Biodegradable films based on copolymers of 3 - polyhydroxybutyrate/3 - polyhydroxyalkanoate

 

(57) Abstract:

The invention relates to a film comprising a biodegradable copolymer, where the copolymer includes at least two statistically recurring Monomeric level, where the first link has the formula

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and the second link has the formula

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and at least 50% of the units have the formula of the first link. The invention relates also to devouring the product, including the top floor, permeable to fluids, biodegradative the bottom floor, impervious to liquids, comprising the above film, and an absorbent Central layer located between the upper and lower surfaces. 2 s and 5 C.p. f-crystals.

The invention relates to biodegradiruemym the copolymers; films, including copolymers; and absorbing the products of a single use, such as diapers, sanitary napkins and panties for patients suffering from incontinence, including such films.

A large variety of shock-absorbing products, designed to be effective for absorption of body fluids such as blood, urine, menstrual flow and the like, is well known. Products disposable ispolzuya, absorbing the Central part and the material is impermeable to liquids, for the bottom cover. Still such absorbing structure is made, for example, using the top cover of woven, non-woven or porous film-forming polyethylene or polypropylene materials. The materials for the lower coverage typically includes a flexible plastic coating. The materials absorbing the Central part typically include fibers of wood pulp or fibers of wood pulp in combination with absorbent gelling materials. One aspect of such absorbing products until recently was their one-time use. Although such products are based include material that was considered ultimately will degrade and although the products of this type make a small contribution to the total solid waste produced by consumers each year, however, there is a need for the development of such products one-time use of materials that are compostable.

Conventional absorbent disposable item already largely is compostable. Conventional disposable diaper use, Napravnik. In the composting process pollutant absorbing products disposable tear and mixed with organic waste, essentially, to composting. After composting, the particles that have not undergone composting, weed out. Thus, even today absorbent products can be successfully processed at composting plants.

However, there is a need to reduce the number decompostion materials in absorbent articles and disposable items. There is a specific need to replace the plastic bottom coatings in absorbing products films of compostable material impervious to liquids, because the bottom floor is usually one of the most decompostion components of conventional absorbent articles and disposable items.

In addition, being compostable, film applied as a bottom coating for absorbing products must meet many other characteristics. For example, the resin must be thermoplastic, so that they can be applied to conventional methods of processing film. These methods include irrigation plank the x structures. Other methods include extrusion coating of one material on another, or on both sides of composted substrate, such as another film, non-woven fiber or paper fiber.

Other properties are essential in the operations of transformation of the product where the use of film for the manufacture of absorbent products. Properties such as ultimate tensile strength, modulus of tensile elasticity, tear resistance and temperature of thermal softening, determine largely how well the film will be used in processing lines.

In addition to the above properties, it is necessary to consider the properties required of the end user of the absorbing product. Film properties such as impact strength, puncture resistance and blagopoluchnye are important because they affect the duration of operation of the absorbing product and capacity in the process of wearing.

Once rid of the absorbing product and it is included in the composting process, other properties become important. Regardless of whether crushed or not the incoming waste, it is important that the film or large fragments of the film podvergalsa speaking, film or large fragments of the film can be eliminated from the stream of compost and can never become part of the final compost.

Previously we studied the Biodegradability and physical properties of various polyhydroxyalkanoates. Polyhydroxyalkanoate are polyether compounds produced by various microorganisms, such as bacteria and algae. Although polyhydroxyalkanoate was of General interest because of their biodegradable nature, their actual use as plastic materials have been difficult because of their thermal instability. For example, poly-3-hydroxybutyrate (RNV) is a natural product energy storage of bacteria and algae, and is present in the form of discrete granules within the cytoplasm. However, in contrast to other biologically derived polymers, such as proteins and polysaccharides, RNW is a thermoplastic polymer having a high degree of crystallinity and unambiguous melting point of approximately 180oC. unfortunately, RNW becomes unstable and will destroy at elevated temperatures near its melting point. Due to this thermal ately studied other polyhydroxyalkanoate, such as poly(3-hydroxybutyrate-co-3 - hydroxyvalerate) (PHVB), hoping to find polyhydroxyalkanoate with sufficient thermal stability and other useful chemical and physical properties to use for practical purposes. Unfortunately, polyhydroxyalkanoate, such as RNB and PHVB, it is difficult to be processed into films suitable for use as the lower cover. As discussed previously, thermal instability RNW did such processing is virtually impossible. In addition, the slow crystallization rate and characteristics of fluidity RNV and PHVB made difficult processing of the film. Examples of homopolymer RNV and copolymers PHVB describe in U.S. patent 4393167, Holmes et.al., published July 12, 1983, and in U.S. patent 4880592, published 14 November 1989. Copolymers PHVB are commercially available from Imperial Chemical Industries under the trade name BIOPOL. Copolymers PHVB currently produce content valerate in area from about 5 to about 24 mole %. The increase in the content valerate reduces the melting temperature, crystallinity and rigidity of the polymer. Technology overview BIOPOL present in Bisness 2000+(Winter, 1990).

Due to the slow rate of crystallization of the film, made the long period of time. The casting of the film, where the film immediately cooled on a cooling roll after it leaves the extrusion head, the melt PHVB often sticks to the rolls, slowing the speed with which it can be processed film, or even preventing the process of winding the film. In the films, obtained by blowing, residual stickiness PHVB causes the tubular film to stick together, after it cooled down and squeeze for winding.

U.S. patent 4880592, Martini et.al., published on November 14, 1989, discloses values achieved PHVB the monolayer films for applications as the bottom cover of the diaper by sextravaganza PHVB between two layers of polymer, such as polyolefin, stretching and orientation of the multilayer film, and then the striping away of polyolefin layers, after PHVB time was provided for crystallization. The remaining film PHVB then laminate or a water-soluble film or water-insoluble films, such as polyvinylidenechloride or other polyolefins. Unfortunately, such strong and bulky measures of processing are necessary when you try to avoid the inherent difficulties associated with the processing of PHVB in the film.

On the basis of when the, diaper) with increased Biodegradability. To meet this need there is a prior need to biodegradation copolymer, which was able to be easily processed into a film for use in such sanitary disposables.

The purpose of the present invention consists in obtaining a film comprising a biodegradable polyhydroxyalkanoate.

One of the purposes of the present invention to provide a sanitary disposable products use, including film containing a biodegradable RNA.

The present invention relates to a film containing a biodegradable copolymer, where the copolymer includes at least two statistically recurring Monomeric link (RRMU), where the first RRMU has the structure

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and the second RRMU has the structure

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where at least 50% RRMU have a structure of the first RRMU.

The present invention further relates to devouring the product, including permeable to liquid top coating that is impermeable to liquids lower floor, including the above-mentioned film, and absorbing the Central part located between radioroom copolymer, which is capable of easily processed into film. Further, the present invention meets the need in the absorbing products single use with high Biodegradability.

The term "ASTM" as it is used here, refers to the American society for testing and materials.

The term "comprising" as used here denotes that can be added to other stages and other ingredients that do not affect the final result. The term includes "consisting of" and "consisting essentially of".

The term "alkyl", as used here, denotes a saturated carbon chain, which may be unbranched or branched; and substituted (mono - or poly-) or unsubstituted.

The term "alkenyl" as it is used here, refers to carbon-containing chain which may be monounsaturated (i.e., one double bond in the chain), or polyunsaturated (i.e., two or more double bonds in the chain); an unbranched or branched; and substituted (mono - or poly-) or unsubstituted.

The term "RNA" as used here, denotes polyhydroxyalkanoate according to the present invention.

The term "RV" as he ides, denotes the copolymer poly(3-hydroxybutyrate-co-3-hydroxyvalerate).

The term "biodegradable" as used here, refers to the ability of the compounds to degradation to CO2and water, or biomass by microorganisms and/or natural environmental factors.

The term "compostable" as it is used here, refers to material that meets the following three requirements: 1) the material is able to be processed in the composting device for solid waste; 2) if the material processed in this way, the material will be the ultimate material in the final compost; 3) if the compost applied to the soil, the material will be fully destructivity in the soil.

For example, there is no need polymeric film material present in the waste to be recycled in the composting device until the final composting. Some composting device is subjected to the solid waste stream of air classification to further processing in order to separate paper and other materials. The polymeric film will most likely be separated from the solid waste stream when such air examining the dummy material according to the above definition, because he is "able" to be processed in the composting device.

The requirement that the material was the final in the final compost, usually means that it undergoes a transition in the form degradiruem in the composting device. Usually the solid waste stream will be subjected to disintegration in the early phases of the composting process. In the polymer film will be rather in pieces than as a whole diaper. In the final phase of the composting process, the final compost will be subject to a stage disqualification. Typically, the polymer pieces will not pass through a sieve, if they keep the size that they had immediately after the grinding stage. Compostable materials of the present invention will lose their integrity sufficiently in the composting process, allowing partially destroyed pieces to pass through the sieve. However, assume that the composting device may expose the solid waste stream is very intense grinding and more coarse filtration, in which case degradiruete polymers like polyethylene will meet the requirement (2). Therefore, to meet the requirement (2) is not sufficient for the material, material, as defined here, from material such as polyethylene, is the requirement (3) when the material is completely biodegraders in the soil. This requirement of Biodegradability is not sufficient for the process of composting or used for composting in the soil. Solid waste and compost derived from them, can contain all kinds of non-biodegradable materials, such as sand. However, in order to avoid accumulation of the products of human activity in the soil, in the present invention requires that such materials are fully biodegradable. In other words, it is not necessary that this process of biodegradation was rapid. Because the material itself and the intermediate decomposition products are not toxic or otherwise polluting the soil or the crop, it is quite acceptable to their biodegradation proceeded for several months or even years, as you only want to avoid the accumulation of products of human activity in the soil.

All relationships copolymer compositions described here, refer to molar relationship, unless otherwise stated.

Film.

The present invention relates to biodegradiruemym lipopolymer PHBV. Before the advent of the present application, polyhydroxyalkanoate studied for use in industrial plastics. As discussed above, polyhydroxyalkanoate, such as RNB and PHBV copolymers are difficult to process because of their thermal instability. In addition, such polyhydroxyalkanoate especially difficult was processed into films due to their slow rate of crystallization. The authors of this application have found that RNA copolymers in accordance with the present invention, which include the second RRMU of comonomer, as defined above, containing alkyl substituent of at least three carbons, are suddenly easily processed into films, especially compared to RNV or PHBV. Applicants unexpectedly discovered that such a linear, random copolymers with a limited number of secondary branched chain (for example, C3-C19) provide in addition to Biodegradability the following properties, especially compared to RNV or PHBV: a) a lower melting temperature, b) a lower degree of crystallinity and improved rheology of the melt.

Regardless of theory, the applicants believe that the characteristics of a) and b) are achieved by eliminating Vtorov and improved stiffness and elongation characteristics. In addition, regardless of theory, the applicants believe that the characteristic (C) is achieved by the increased entanglement between chains of the copolymer due to the side chains of the second RRMU. This heightened weave may be due to the increased hydrodynamic volume of the copolymer (for example, the second Monomeric link creates a loop in the spiral structure), "hooks" or "traps" of the side chains on the main chain of the various copolymers during melting or low open circuit due to lower TPL(i.e., increased window thermal process).

Biodegradable RNA, useful for processing into films according to the present invention includes two statistically recurring Monomeric link (RRMU), where the first RRMU has the structure

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and the second RRMU has the structure

< / BR>
where at least 50% RRMU have a structure of the first RRMU.

In a preferred embodiment, RNA includes one or more additional links RRMU having the structure

< / BR>
where R1is H, or C2or C4WITH5WITH6C7C8C9C10WITH11WITH12WITH13WITH14WITH15C16C17C18or19-alcance, a continuous piece of matter, characterized by the ratio of the length to the thickness and the ratio of width to thickness. Although not shown the exact requirements to the upper limit of thickness, preferably the upper limit will be about 0,254 mm, more preferably 0.01 mm, and even more preferably of 0.005 mm Protective value of any film depends on how it is homogeneous, i.e., without holes or cracks, as it must be an effective barrier to molecules such as atmospheric water vapor and oxygen. In a preferred embodiment of the present invention, the film is impermeable to liquids and is suitable for use in absorbent sanitary products, disposable use, such as disposable diaper, feminine hygiene products and the like. More preferably, the film obtained in accordance with the present invention, in addition to increased Biodegradability and/or computermemory have the following properties:

(a) the modulus of tensile elasticity in the machine direction (BD) from about 6,895 108Dyne/cm2to about 6,895 109Dyne/cm2,

b) tear resistance MD at least 70 g 25.4 microns of thickness,

C) Copr,

d) impact strength of at least 12 cm, as measured by the falling ball

(e) the rate of moisture transport is lower than about 0,0012 g cm2for 6 hours,

f) a module at 60oC at least 5,52 107Dyne/cm2and

W / thickness of from about 12 microns to about 75 microns.

Test methods for these operational characteristics are discussed in more detail below.

Operational characteristics and test methods of films.

Film with satisfactory characteristics, such as computermemory the bottom of the disposable diaper use should be made of resins or materials that are biodegradable and must demonstrate a high strength, to meet the requirement of a liquid barrier having a high melting point.

The lower part of disposable nappies should possess sufficient strength in terms of processing high-speed processing machine for disposable diaper use, and ensure the "moisture-proof" barrier when used for a child. It must be enough moisture so that the clothes or bed (diaper) of the child or caregiver is not specialis what Yalom, pleasant in order to be used as the outer cover of the diaper for a child, but still high enough to be easily processed on high-speed machines for the manufacture of disposable nappies without wrinkles, creases or folds. It must have sufficient heat resistance so as not to be deformed, does not melt or permanently lose strength under normal conditions of hot storage or lose uniformity in a high-speed converters disposable nappies, which usually use the hot melt adhesives to bind together the components of the disposable diaper use.

Films that are strong enough and suitable as biodegradable and/or compostable bottom coatings for disposable nappies, preferably exhibit two properties: (a) tear resistance drop weight and b) tear resistance in the machine direction for the manufacture of the film and in the direction perpendicular to the machine for the manufacture of the film. Preferred lower the coatings obtained in accordance with the present invention, withstand the fall of the spheres is re 50% of the trials do not lead to any gaps (deformation is acceptable). The preferred materials are those materials that show a 50% or less damage when you drop a ball from a height of more than 20 see Similarly acceptable lower cover shows the average tear resistance 70 g material thickness of 25.4 μm in both directions of the machine in longitudinal and perpendicular when using a standard testing device - the pendulum of Elmendorf, such as Elmendorf Model No. 60-100 compared to 16 folds of material, which was prepared without incision or incision according to TAPPI Method T 414om-88. More preferred are lower cover, which show the tear resistance of 200 or more grams on the thickness of 25.4 μm perpendicular to the machine direction, because these coatings are especially good in the sense that they have avoided destruction during use due to the incision.

It was also found that the films possess a sufficient barrier for moisture transport and allowing less than 0,0012 g of synthetic urine to pass on absorbing paper towel on cm2area when the film thickness of 25.4 microns for every 16 hours, when the test film was placed between absorbent paper and normal will the t child. Specific test conditions was that the area of the Central part was found to be greater than the area of the test material, the Central part load synthetic urine to its theoretical capacity and it is under pressure weight of about 35 g/cm2(0,5 psi.).

It was also found that the materials of sufficient heat resistance demonstrate the heat Vika at least 45oC. the Heat Vika experience using Heat Distortion Apparatus Model No.Cs-107 or equivalent and modification of ASTM D-1525. The modification consists in the preparation of the sample. Prepare film size 19 mm2the thickness of 4,5-6,5 mm for testing according to Vic on the penetration of the needle due to the melting of the material to be tested, in the form, using a temperature of 120oC and pressure 7,031 105g/cm2(10000 psi) (using Caver or similar press) within two minutes after a period of heating at least for 2 minutes. The heat Vika is the temperature at which the needle with the flat end of the 1 mm2rounded profile will penetrate into the sample to a depth of 0.1 cm at a load of 1000 g with uniform speed of temperature rise 50oC per hour.

The former type above at least 6,895 108Dyne/cm2and below at least 6,895 109Dyne/cm2. Testing is carried out on an electronic machine for testing the strength properties, such as an Instron Model 4201. A strip of material of a width of 2.54 cm, preferably 0,00254 cm thick, cut into a length of about 30 cm, with the long part of the material parallel to the direction of the machine. The test strip is fixed in the clamps of the tester for testing the strength so that the scale or the actual length of the test material was 25.4 see Clips bred with slow speed component of 2.54 cm per minute to 25.4 cm per minute, and record the curve of stress - strain chart within an attached recording device. 1% secant modulus determined by reading the voltage or the limit tensile stress from the diagram in point 1% relative elongation. For example, point 1% strain is reached, when the distance between the clamps is increased by 0,254 see When the clamps are bred with a speed of 2.54 cm per minute and the recording device operates at a speed of 25.4 cm per minute, point 1% deformation will be located at a distance of 2.54 cm from the starting point. Characterization of the limit of the tensile strength of the DMA preferred materials show a 1% secant modulus in the field 6,895 108to 2,068 109Dyne/cm2.

As absorbing products can experience such a high temperature as 140oF (60oC) during storage on commodity warehouses or when transported in trucks or freight cars, it is important that the film of the lower cover and other components retained integrity at these temperatures. Although expect the modules films will to some extent be reduced at temperatures between 20oC and 60oC, the modules should not decrease so much and allow the film to be deformed in the package before it will not be the end consumer.

For example, a plastic bottom cover module about 4 to 109Dyne/cm2at room temperature may have a module 1,2 109Dyne/cm2at 60oC, which is acceptable. Softer plastic bottom cover module at room temperature, equal to 8.0 108Dyne/cm2may have a module about 3.5 108Dyne/cm2at 60oC, which is still acceptable. Usually acceptable film of the lower cover of the present invention will have a module at 60oC at least 5,52 107Dyne/cm2.

The dependence of the module t is logical analyzer (DMA), such as Perkin Elmer 7 Series/ Unix TMA 7 Thermomechanical analyzer equipped with the 7 Series/ Unix DMA 7 Temperature/Time sofware package, which is hereinafter referred to as DMA 7 available from Perkin-Elmer Company of Norwalk, Connecticut. There are many other types of DMA devices and the use of dynamic mechanical analysis to study the spectrum of the polymer module/temperature is well known to specialists in this field of research of polymers (copolymers). This information is well summarized in two books, the first Dynamic Mechanical Analysis of Polymeric Materials Science Monographs Volume I, Murayama (Elsevier Publishing Co., 1978) and the second Mechanical Properties of Polymers and Composites, Volume I, L. E. Nielsen (Macel Dekker, 1974).

Mechanical operations and procedures for use DMA 7 described in the Perkin-Elmer User's Manuals 0993-8677 and 0993-8679, both dated may 1991, For experts in the use of DMA 7, the following conditions of the experiments should be sufficient to obtain data modules at 60oC, below.

For measuring range module/temperature of the sample film DMA 7 is set in the mode under consideration of temperature and equip the tension measurement system (EMS). A sample film having a width of approximately 3 mm and a thickness of 0,0254 mm and of sufficient length to cover 6-8 mm distance between the clamps placed in tension to the film in the direction of the length to achieve the strain or tension of 0.1% of its original length. Applied to the sample dynamic sinusoidal voltage at a frequency of 5 cycles per second. In this mode, the temperature of the temperature increase with speed 3.0oC/minute from 25oC to the point where the sample is melted or destroyed, while the frequency and voltage withstand constant. The behavior of the temperature dependence is characterized by controlled variation of the voltage and the phase difference in time between stress and strain. The magnitude of the dynamic modulus of elasticity in shear Pascals estimated using a computer together with other data and recorded as a function of temperature on the video display. Typically, the data stored on computer disk or on the hard disk and range of module/temperature print out for further review. Module at 60oC determined directly from the spectrum.

Method of production of the film.

The film of the present invention, used as the bottom coating with enhanced Biodegradability, and/or computerweekly, can be obtained using conventional procedures to obtain single and multilayer films on conventional equipment for the manufacture of the film. The RNA pellets m is a hundred insufficient mixing in plastic film extruder, granules can be first subjected to mixing in dry form and then mixing in the melt in the extruder with the preliminary canadianowned then granulating before extrusion of the film.

RNA of the present invention can be processed from the melt into a film, using either method of irrigation, or extrusion film blowing machinery, both methods are described in Plastics Extrusion Technology, 2nd Ed., Allan A. Griff (Van Nostrand Reinhold-1976). Watered film ekstragiruyut through a linear slit die plate. Usually flat sheet is cooled on a large moving the polished metal roll. The film is rapidly cooled and peeled from the first roll, passes over one or more auxiliary cooling rolls, then through a set of traction devices or snatch devices", rubber-covered, and, finally, to the winding machine. A method of manufacturing the film for the lower coverage irrigation for absorbent products are described in the examples below.

During extrusion film blowing machinery melt ekstragiruyut up through a thin annular hole Spinneret. This method also applies to the extrusion of a tubular film. The air injected through the Central part of the nozzle for filling the sleeves of the film and thereby operate OSU control of external air pressure. Sleeve film is cooled by air, blowing through one or more cooling ring surrounding the sleeve. Then the sleeve tapers by pulling it through a flat frame through a pair of pull rolls and the winding machine. For use as a bottom coating of flat tubular film sequentially cut, unfold and then cut into a width that corresponds to the dimensions of the product.

Both film production irrigation and blowing can be used to produce either single-layer or multilayer film structures. For the manufacture of single-layer films from a single thermoplastic material or a mixture of thermoplastic components requires only a single extruder and a single distribution filer.

For the production of multilayer films is the preferred method of coextrusion. Such methods require more than one extruder or coextruded block supply or distribution system of several nozzles or a combination of both to achieve a multilayer film structure.

U.S. patents 4152387 and 4197069 disclose the principles of the feed block coextrusion. Many extruders attached to the feed block, which is the material flow in direct relation to the volume of polymer, passing through these flow channels. The flow channels designed so that at their point of confluence of the materials came from the same flow rate and pressure, eliminating interfacial tension and instability of the flow. Once the materials were combined in the feed block, they come in a single distribution head as a composite structure. For such processes it is important that the viscosity of the melt and the melt temperature of the materials was not significantly different from each other; in other words, the instability of flow may lead to poor control of the thickness distribution of a layer in a multilayer film.

As another option coextruded block feed is monographella comb or head Apastovo type that is disclosed in the aforementioned U.S. patents 4152387 and 4197069 and U.S. patent 4533308. While the block feeder streams of the melt unite together outside before entering the body of the head, in mnogozastrelenny the comb or head Apastovo type each melt flow has its own distribution comb in the head, where the polymers are independently distributed in their respective dies. The flow of the melt near his summe connect the e slit channel of each stream is directly proportional to the volume of material running through it, allowing the melt to connect with one and the same linear flow velocity, pressure and the desired width.

Since the flow properties of the melt and the melt temperature of the processed materials can vary within a wide range, using head Apastovo type has several advantages. The head is suitable for specific thermal characteristics, where materials with very different temperatures of the melt, for example up to 175oF (80oC), can be processed together.

Each comb in the head Apastovo type can be designed and manufactured according to specific polymer (or copolymer). Thus, the flow of each polymer is determined only by the design of the dies, and not the forces imposed by other polymers. This allows materials with very different viscosities of the melt to be coextrudable in multilayer films. In addition, Lapteva head also provides the opportunity to have the desired width of the individual dies in such a way that the inner layer, for example, water-soluble biodegradable polymer, such Vinex 2034, can be completely manatee patents also disclose sharing systems of power supply and laptevykh heads to achieve more complex multilayer structures.

Multilayer film according to the present invention may include two or more layers. In General, balanced or symmetrical three-layer or five-layer film are preferred. Balanced multi-layer three - layer film include the Central inner layer and two identical outer layer, where the specified Central inner layer is located between these two outer layers. Balanced multi - layer, five-layer film include the Central inner layer, two identical binding layer and two identical outer layer, where the specified internal Central layer is located between two specified binding layer and connecting layer is located between the said Central inner layer and each outer layer. Balanced films are less prone to twisting or distortion than unbalanced multilayer films.

In the three-layered films of the Central inner layer may be from 30 to 80 percent of the total film thickness and each outer layer may be from 10 to 35 percent of the total film thickness. Layers, if used, each is from about 5 to about 10 percent of the total film thickness.

X-ray analysis is most appropriate when little is known about thermal properties of the material and the change of crystal structure, which may take place. The basic principle of the analysis is that the amorphous part of the material pass x-rays in the field of diffuse or wide angles, while the crystals are subjected to the diffraction of x-rays in the form of sharp, well-defined corners. Full missed the intensity, however, is constant. This allows you to calculate the amount of crystalline material in the sample, the EU is izraboten Ruland, which could detect the difference in the percentage of crystallinity is low as 2% (see, Vonk,C., F. J. Balta-Capelleje, X-Ray Scattering fom Synthetic Polymers, Elesevier: Amsterdam, (1989); and Alexsander,L., X-Ray Diffraction Method in Polymer Science, Robert Kreiger Pub. Co., New York, (1979)).

During melting the crystals require a fixed amount of heat at the melting point of passing from the crystalline to the molten substance. This heat of fusion can be measured using several thermal methods, the most popular of which is DSK. If you know the temperature of melting of 100% crystalline material and no significant annealing, or the phenomena of melting/crystallization when heated to melting point, then using the DSK can quite accurately determine the weight fraction crystallinity (see Thermal Characterization of Polymer Materials, E. Turi. , Ed., Academic Press, New York, (1980); and Wunderlichh,B., Macromolecular Physics, Academic Press, New York, (1980)).

If you know the density of pure crystalline and pure amorphous materials, then measuring the density of the material can give the degree of crystallinity. This implies additivity of specific volumes, but this requirement is fully observed for polymers (or copolymers) homogeneous structure. This method depends on the SS="ptx2">

If you can be identified purely crystalline and amorphous absorption band, then the spectrum of infrared absorption is a powerful method for determining the crystallinity (see, Todokoro.H. Structure of Crystalline Polymers, John Wiley and Sons, New York, (1979)).

It should be noted that different methods will often give quite different values of fcbecause they are based on different physical principles. For example, density measurements often give higher values than the data of x-ray analysis. This is due to the continuous variation of density at the interface between crystalline and amorphous polymer (or copolymer) material. While x-ray analysis does not register such thing as crystallinity, density measurement will largely depend on this region on the phase boundary.

Order processing in film PHAs corresponding to the present invention, preferably have a crystallinity from about 2% to about 65%, as measured by x-ray crystallography, more preferably from about 5% to about 50% and even more preferably from about 20% to about 40%.

The temperature is about 30oC to about 160oC, more preferably from about 60oC to about 140oC and even more preferably from about 90oC to about 120oC.

Absorbing product.

Further, the present invention relates to absorbent articles comprising RNA. Such absorbent articles include, but are not limited to, diapers, briefs and pads for adults suffering from incontinence and feminine hygiene soft lining and backing. Film used as the lower cover in the absorbing products, impervious to liquids, such as disposable diaper, typically have a thickness from about 0.01 mm to about 0.2 mm, preferably from about 0.012 mm to about 0,051 mm

Generally the lower floor, impervious to liquid, together with a top coating that is permeable to liquid, and absorbing a Central part located between the upper floor and lower floor. May not necessarily be included elastic membrane and sewn belt buckle. While the upper floor, lower floor, absorbing the Central part and the elastic membrane can be combined in a variety of well known configurations, predpochtitel is isawanya".

Top coating is preferably soft and not irritating the skin of the user. In addition, the top coating is permeable to fluid, allowing the fluid to easily pass through. Suitable top coating can be made from a wide variety of materials, such as porous foam material, reticulated foam materials, mesh plastic films, natural fibers (for example, wood fibers or cotton), synthetic fibers (e.g. polyester or polypropylene fibers) or from a combination of natural and synthetic fibers. Preferably, the top coating is made from a hydrophobic material to isolate the skin of the user from absorbing liquids in the Central part.

Especially preferred upper floor includes staple fibers having a number of about 1.5.

There are a number of techniques that can be used to make the upper cover. For example, a top coat may be spinning, napadenim, molded, Cardo and the like. The preferred top floor is the Cardo and thermally connected with well-known specialists of techniques is>minimum ultimate tensile strength in the dry state at least about 400 g/cm in the machine direction and ultimate tensile strength in the wet state of at least about 55 g/cm in the direction perpendicular to the machine direction.

The upper floor and lower floor connected together in any suitable manner. The term "connected" as used here, includes the configuration where the upper floor directly attach to the lower floor through gluing the top cover directly to the lower floor, and a configuration where the upper floor is not directly attached to the lower floor, and by bonding the upper surface of the intermediate membrane, which in turn is glued to the lower floor. In a preferred embodiment, the upper floor and the lower floor is glued directly with each other on the periphery of the diaper using substances, such as glue, or other substances known in this area. For example, a uniform continuous layer of adhesive, a structural adhesive layer or an adhesive in the form of a number of separate lines or spots may be used for bonding the upper surface to the lower floor.

Predictabilty to maintain the diaper on the user. Sewn belt fasteners can be of any type well known in this area, such as types of fasteners disclosed in U.S. patent 3848594. These sewn belt buckle or other type of fasteners for diaper usually placed near the edges of the diaper.

Preferred diapers contain elastic membrane located near the periphery of the diaper, preferably along each longitudinal edge, so that the elastic membrane tend to stretch and hold the diaper about the user's legs. Elastic membranes provide the diaper in unstretched condition that the normal unstretched configuration elastic membrane effectively reduce or compress the diaper. The elastic membrane can ensure reduction in at least two ways. For example, the elastic membrane can be stretched and at the same time to provide the diaper with the opportunity to be in the unstretched condition. Or the diaper may be compressed, for example, by folding the elastic membrane, which is equipped with a diaper and with which it is associated, while the elastic membrane is in its relaksirano or unstretched condition.

The elastic membrane can PR is up to about 25 mm or more; the elastic membrane may include a single strand of elastic material or elastic membrane may be rectangular or curved. Further, the elastic membrane can be glued to the diaper by any of several known in this field techniques. For example, the elastic membrane can be attached ultrasono by thermal sealing or sealing by pressure on the diaper, using a variety of anchoring samples, or elastic membrane can be simply glued to the diaper.

Absorbing the Central part of the diaper have between the top floor and bottom floor. Absorbing the Central part can be produced with a large variety of sizes and shapes (e.g. rectangular, in the form of an hour glass, asymmetric, and so on) and from a wide variety of materials. The total absorption capacity of the absorbing Central part must, however, be compatible with the design of liquid-propellant load for the intended use of the absorbent article or diaper. Further, the size and absorbent capacity of the absorbent Central part can vary depending on adapting to the user from a child to an adult.

the General Central part is preferably the element, including non-woven fabric or felt air fill, the fibers of the paper pulp and/or specific absorptive polymer composition located in them.

Other examples of absorbent articles in accordance with the present invention are sanitary napkins, designed for the reception and retention of vaginal discharge, such as menstrual. Sanitary napkins disposable design in such a way as to keep them near the user's body by means of clothes, such as underwear or panties, or through specially designed fasteners. Examples of the types of sanitary napkins, which applies the present invention, shown in the U.S. patents 4687478 and 4589876. Obviously, the film of the present invention described herein may be used as the bottom cover, impervious to liquids, such as sanitary napkins. On the other hand, it will be clear that the present invention is not limited any particular configuration or structure of the sanitary napkin.

In General, sanitary napkins include a bottom cover that is impermeable to liquid, the top covering is permeable to liquid, and Piglet RNA in accordance with the present invention. The upper floor may be composed of any materials of the upper surface, as discussed in relation to the cradle.

It is important that the absorbent articles according to the present invention are biodegradable and/or compostable in a greater degree than conventional absorbent products that use materials such as polyolefins (e.g. polyethylene bottom floor).

Synthesis of biodegradable PHAs.

Biodegradable PHAs in accordance with the present invention are obtained by synthetic chemistry or using biological methods. Chemical approach involves the polymerization is Viktorovich monomers with opening cycle, as described below. The catalysts or initiators may be different, such as alumoxane, distannoxane or alkoxy-zinc and aluminum compounds (see, Agostini. D. E. , J. B. Lando and J. R. Shelton, Polym.Sci.,Part A-1, Vol.9, pp. 2775-2787 (1971); Gross.R.A., Y. Zhang, G. Konrad and R. W. Lenz, Macromolecules, Vol.21, pp. 2657-1668 (1988); and Dubois.P., I. Barakat, R. Jerome, and P. Teyssie, Macromolecules, Vol., 26, pp. 4407-4412 (1993); Le Borgne.A., and N. Spassky, Polymer, Vol., 30, pp. 2312-2319 (1989); Tanahashi.N., and Y. Doi, Macromolecules, Vol. , 24, pp. 5732-5733 (1991); Hori.Y., M Suzuki, Y. Takahashi, Y. Ymaguchi and T. Nashishita, Macromolecules, Vol., 26, pp.4388-4390 (1993); and Kemnitzer.J.E., S. P. McCarty and R. A. Gross, Macromolecules, Vol., 26, pp. 1221-1229 (1993). Getting isotactic polymers can RBSU is, is because with inversion of the configuration of the stereocenter, or by polymerization of racemic monomer with an initiator, which will mainly polimerizuet one enantiomer. For example:

< / BR>
Statistical copolymer RNW/NSS

R=CH2(CH2)yCH3, y1

Naturally derived PHAs are isotactic and have the R absolute configuration at stereocenter in the main polymer chain. On the contrary, can be obtained isotactic polymers, where the configuration stereocontrol may be predominantly S configuration. Both isotactic material will have the same physical properties and basically the same reactivity, except when include stereospecific agent, such as an enzyme. Atactic polymers, polymers with the statistical occurrence of stereocontrol R and S, can be obtained from racemic monomers and initiators or polymerization catalysts, which do not have a preference to any enantiomer, while such initiators or catalysts often polymerized monomers of high optical purity to isotactic polymers (for example, distannoxane catalyst) (see Hori. Y. , M/ Suzuki, Y. Takahashi, Y. Ymaguchi and T. Nashishita,suits, if the polymerization catalyst has a high reactivity towards one enantiomer compared to others. Depending on the degree of preference can be obtained separate R or S stereophotomaker, stereoblock copolymers or a mixture of stereoblock copolymers and stereophotomaker (see Le Borgne.A., and N. Spassky, Polymer, Vol., 30, pp. 2312-2319 (1989); Tanahashi. N. , and Y. Doi, Macromolecules, Vol., 24, pp. 5732-5733 (1991); and Benvenuti. M. , and R. W. Lenz, J. Polym.Sci.; Pert A: Polym. Chem. Vol., 29, pp.793-805 (1991)). Known to some initiators or catalysts to obtain mainly syndiotactic polymer, polymers with repeating units of alternating R and S stereocontrol from racemic monomer (see, Kemnitzer.J.E., S. P. McCarty and R. A. Gross, Macromolecules, Vol. , 26, pp. 1221-1229 (1993)), while some initiators or catalysts can provide all three types of stereopairs (see Hocking, P. J. and R. H. Marchessault, Polym. Bull., Vol.30, pp. 163-l70 (1993)).

For example, obtaining the copolymer(3-hydroxybutyrate-co-3 - hexanoate-with-3-hydroxyalkanoate), where 3-hydroxyalkanoates comonomer is 3-alkyl-propiolactone, where the alkyl group contains at least 3 carbon carried out as follows. Take appropriate precautions to eliminate who is lcil--propiolactone in the desired molar ratio, download via siphon or cannula in kiln dried, purged with argon and treated with flame ampoule of boron-silicate glass or flask equipped with a rubber stopper. The polymerization catalyst is added in the form of a solution in toluene through a siphon. The ampoule gently shaken for mixing reagents (but without contact with the rubber stopper) and then heated in an oil bath at the desired temperature for a prescribed period of time. In the process of the reaction mixture becomes viscous and can harden. If you get isotactic polymer, the solid polymer is precipitated before the complete solidification of the mass. Then the product may be cooled, removed from the ampoule and freed from residual monomer by vacuum drying. On the contrary, the product can then be dissolved in an appropriate solvent (e.g. chloroform) and selected precipitation from solution, which is not a solvent (e.g. ether-hexane mixture, 3:1 vol./about.) and dried in vacuum. The molecular weight determined by standard methods, such as gel permeation chromatography (SEC, also known as gel permeation chromatography or GPC). The content of the co monomer in the polymer is determined using nuclear magnetizing, such as disclosed in patent application U.S. entitled "Polymerization of beta-substituted-beta-propiolactone initiated alkoxides alkylzinc" declared Procter and Gamble Company 28 January 1994. Such initiators have the General formula R1ZnOR2where R1and R2independently represent C1-C10-alkyl. In a preferred method of synthesis of the initiator is chosen from the group consisting of isopropoxide atitinka, isopropoxide medicine, ethoxide atitinka, or methoxide atitinka; more preferably isopropoxide atitinka.

Other copolymers useful in the present invention can be obtained by replacing the original substances (monomers) in the above procedure 3-alkyl-lactones corresponding to the desired Monomeric links in the final copolymer product.

On the contrary, the biological synthesis of biodegradable PHAs that are useful in the present invention, can be carried out by fermentation with the appropriate body (of natural origin or obtained through genetic engineering) with an appropriate nutrient medium (single or multi). Obtaining poly(3-hydroxyalkanoate-co-3-hydroxybutyrate) with Aeromonas caviae disclosed in European the ski samples obtained through genetic engineering, expression of interest copolymers (see application PCT/US93/02187, published February 4, 1993; and patent application U.S. No. 08/108193, filed August 17, 1993; and Poole.R.m, Science, Vol., 245, pp. 1187-1189 (1989)).

Example 1.

Copoly(3-hydroxybutyrate-co-hydroxyhexanoate).

Copoly(3-hydroxybutyrate-co-hydroxyhexanoate) (RNW-NC) receive, in accordance with the conventional methods described above, and based on the procedure published by Hori et.al. (Hori,Y., M. Suzuki, Y. Takahashi, Y. Ymaguchi and T. Nashishita, Macromolecules, Vol., 26, pp.4388-4390 (1993)), for polymerization-butyrolactone. Specifically, purified [S] -3-methylpropionate ([S]--butyrolactone) (9,50 g, 110 mmol) and [S]-3-propylparaben (0.66 g, 5.8 mmole) download via siphon in purged with argon, dry vial with stopper. The initiator is 1,3-dichloro-1,1,3,3-tetramethyldisiloxane prepared according to R. Okawara and M. Wada (J. were obtained.Chem., (1963) vol. 1, pp.81-88) and dried overnight in vacuum at 80oC, dissolved in dry toluene with 0,18 mol/l solution. Through the siphon into the ampoule type of 0.65 ml of initiator solution (0.12 mmole distannoxane). The ampoule gently shaken to mix the contents and then heated at 100oC for 4 hours, immersing the lower part of amniotic time the vials are removed from the oil bath and allow to cool to room temperature. The solid is dissolved in chloroform. Substance produce by precipitation in hexane-ether, collected by filtration and dried in vacuum. The composition of the copolymer is determined using1H-NMR spectroscopy and are within experimental error, that the composition of the copolymer corresponds to the same composition as that of the original mixture (95:5). The molecular weight determined using gel permeation chromatography with chloroform as the mobile phase and for calibration using a standard sample of polystyrene with narrow MMD.

Example 2.

Copoly(3-hydroxybutyrate-co-3-hydroxyhexanoate-with-3 - hydroxyoctanoic).

Copoly(3-hydroxybutyrate-co-3-hydroxyhexanoate - with-3-hydroxyoctanoic) are obtained following the same procedure as described in example 1, except that the monomer mixture used [S]-3-methylpropionate (9,50 g, 110 mmol), [S]-3-propylparaben (0.40 g, 3.5 mmole) and [S]-3-phenylpropiolate (of 0.60 g, 3.5 mmole).

Example 3.

Copoly(3-hydroxybutyrate-co-3-hydroxyhexanoate-with-3 - hydroxydecanoate).

Copoly(3-hydroxybutyrate-co-3-hydroxyhexanoate - with-3-hydroxydecanoate) are obtained following the same procedure described in the example is openproject (0.40 g, 3.5 mmole) and [S]-3-getimplobject (of 0.60 g, 3.5 mmole).

Example 4.

Copoly(3-hydroxybutyrate-co-3-hydroxyhexanoate-with-3 - hydroxyethanoic).

Copoly(3-hydroxybutyrate-co-3-hydroxyhexanoate-with-3 - hydroxyethanoic) are obtained following the same procedure as described in example 1, except that the monomer mixture used [S]-3-methylpropionate (9,50 g, 110 mmol), [S]-3-propylparaben (0.40 g, 3.5 mmole) and [S]-3-butylparaben (0.45 g, 3.5 mmole).

Example 5.

Compostable single-layer film.

RNW-NC composition 8 mol.% hexanoate/92 mol.% the butyrate is administered in a single screw extruder (Rheomix Model 202) with screw diameter of 1.88, see Use a constant taper screw having a length to diameter, 20:1 and the ratio of the pressure 3: 1. The temperature of both heating zones of the extruder barrel 25oabove the melting temperature RNW-NC. The extruder is equipped with a cylinder, of a width of 15 cm and a gap of 0.1, see the head of the extruder support at a temperature of 20oC above the melting temperature RNW-NC. The copolymer is melted within the extruder and pumped to the head from the other end of the extruder. Rotation of the auger remain constant at 30 rpm Copolymer push through g the I the copolymer prior to lifting. The width of these films is usually 10 cm and a thickness of about 0.05, see

Example 6.

Compostable single-layer film.

Film RNW-HX is made by melting the material between Teflon plates in a Carver Press (Fred S. Carver Inc.,Menomonee Falls, W) at a temperature of 20oabove the melting temperature of the film. The pressure on the plates was adjusted to obtain a film thickness of approximately 0.25 mm, Then the film is equally cooled to room temperature by placing forms between large (5 kg) aluminum plates and cooling to room temperature.

Example 7.

Compostable multilayer film.

Plate film RNW-NH can be prepared as described in example 6. These plates are then put into the base polymer with good oxygen barrier properties and a bad transmission rate of water vapor or polymer film, which may be water soluble, such as polyvinyl alcohol (PVA). The film is placed in a cutting press, stacking in the following order RNW-HX (95:5), RNV-HX (50:50), PVA, RNV-HX (50:50), RNV-HX (95:5). The material is then pressed at a temperature of 5oabove the melting temperature RNW-HX (50: 50), but still below those is to cool to room temperature.

Example 8.

Compostable disposable diaper use.

Baby disposable diaper in accordance with the present invention is prepared as follows. These dimensions correspond to the diaper, suitable for baby weight 6-10 kg of These sizes can be changed in proportion to the different weights of the child or for hygienic underpants for adult users suffering from incontinence, according to standard practice.

1. Lower floor: at 0.020 - 0.038 mm, consisting of MV-NC copolymer (obtained as described in example 6); width of the upper and lower parts 33 cm; with the notch inside on both sides with a width in the center of 28.5 cm; length of 50.2 see

2. Upper floor: Cardo and thermally connected staple fiber (polypropylene of Hercules type 151); the width of the upper and lower parts 33 cm; with the notch inside on both sides with a width in the center of 28.5 cm; length of 50.2 see

3. Absorbent Central layer: includes 28.6 g of cellulose wood pulp and 4.9 g of absorbent gelling particles of material (industrial polyacrylates (Nippon Shokubai); 8.4 mm thickness, celandroni; width upper and lower parts of 28.6 cm; with the notch inside on both sides with a width of which on each side); width of 4.77 mm, length 370 mm; thickness 0,178 mm (all the above dimensions are represented in the unstretched state).

The diaper is prepared in the standard manner by placing the Central material, covered with a top coating on the bottom surface and gluing.

Elastic tape (marked "internal" and "external" corresponding to the bands closer and more remote from the Central part, respectively) stretch to about 50,2 cm and have between the top cover/bottom cover along each longitudinal side of (2 lanes on each side) of the Central part. The inner strip along each side have a distance of about 55 mm from the narrowest part of the Central layer (measured from the inner edge of the elastic band). This provides a spatial element along each side of the diaper, comprising a flexible material top cover/bottom cover between the inner elastic and curved edge of the Central layer. The inner strip is glued down along their length in the stretched condition. Outer bands have a distance of about 13 mm from the inner strips and glued down along their length in the stretched condition. The ensemble of the top coating is I.

Example 9.

Compostable light trousers.

Light trousers, suitable for use between menstrual periods, include a gasket (surface area 117 cm2, SSK, filled with air 3.0 g) containing 1.0 g of absorbing particles gelling material (industrial polyacrylates; Nippon Shokubai); porous strip, which come in between the porous plenkoobrazovatelem top coating according to the U.S. patent 4463045 and bottom floor, which includes a film of copolymer RNW-HX thickness of 0.03 mm, prepared in accordance with example 1.

Example 10.

Composting sanitary napkin.

Menstrual napkin in the form of wipes, having two wings, which are located on the outer side from its absorbent Central layer is made using a gasket obtained in accordance with example 9 (surface area 117 cm2, SSK, filled with air 3.0 g), for U.S. patent b dated 18 August 1987. The materials of the upper cover and the lower cover are the same as described in example 6.

Example 11.

Compostable disposable diaper use.

Made in example 9, by modifying the limera run-HX (prepared as described in example 6).

It is clear that the examples and variants described here are presented only for the purpose of illustration and that various modifications or changes in this regard are obvious to experts in this field and are included in the scope of the claims.

1. Film comprising a biodegradable copolymer, wherein the biodegradable copolymer comprises at least two statistically recurring Monomeric level, where the first statistically recurring Monomeric link has the formula

< / BR>
the second statistically recurring Monomeric link has the formula

< / BR>
and where at least 50% statistically repeating monomer units have the formula of the first statistically recurring Monomeric level, the copolymer has a melting point of from 30 to 160oC and a crystallinity, measured by x-ray analysis, from 2 to 65%.

2. Film under item 1, characterized in that the copolymer includes one or more additional statistically repeating monomer unit having the formula

< / BR>
where R1represents N or C2or4- C19-alkyl or alkenyl;

n = 1 or 2.

3. Film under item 2, characterized in that h is e top floor, permeable to liquid; the lower floor, impervious to liquids, comprising a biodegradable copolymer comprising at least two statistically recurring Monomeric level, where the first statistically recurring Monomeric link has the formula

< / BR>
the second Monomeric link has the formula

< / BR>
and where at least 50% statistically repeating monomer units have the formula of the first statistically recurring Monomeric link and the copolymer has a melting point of from 30 to 160oC and a crystallinity, measured by x-ray analysis, from 2 to 65%, and an absorbent Central layer located between the upper and lower surfaces.

5. Absorbing product under item 4, wherein the biodegradable copolymer comprises one or more additional statistically repeating monomer unit having the formula

< / BR>
where R1represents N or C2or4- C19-alkyl or alkenyl;

n = 1 or 2.

6. Absorbing product under item 5, wherein R1is2or4- C19-alkyl.

7. Absorbing article on p. 4, characterized in that it is made in

 

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Medicinal bandage // 2245164

FIELD: medicine.

SUBSTANCE: invention relates to dressing materials based on polymeric compositions and can be used in surgery and traumatology for closing wounds of different etiology. The polyol component-base medicinal bandage based on propylene oxide or ethylene oxide comprises water, catalyst for urethane formation and isocyanate complex consisting of isomers of diphenylmethane diisocyanate. High-molecular simple polyetherpolyol with molecular mass 3000-10000 Da is used, and isocyanate complex comprises additionally oligourethane isocyanate based on low-chain oligoetherpolyol with the content of isocyanate groups 26.0-29.5 wt.-%. Also, the bandage comprises activation additive consisting of polyurethane chain lengthener, foam-opening agent and foam-hardening agent. Bandage provides exclusion additional pain senses in the patient, enhancing absorption effect and provides absence of skin sticking.

EFFECT: valuable medicinal properties of bandage.

7 ex

FIELD: medicine, special additives.

SUBSTANCE: invention relates to hygroscopic additive that represents particles of hygroscopic additive containing particles of hygroscopic resin (α) and additive improving penetrability for liquid (β) wherein particles of hygroscopic resin (α) represent particles of cross-linked polymer formed from a monomer comprising acrylic acid and/or its salt and subjected for treatment resulting to formation of cross-links on its surface. Particles of the proposed hygroscopic additive show average-mass diameter (D50) in the range from 234 to 394 mcm, logarithm standard deviation (σξ) for distribution of particles by sizes in the range from 0.25 to 0.45, absorbing capacity without loading 15 g/g, not less, and the level of the water-extractive component content 15 wt.-%, not above, and, except for, the level of the additive content improving penetrability of liquids (β) in the range from 0.01 to 5 mass parts per 100 mass parts of particles of hygroscopic resin (α). Proposed hygroscopic additive combines exploitation indices describing both capillary absorption strength and penetrability for a liquid.

EFFECT: improved and valuable properties of additive.

8 cl, 7 dwg, 29 ex

FIELD: medicine.

SUBSTANCE: the present composition includes nonvolatile, a silicone, fluid substance in the mixture with finely divided silicon dioxide and antibacterial active substance. Pharmaceutically active substance is a nondecomposing one and manifests physical stability in the composition.

EFFECT: higher efficiency.

31 cl, 5 ex, 2 tbl

FIELD: biotechnology, microbiology, medicine.

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EFFECT: valuable properties of strains.

43 cl, 12 ex

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FIELD: medicine.

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EFFECT: has improved composition.

33 cl, 4 tbl, 7 ex

FIELD: medicine.

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16 cl

FIELD: medicine.

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7 ex

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EFFECT: multilayer bandage is not adhered to wound and thereby do not interpenetrate with it.

15 cl, 6 dwg

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