plate teeth of second forming wheel. Second wheel is arranged in casing between top and bottom flanges with minimum clearance to run free therein. Second wheel teeth are regularly spaced on inner surface at the same spacing and with the same inclination at angle a to direction of rotation.

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6 cl, 6 dwg

FIELD: machine building.

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EFFECT: higher reliability of the device.

17 cl, 4 dwg

FIELD: process engineering.

SUBSTANCE: invention relates to fuel agglomeration machines and production of moulded solid fuel to be used in utilities and power engineering. Proposed device comprises housing with screw, solid fuel feed trough, and female die with moulding holes and ducts. Device housing accommodates conditioning system while screw is furnished with processing blades and heating elements arranged inside screw hollow tube and connected to external power source by means of terminals.

EFFECT: higher quality of fuel pellets.

3 cl, 2 dwg

FIELD: agriculture.

SUBSTANCE: invention relates to agricultural machinery industry and can be used for granulation and briquetting the forage. Press for shredded forage comprises two gear wheels with radial holes in the cavities and flanges on the sides of the gear wheels with a height equal to half the height of the tooth. The gear wheels are arranged horizontally. In the area of feeding the material the receiving chamber is located, formed by a base, rear and two side walls. The base is adjacent to the surface generators of the lower flanges. The upper bound of the base is in the same horizontal plane as the upper surfaces of the lower flanges. The rear wall is mounted so that the angle between it and the base from the side of the receiving chamber is blunt and does not exceed 135°. The lower part of the rear wall is tangent to the outer diameters of both pressing gears. The side walls of the pressing chamber converge at the point of contact of the pitch circles of pressing gears and are adjacent to the surface generators of the upper flanges on sectors with central angles of 90°. The lower end faces of the side walls of the pressing chamber are in the same horizontal plane as the lower surfaces of the upper flanges.

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2 cl, 5 dwg

FIELD: process engineering.

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EFFECT: simplified assembly/disassembly, decreased weight, higher reliability.

5 cl, 4 dwg

Press-granulator // 2464171

FIELD: process engineering.

SUBSTANCE: invention relates to machine building, particularly, to pelletisers to be used in chemical, construction, agricultural industries, etc. Proposed device comprises case, perforated cylindrical female die and two forming rollers, at least one pellet cutting mechanism that allows adjusting clearance between female die and knife, cutting mechanism with knife arranged pelletising chamber engaged with said adjusting mechanism and provided with stop gear. Device drive accommodates pellet cutting knife fitted on bar secured on shaft mounted on case. Shaft second end is located inside said case and engaged with clearance adjusting mechanism made up of reduction gear fitted on shaft second end and engaged with clearance adjustment handle arranged on case side and provided with knife position indicator.

EFFECT: simplified design, higher efficiency and quality.

3 cl, 2 dwg

FIELD: process engineering.

SUBSTANCE: invention relates to crushing lignocellulose materials to fibers for production of structural, insulating and reinforcing materials and fillers. Lignocellulose materials with wet surface and mixed with fiber modifiers are subjected to controlled pressure of roller-dish grinder rolls of plane-matrix pelleting press. Note here that fiber modifiers penetrate deeply into said material to react therewith inside fibrous material pores stimulated by high moisture content. Minced and refined material is then extruded through holes drilled in plate dish matrix.

EFFECT: possibility to vary fiber thickness and length, intensified inner void volume compaction, hygroscopic property and adhesion.

12 cl, 2 dwg, 6 ex

FIELD: process engineering.

SUBSTANCE: invention relates to light material, particularly to films with textile properties. It if made from thermoplastic polymer. It is processed to form linear areas A interconnected by linear crosspieces B. Note here that every area A and crosspiece B are oriented. Note here that prevailing direction of orientation in areas A forms angle v relative to direction wherein A extend. Note also that crosspieces B comprises multiple straight grooves of finer material or slits making angle u larger than v relative to direction in which A pass. Proposed method comprises passage of oriented film through two engage rifled rolls for cold stretching of the film in direction at the angle relative to prevailing initial orientation. Note also that, at least, one of said rifled rolls has sharp-edge flanges to separate areas A from crosspieces B and to stretch the material for making crosspieces B. at the same time material stretching to form areas A is smaller or is not made at all. Preferably, one of said rifled rolls has ledges with wavy surface.

EFFECT: film with textile properties.

18 dwg, 3 ex

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