Barrier films with calcium carbonate and use thereof

FIELD: chemistry.

SUBSTANCE: film contains a polyolefin base resin and a polyolefin carrier resin which contains 5-35 wt % CaCO3. The base and carrier resins are distinguished by molecular weight, density, flow melt index and/or polydispersity. The film can be multilayered, where the first layer contains one or more compounds such as ethylene vinyl acetate, ethylene ethyl acetate and ethylene acrylic acid, and the second layer is made from polyolefin containing calcium carbonate. The calcium carbonate can be surface-treated with one or more fatty acids having 8-24 carbon atoms. The films have low rate of vapour and moisture penetration.

EFFECT: packaging materials made from said films are moisture sensitive.

33 cl, 5 tbl, 34 ex

 

CROSS-REFERENCE TO RELATED APPLICATION

This application has a priority based on provisional Application for U.S. patent No. 60/755659, filed December 29, 2005, the contents of which are listed here as a reference.

The technical FIELD TO WHICH the INVENTION RELATES

This invention is directed to obtaining a film structure comprising a polyolefin and calcium carbonate, which has reduced the rate of transfer of moisture vapour and is suitable for packaging moisture-sensitive materials, such as dry food, food for animals and pharmaceutical products.

The prior art of the INVENTION

In this application references various publications are given in parentheses. Full citations of these references can be found at the end of the description immediately before the claims. The disclosure of these publications is given here by means of complete references on the subject of the application for a more complete description of the field that is the topical application.

For packaging dry food products and other materials sensitive to moisture, it is preferable that the packaging had a barrier that prevents the penetration of moisture vapour and thus protects the contents from impregnation moisture. The packaging must allow placement of the food material in the container in the form of cardboard boxes for what was on the shelf and to facilitate handling.

Were developed polymer film to increase and not reduce the penetration of moisture vapour through the film (for example, PCT international publication number WO 02/10275 A2, 03/020513 A1 and WO 03/031134 A1). In contrast, reduced the rate of penetration of water vapor (SPV) was achieved using laminated cardboard substrate, which is suitable as a container for beverages (Publication of the patent application U.S. No. 2004/0105942). Reduced SPV was also obtained through the orientation films of high density polyethylene (HDPE) (U.S. Patent№4183893, 4870122, 6391411).

Although there are various technologies that provide a barrier against vapor moisture in packaging films, there is a need for improved barrier films for packaging dry food products and other materials sensitive to moisture, where the film has resistance to moisture, and efficiency.

The INVENTION

The present invention satisfies this need through the use of calcium carbonate (caso3to obtain improved polyolefin barrier films. Barrier film provides good resistance against vapor moisture, heat welding and properties to facilitate handling. Barrier structure consists of a polyolefin film containing calcium carbonate, in the form of a single layer or what mnogosloinoi film design. In structures with a large number of film barrier layers, including caso3Caso3provides each of the many barrier layers reduced the rate of penetration of moisture vapour through the respective barrier layers. These films are particularly suitable for food packaging, packaging of food for animals, packaging of pharmaceutical products and for packaging other materials moisture-sensitive.

Incremental objectives of the invention will be apparent from the description which follows.

DETAILED description of the INVENTION

The present invention is directed to the fabrication of films, including polyolefin and calcium carbonate, and the films have a reduced rate of penetration of moisture vapour (SPV).

Polyolefins are a family of polymers derived from olefinic monomers. Examples include polyethylene (PE), polypropylene and polyisoprene. PE can be high density polyethylene (HDPE, density ≥0.95 g/cm3), Medium density polyethylene (PESP, the density of 0,934 to less than 0.95 g/cm3), low density polyethylene (LDPE, density less 0,934 g/cm3). LDPE can be linear LDPE (LLDPE). HDPE is the preferred polyolefin. HDPE with an average molecular mass (hmm-HDPE) HDPE is the preferred.

Used herein, the polymers with an average molecular mass (hmm) have the following mass distribution: srednekamennogo molecular weight (Mn) of from 6000 to 13000, srednevekovoy molecular weight (Mw) from 50,000 to 120,000 units, and Z average molecular weight from the 175,000 to 500,000. Preferably, srednekislye molecular weight (Mn) was from 8000 to 11000. Preferably, srednevekovaja molecular weight (Mw) was from 70000 to 100000. Preferably, the Z average molecular weight was from 250,000 to 400,000.

Preferred film includes: a) a polyolefin base resin and (b) polyolefin carrier resin mixed with calcium carbonate (caso3), while caso3and the carrier resin are present at a mass ratio of from 15/85 to 80/20. Preferably, the base resin and the carrier resin were different resins. The base resin and the carrier resin may vary, for example, molecular weight, density, melt index and/or index polydispersity. The rate of polydispersity is private from division srednevekovoi molecular weight (Mw) on srednekamennogo molecular weight (Mn). The carrier resin may have a ratio Mw/Mn, for example, 6.82 and the base resin can have this attitude, for example, 9,35. The carrier resin and the base resin can vary the magnitude of the Z average molecular weight (Mz), while, for example, the carrier resin has a Mz 203000 and the base resin has a Mz 332000.

Another preferred film comprises a polyolefin and calcium carbonate (caso3during this film VK is uchet: (a) a polyolefin base resin, having a melt index of from 0.05 to 2.0 DG/min and density of 0,958 to 0,963 g/cm3; (b) polyolefin carrier resin for caso3moreover , the carrier resin has a melt index 4 to 10 DG/min and density of 0,958 to 0,963 g/cm3; and (C) caso3that is present in the film total concentration of from 5 to 35 wt.%.

Additional preferred film includes: a) a base resin of high density polyethylene (HDPE), HDPE has a melt index of from 0.05 to 2.0 DG/min and density of 0,958 to 0,963 g/cm3; (b) HDPE carrier resin for calcium carbonate (caso3), while HDPE carrier resin has a melt index 4 to 10 DG/min and density of 0,958 to 0,963 g/cm3; and (C) caso3while caso3has a median particle size of 0.7-2.5 μm, the upper section d98 4-15 microns, a surface area of 3.3 to 10.0 m2/g and the total concentration in the film 5-35 wt.%, at the same time, caso3processed by the agent for the surface treatment at the processing level of 0.3-2.3 wt.%, and at the same time, caso3and the carrier resin of HDPE are present at a mass ratio between them from 15/85 to 80/20. Preferably caso3processed by the agent for the surface treatment with a processing rate of 1.5-3 mg agent for surface treatment/m2Caso3. Preferably caso3wet grinded and/or dry grinded before his introduction in the film. Wet the e grinding can be carried out in the absence of grinding tools or in the presence of grinding tools, includes, for example, salt of polyacrylic acid and/or salt of a copolymer of acrylic acid. Preferably the calcium carbonate is dried after grinding. Caso3can be handled by the agent for the surface treatment before and/or during and/or after grinding caso3.

Another preferred film includes: a) high density polyethylene (HDPE)having a density 0,958-0,963 g/cm3and (b) calcium carbonate (caso3), having a median particle size of 0.7-2.5 μm, the upper section d98 4-15 microns, a surface area of 3.3 to 10.0 m2/g and the total concentration in the film 5-35 wt.%.

Caso3and the carrier resin may be present in the film at a mass ratio of from 15/85 to 80/20, for example from 40/60 to 80/20. The preferred ranges for the mass ratios of caso3/the carrier film is from 15/85 to less than 60/40 or to 60/40, for example from 40/60 to ≤60/40 and from 45/55 to 55/45. In the most preferred film of caso3and the carrier resin are present in a mass ratio of 50/50.

Caso3may be present in films with a total concentration of, for example, 5-35 wt.%, preferably 20-30 wt.% and more preferably 25 wt.%. These concentrations are applicable to single-layer films and multilayer films, where some layers may not contain caso3or where different layers can contain a different number is the number of caso 3.

The base resin of the present invention may have a melt index, for example, 0.05 to 2.0 DG/min, preferably 1 DG/min. base resin can have a density 0,958-0,963 g/cm3preferably 0,962 g/cm3. Preferably, the base resin is a high density polyethylene (HDPE). Preferably HDPE is high density polyethylene with an average molecular mass (hmm-HDPE). The base resin, such as SMM-PC resin can be obtained by using the catalysts of the Ziegler-Natta, and they usually fall in the range of melt index from 0.85 to 1.5 DG/min and density from 0,9580 g/cm3and more to the maximum limits for polyethylene obtained without comonomers. The preferred base resin is a resin having the properties of a Resin A (see Table 1 below). In the traditional application areas of the film can be manufactured by extrusion of this material or similar material in its pure form (without any other additives or uterine mixtures). As used herein, this material is called the "base resin".

The carrier resin for caso3may have a melt index 4 to 10 DG/min, preferably about 6.5 to 8.0 DG/min and most preferably of 6.5 DG/min Carrier resin can have a density, for example, 0,958-0,963 g/cm3preferably 0,962 g/cm3. Preferably the carrier resin I which is a high density polyethylene (HDPE). Preferably HDPE is high density polyethylene with an average molecular mass (hmm-HDPE).

Caso3the films may have a median particle size of 0.7-2.5 μm, preferably of 1.4 to 2.0 μm, and more preferably of 1.4 μm. Caso3may have the upper cut d98 4-15 μm, preferably 8-10 microns and more preferably 8 μm. Upper cut d98 called average particle diameter of the calcium carbonate at the 98 th percentile of the masses. Caso3may have a surface area of 3.3 to 10.0 m2/g, preferably 3,3-5,5 m2/g and more preferably 5.5 m2/year

Calcium carbonate may be natural ground calcium carbonate, such as, for example, crushed marble, limestone or chalk, and/or precipitated calcium carbonate (e.g., aragonite, vaterite or calcite). Preferably, calcium carbonate is a natural powdered calcium carbonate. Calcium carbonate can be reduced dry and/or fragmentation in the wet state. Wet grinding is the grinding of calcium carbonate in a liquid medium. Wet grinding can be carried out in the absence of grinding tools or in the presence of grinding tools. You can enter one or more grinding agents, such as polyacrylate sodium salt of polyacrylic acid and/or salt of a copolymer of acrylic acid. E.g. the measures calcium carbonate can be obtained from the marble, which is finely ground in water with a high content of solid particles using a dispersion means for maintaining the suspension of particles during the process. The material is then dewatered, dried, processed and deagglomerated again finely divided individual particles. Drying may be performed using any suitable equipment for drying and may, for example, to include thermal drying and/or drying under reduced pressure using such equipment as an oven, spray dryer (such spray dryer sold by the firm Niro and/or Nara) and/or drying in a vacuum chamber. Drying may be periodic and/or continuous.

Agents for the surface treatment may be added to caso3to facilitate dispersion of caso3in the resin. Agents for the surface treatment may be, for example, one or more fatty acids having from 8 to 24 carbon atoms. These agents include, for example, one or more of such acids as the arachnid acid, Bekenova acid, capric acid, zerotinova acid, ezoterikova acid, lauric acid, myristic acid, montanoa acid, palmitic acid and stearic acid. Preferred processing agents are article is Aranova acid and a mixture of stearic acid and palmitic acid. The fatty acid may be from a plant source. The fatty acid can be kosher. CaCO3can be handled by the agent for the surface treatment with the processing level of 0.3-2.3 wt.% processing agent at 97,7-of 99.7 wt.% Caso3. Preferably the processing level is 0.8-1.1 wt.% processing agent (89,9-of 99.2 wt.% Caso3and more preferably 1.1 wt.% processing agent (to 89.9 wt.% Caso3). Preferably the processing level is 1.5-3.0 mg agent for the surface treatment of 1 m2Caso3more preferably 2-2,4 mg of agent/m2Caso3. In the case crushed of caso3this caso3can be handled by the agent for the surface treatment before and/or during and/or after grinding caso3.

Design packaging films with barrier against vapor moisture is either a single layer or a multilayer. The present invention also aims at obtaining multilayer films that include any of the disclosed here polyolefin films with calcium carbonate. In multilayer films typically used inner contact layer to improve the sealing, while the inner contact layer includes one or more of such compounds as ethylene vinyl acetate (EVA), ethylenethiourea (EEA) and ethylenically acid (EAK). Provide the e vinyl acetate in the contact layer of the resin is usually about 18 wt.%. Depending on the configuration of the extruder in the process of co-extrusion film may be approximately from 2 to 7 or more layers.

The preferred multi-layer film comprises an inner layer comprising one or more such compounds as ethylene vinyl acetate (EVA), ethylenethiourea (EEA) and ethylenically acid, serdechnikov layer polyolefin and calcium carbonate (caso3) and an outer layer comprising a polyolefin and calcium carbonate (caso3). As used here, the terms "inner", "serdechnikov" and "outer" are used to describe and explain the relative position of the various layers in the multilayer film structure. The term "internal" refers to the surface of the packaging film, which comes in contact with the packaged product, and the term "outer" refers to the outer side of the packaging film which is in contact with the surrounding atmosphere. The term "serdechnikov" describes the layer, effectively placed between the inner and outer layers. The multilayer film may have a layered mass distribution, for example the outer layer of 25-35%, serdechnikov layer 50-60% and the inner layer of 10-20%, for example 30% of the outer layer, 55% - serdechnikov layer and 15% of the inner layer.

The concentration of ethylene vinyl acetate (EVA), Ethylenediamine (EEA) or ethylenically key is lots (EAK) film layer, containing EVA, EEA or EAK, may be, for example, 15-20 wt.%. The ethylene vinyl acetate (EVA) may have a density, for example, 0.95 g/cm3. The ethylene vinyl acetate (EVA) may have a melt index, for example, 1.5 DG/min

Another multi-layer film includes at least a first layer containing one or more such compounds as ethylene vinyl acetate (EVA), ethylenethiourea (EEA) and ethylenically acid (EAK), and at least a second layer containing a polyolefin and calcium carbonate (caso3), and caso3is present in the multilayer film in a total concentration of 5-35 wt.%, preferably 20-30 wt.% and more preferably 25 wt.%.

The invention also provides methods of obtaining uterine compositions for the manufacture of films, the methods include mixing any of caso3and polyolefin carrier resin disclosed here. By itself, the calcium carbonate is finely milled powder and can be a difficulties during transportation, dispensing and flow into the extrusion system. To facilitate entry of finely ground mineral in the extrusion process may be prepared in tablet uterine composition selected from polyolefin (e.g. polyethylene) resins (resins) and calcium carbonate (calcium carbonates). Tablet uterine compositions contain calcium carbonate and carried the appropriate resin for binding tablets. Usually add a small amount of antioxidant to prevent degradation of the polymer.

The preferred method involves mixing caso3with a polyolefin carrier resin, and caso3and the carrier resin are present in a mass ratio of 15/85 to 80/20, more preferably from 15/85 to ≤60/40. Another preferred method involves mixing caso3with HDPE carrier resin, while caso3and HDPE are present in a mass ratio between them from 15/85 to 80/20, more preferably from 15/85 to ≤60/40. The methods may include forming uterine compositions in tablet form.

The invention provides fallopian composition obtained by any of the methods disclosed here. Preferred uterine composition, for example, includes 50 wt.% calcium carbonate with a median particle diameter of 1.4 μm, the particle size of the upper edge d98 8.0 µm, with a surface treatment to 1.1 wt.% stearic acid, 50 wt.% the carrier resin of high density polyethylene (HDPE) with a density of 0,962 g/cm3and a melt index of 6.5 DG/min processing Level 1.1 wt.% stearic acid means 1.1 wt.% stearic acid and 98.9 wt.% of calcium carbonate.

The invention also provides methods of making a film comprising a polyolefin and calcium carbonate (caso3), the method involves mixing any of the C uterine compositions disclosed here, with any of the polyolefin base resins disclosed here. Each uterine composition and the base resin may be in the form of tablets, which can be mixed in a predetermined ratio. Mixed tablets are melted and then extruded or stretched in the intermediate film, which can then be stretched with the formation of the final film.

The selection of the carrier resin is very important to determine the final physical properties of the film, especially at higher levels of caso3. As disclosed in the present invention, it is preferable to use a carrier resin which is different from the base resin in order to obtain or higher production efficiency, or higher quality fallopian composition, and/or specified physical properties of the obtained extruded product. Preferred carrier resins are polyethylene with a higher melt index (lower molecular weight), the function of which is to improve the barrier properties to reduce SPV. Preferred carrier resin is a resin having the properties of the Resin (see Table 1 below).

The alternative to using a tablet uterine system for depositing calcium is completely made of resin. In this case, the resin will see the Shana with a given amount of calcium carbonate and tablets. The tablet will then be added directly to the extruder for receiving the extrudate of the requested type.

Methods of producing films may include joint extrusion of the first film layer comprising a polyolefin and calcium carbonate, with the film layer includes one or more of such compounds as ethylene vinyl acetate (EVA), ethylenethiourea (EEA) and ethylenically acid (EAK). For example, the inner film layer including one or more of such compounds as ethylene vinyl acetate (EVA), ethylenethiourea (EEA) and ethylenically acid (EAK), co-extruded with serdechnovym film layer comprising a polyolefin and calcium carbonate (caso3), and with an outer film layer comprising a polyolefin and calcium carbonate (caso3).

In co-extrusion as a method of processing polymer materials have been used for many extruders for feeding polymer in the head block for combining the many threads of the polymer before forming the combined melt in the head. The advantage of using co-extrusion is the ability to form a well-connected structure of many materials with different properties in a single step. A method of manufacturing by co-extrusion in accordance with this invention may, for example, be conducted with two or more kinds of the olefin resins, plasticized by means of two or more extruders and entered in a common cylinder, and causing their contacts inside or in the head opening, to thereby molded in a single phase film with two or more layers.

Preferably, the film was processed with the degree of the bulge (WED) from 1.6:1 to 2.2:1, more preferably of 1.6:1. Preferably, the film was processed in the thickness dimension mil 2.0 to 3.0, more preferably 2.0 to 2.5.

The invention provides a film made of any of the disclosed here.

Preferred is calcium carbonate polyolefin film of the present invention have a reduced rate of penetration of moisture vapour (SPV) through them in comparison with the film, in which there is no caso3. As used here, the rate of penetration of moisture vapour (SPV) and the rate of penetration of water vapor (SPV) are used interchangeably. Preferably, the speed of penetration of moisture vapour was reduced by 10-30% in comparison with SPV through the film, in which there is no caso3. More preferably, when sppv less than 20-30% in comparison with sppv film in the absence in the latter caso3. Even more preferably, when sppv less than 25-30% in comparison with sppv film in the absence in the latter caso3.

The film may have a speed Prony the breath of water vapor (SPV) through them, for example, 0,213-0,230 grams of water vapor-mil/100 inch2film/day, more preferably 0,213 grams of water vapor-mil/100 inch2film/day, at 37,5°C and 100% relative humidity. As here used for values SPV, the term "mil" refers to the thickness of the film, where 1 mil=1/1000 of an inch.

The invention provides a packaging film comprising any of the disclosed films here. These films are particularly suitable for food packaging, food for animals, pharmaceutical products and packaging materials that are sensitive to humidity. Food can be dry foods, such as air cereals cereals or crackers. Reduced SPV in these films, as here disclosed, helps to prevent the penetration of water vapor through them and thereby to maintain the food product from excessive moisture. Transparent packaging allows you to place food in containers in the form of cardboard boxes for display on the shelves and facilitates their transfer and transport. Films provide a longer shelf life of products on the shelves in a cost-effective packaging that meets the various needs. These films can serve as unrestricted films, which are not laminated on a substrate, such as a cardboard backing or other hard substrate.

Present from Britanie illustrated in the next section the Details of the experiment, shown to facilitate understanding of the invention and should not be construed as limiting in any way the scope of the invention defined in the following claims.

DETAILS of EXPERIMENTS

Review

To demonstrate the properties of the polyolefin film having a Supplement of calcium carbonate, a comparative study of extruded three-layer hmm-HDPE film and comparing it to a film of similar design, including 20-30 wt.% calcium carbonate in the entire film structure. The calcium carbonate contained only in the outer and serdechnikov layers but not in the inner layer. Calcium carbonate was administered in the form of uterine composition of calcium carbonate.

Three-layer film was jointly extraditables using SMM-HDPE base resin (Resin a in Table 1), having a density of 0,962 g/cm3and a melt index of 1.0 DG/min for outdoor and serdechnikov layers, with the inner layer made of ethylene vinyl acetate (EVA) (Dupont Evlax® 3169Z) had a density of 0.95 g/cm3the melt index of 1.5 DG/min and 18 wt.% acetate co monomer. The purpose of the inner EVA layer is the achievement of improved sealing due to the lower temperatures of the initiation of sealing and faster shutter speeds to seal in the manufacturing process of the package.

PEFC is inoe distribution during co-extrusion consisted of 30 wt.% the outer layer, 55 wt.% serdechnikov layer and 15 wt.% inner EVA layer. Given the total mineral content was 25 wt.% Caso3in most films (see Table 4 below); it was therefore necessary to 29.5 wt.% calcium carbonate in the outer and serdechnikov layers to form an effective amount. Accordingly, the system of feed additives was set to 58.8 wt.% uterine concentrate and 41.2 wt.% Hmm-HDPE (Resin And Table 1) extrusion of the outer and serdechnikov layers to get to 29.5%in these respective layers, to accurately obtain an effective amount of 25 wt.% in films.

The resulting films were evaluated for their physical properties, including the rate of penetration of moisture vapour (SPV) using the device Mocon PERMATRAN-W® Model 3/33. Comparison of standard films without calcium carbonate thickness of 3.0 mils with the degree of blowing 1.6 films, extruded with a smaller thickness of 2.5 mils) using 25 wt.% calcium carbonate and with the same degrees of the bulge showed improvement SPV shown below.

The presence of calcium carbonate in the outer film layer increases the surface roughness, which provides a more efficient and easy handling of the film during secondary operations on the equipment for manufacturing of packages and allows more easier and better to ensure that the printing on them and R is gistr print. Besides, it's changing surface with the addition of calcium carbonate has been shown to reduce the coefficient of friction.

Although the preferred embodiment is made with reference to jointly extruded polyolefin film having about 25 wt.% the content of calcium carbonate, but recognized that can be used and other relative interest in single or various multilayer structural forms of films. For example, the distribution of layers in the design of the film or the introduction of calcium carbonate (calcium carbonate only in serdechnikov layer) network structure with properties similar to those of the embodiment described in the example.

Details of the experimental work

Measurement of melt index, density, and molecular weight:The melt index was measured using standard method ASTM D 1238-04, Standard Test Method for Melt Flow Rates of Thermoplastics by Extrusion Plastometer. This standard can be found in the Annual Book of ASTM Standards 2005, Section Eight-Plastics Volume 8.01. The density was measured using ASTM standard method D1501-03, Standard Test Method for Density of Plastics by the Density-Gradient Technique. This standard can be found in the Annual Book of ASTM Standards 2005, Section Eight-Plastics Volume 8.01. Molecular weight was determined using gel permeation chromatograph firms Waters. Used pump was 150C operating at a flow rate of 1.0 ml/min in entirely volume of 250 μl at 135°C. The sample was prepared using 12 mg of polyethylene sample, dissolved in 4 ml of 1,2,4-trichlorobenzene. Used columns were Waters Styragel HT3, HT4, HT5 and HT6E. Srednekislye molecular weight (Mn), srednevekovaja molecular weight (Mw) and Z average molecular weight (Mz) was calculated as follows.

Srednekislye molecular weight (Mn) is the total weight of all the polymer molecules in the sample, divided by the entire number of polymer molecules in the sample. Mn mathematically expressed as

where Ni is equivalent to a specific number of molecules in a given molecular mass, and Mi is the mass of a mole of the corresponding molecules.

Srednevekovaja molecular weight (Mw) is the next higher molecular weight, mathematically expressed as

where each molecule gives the contribution to Mw, is proportional to the square of its corresponding mass.

Z average molecular weight (Mz) is the next higher molecular weight compared to Mw, and it is mathematically expressed as

where each molecule gives the contribution to Mz proportional to the cube of its corresponding mass.

The measurement of the permeation rate of moisture vapour:Estimates of the rate of penetration of moisture vapour (SPV) film was placed on the instrument the Mocon Permatran-W Model 3/33. The samples were tested in accordance with ASTM F1249-05 Standard Test Method for Water Vapor Transmission Rate Through Plastic Film and Sheeting Using a Modulated Infrared Sensor operating at 37.8°C. and 100% relative humidity. This standard can be found in the Annual Book of ASTM Standards 2005, Volume 15.09.

Measuring the distribution of particle sizes:Estimate of the distribution of particle sizes (WBR) was carried out by x-ray sedimentation method using a Sedigraph 5100, in accordance with ISO standards 13317-1 General Principles and Guidelines, and 13317-3 X-Ray Gravitational techniques. Measurements by Sedigraph (Sedigraph) was performed in the control mode high-speed analysis using pipelines Tygon c long life when bending. The sample was prepared in the dispersant of 0.2 wt.% sodium hexametaphosphate. a 5.0 gram sample was estimated at 35°C using the internal fixed position of the source/detector x-rays. The measured diameters of the particles in the initial and end points of the sample, respectively, were 50-0,5 ám.

Equipment:

Extruders: For co-extrusion is used machines Battenfeld Gloucester: for the inner layer 2”extruder; for serdechnikov (middle) layer 3.5” extruder for the outer layer 2” extruder.

The ratio of layers: A (Internal)-30% (Serdechnikov)-55% (Outer)-15%.

The set of nets:20/80/20 Mesh. The same configuration of the grids in all three extruders.

Head: 8” the head of the firm Battenfeld Gloucester w/slit in the head size 80 mil.

Annular gap for air: Standard with two edges firm Egan Davis.

Resin:

Table 1
ResinDensityIL (melt Index)MnMwMz
Resin A0,9621,0879982314331501
Resin0,9626,5
Resin0,9628,0913262247203165
Resin D0,9628,0

The density in g/cm3

Resin D contains facilitate processing ftorjelastomery polymer (activator turnover) and showed a bad result against SPV.

Minerals on the basis of calcium carbonate:

Table 2
Minerals with calcium carbonate
The type of calcium carbonate (CC)DescriptionThe median particle size (microns)The upper cut-d98 (µm)Surface area (m2/g)Processing level
ADCFinely crushed marble is ground in a wet condition at 70% solids in the presence of a dispersant in the form of sodium polyacrylate, dried and subjected to surface processing1,485,51.1 wt.%, 2 mg/m2
QwicFinely crushed marble is ground in a wet condition in the absence of dispersant at 20% solids, and dried on the surface has been processed 2,0103,3to 0.8 wt.%, 2.4 mg/m2
The upper section d98 refers to particles of calcium carbonate at the 98th percentile. Processing level relates to surface treatment of caso3a mixture of stearic and palmitic acids.

Way

Ring gap (air): the temperature of the cooling 52-54°F at a pressure of 3.5 lb/in2.

Muddy stripe on the film: size Range in height from 18 to 19 inches.

Performance: Constant at 250#/hour

Conditions: the combination of the extent of the bulge and the film thickness, measured in mils.

Table 3
The machining conditions
ConditionsCF (the degree of the bulge)UnchangedThickness in mils
11,602,00
22,50
32,20 2,00
42,50
51,603,00
62,23,00
CF=the Degree of the bulge

Samples

Table 4
Samples
SampleSpecified wt.% Caso3in the filmUterine mixture of caso3/resinAttitude in masterbatches mineral/resin
Control0--
Sample A20ADC/Resin50/50
Sample25ADC/Resin50/50
Sample30ADC/Smolov 50/50
Sample D25Qwic/Resin50/50
Sample E25ADC/Resin50/50
Sample F25ADC/Resin D60/40
Sample G25ADC/Resin50/50
Sample H25ADC/Resin75/25

Descriptions of the types of resins and types of calcium carbonate (CC) in masterbatches are respectively in Tables 1 and 2.

Comments after testing: Nine samples, including the control and five different uterine mixtures with calcium carbonate was extraditables on line co-extrusion injection blow firms Battenfeld Gloucester for the manufacture of films. Except for samples a and C, each of these samples was abstrogirovalsya at four different conditions (film thickness of 2.0 and 2.5 mils and the degree of blowing of 1.6 and 2.2). Samples a and C are processed only when the film thickness of 2.5 mils and degrees blowing 1,6 who 2,2, respectively. Conditions 5 and 6 (table 3) was used only to control.

Results and discussion

The purpose of the evaluation was to determine which combinations of a set of extrusions and concentrate calcium carbonate provide the greatest resistance to penetration of moisture vapour. It was shown that the film obtained from the Resin And introduced with 25 wt.% calcium carbonate through a 50/50 masterbatches, or Resin, or C (table 1) with calcium carbonate (CC) type a (table 2), has secured the highest improvements in SPV, when produced, the extent of the bulge 1.6 and when the film thickness of 2.5 mils. In Tables 5A-5C illustrates the properties of the films, including the effect on the rate of penetration of moisture vapour in them. Codes in Tables 5A-5C for the samples and the process conditions are in Tables 3 and 4.

Reviewed here films provide a cost-effective tool in comparison, for example, metallized films, because they are films with low SPV, which can be used for packaging moisture-sensitive products, such as dry food.

Table 5A
The results of the behavior of the films (continued and Tables 5B and 5C)
The condition of the sample and processThe content of CaCO3in masterbatchesThe base resin for masterbatchesType caso3(QC)Caso3in the filmCaso3in the film (after burning to ash)CF (the Degree of the bulge)The thickness of films
Specified-
Naya
Measured-
Naya
When the basic weight
wt.%wt.%milmilmil
Control
NYY
10 0,191,622,011,46
Control
NYY
200,161,62,52,632,15
Control
NYY
300,152,221,971,6
Control
NYY
400,152,22,52,472,11
Control
NYY
50 0,031,633,112,31
Control
NYY
600,122,233,062,54
A250InADC2020,201,62,5to 2.57to 2.67
A450InADC2019,452,22,52,46of 2.51
In150InADC25 24,191,621,962,11
In250InADC2523,701,62,52,432,77
In350InADC2525,702,222,03of 2.26
In450InADC2524,432,22,52,452,79
250InADC3028,52 1,62,52,582,87

450InADC3028,622,22,5to 2.572,78
D150Qwic2526,581,622,022,18
D250Qwic2525,201,62,52,562,7
D350Qwic25 24,712,222,032,17
D450Qwic2525,642,22,52,532,75
E150ADC2523,901,622,042,19
E250ADC2524,231,62,5to 2.572,72
E350ADC2523,83 2,222,04of 2.21
E450ADC2524,282,22,5of 2.512,6
F160DADC2521,601,621,992,23
F260DADC2521,781,62,52,542,8
F360DADC2526,272,2 21,972,2
F460DADC2523,982,22,52,462,63
G150InADC2525,621,621,912,23
G250InADC2527,201,62,52,42,85
G350InADC2524,702,22 1,932,24
G450InADC25to 26.022,22,52,552,86
N175InADC2522,821,621,971,91
N275InADC2526,701,62,52,522,83
N375InADC2525,242,222,07 2,19
N475InADC2530,252,22,52,542,83

Table 5B
The results of the behavior of the films (continuation of Table 5A)
The condition of the sample and processSPVpspvpspv (2)The influence of caso3The influence of the degree of the bulge
MeasuredSpecifiedpspvpspv
g/100 inch2/dg-mil/100 inch2/dg-mil/100 inch2/d% improvement% improvement
Pin the Aulnay 10,1770,3560,354
Control2to 0.1080,2840,270
Control30,132is 0.2600,26426,91
Control40,0970,2400,2438,45
Control50,0940,2920,282
Control60,0750,2300,225
A 20,10,2570,2509,52
A40,0920,2260,23012,9711,94
In1is 0.1350,2650,27025,63
In20,0910,2210,22822,15
In30,1070,2170,21416,4717,91
In40,0870,2130,21818,033,61
20,095 0,2450,23813,71
40,0970,2490,2434,13-1,71

D10,1230,2480,24630,16
D20,0950,2430,23814,38
D30,1150,2330,23010,236,04
D40,0920,2330,23010,494,29
E10,139 0,2840,27820,30
E20,0960,2470,24013,14
E3amount of 0.1180,2410,236the 7.4315,11
E40,0970,2430,2436,371,32
F10,1610,3200,3229,94
F20,1150,292in 0.288-2,84
F30,1340,2640,268 -1,5217,61
F40.104 g0,256is 0.2601,6212,41
G1is 0.1350,2580,27027,52
G20,0950,2280,23819,73
G30,1150,2220,23014,6513,92
G40,0890,2270,22312,720,46
N1of € 0.1950,3840,390-7,98
N20,1210,3050,303-7,35
N30,1290,2670,258-2,6930,49
N40,0910,2310,228to 11.1124,20

In
Table 5C
The results of the behavior of the films (continued Tables 5A and 5B)
The condition of the sample and processThe HDPE film thickness of 2.5 mils, containing caso3in comparison with HDPE film thickness of 3.0 mils (without caso3)The average improvement pspvThe average improvement pspv
pspv
% improvement% improvement% improvement
Control1
Control2
Control3
Control4
Control5
Control6
A211,24
A4
123,8920,57
In224,36
In317,25
B47,12
C216,168,92
C4-8,62

D122,27to 16.31
D2the value of 16,81
D310,36
D4-1,42
E116,7211,81
E215,61
E36,90
E4-6,09
F13,551,80
F20,08
F30,05
F4-11,48
G123,6318,66
G222,01
G313,69
G41,11
N1-7,66-1,73
N2-4,30
N34,21
N4-0,71

Notes to Table 5B: "SPV" is the source sppv, "pspv is sppv adjusted using the measured thickness, "the Impact of caso3" shows the improvement in sppb (measured and corrected taking into account the thickness in comparison with the control film of the same thickness and film orientation (CF), "the Impact of CF" shows the improvement in sppb caused WED with equivalent content of caso3and the film thickness. Positive numbers indicate an improvement (for example, on a reduced SPV); a negative number indicates wkhuds the interview.

Notes to Table 5C: Comparison of column 3 is held between the film thickness of 2.5 mils, containing caso3and pure HDPE film thickness of 3.0 mils at equivalent CF. "The average improvement pspv" in column 5 is the average improvement in sppb samples containing caso3in comparison with the control, depending on film thickness and CF. Positive numbers indicate improvement; a negative number indicates a deterioration.

LINKS

PCT International Publication No. WO 02/10275 A2, published February 7, 2002, Eastman Chemical Company.

PCT International Publication No. WO 03/020513 A1, published March 13, 2003, Kimberly-Clark Worldwide, Inc.

PCT International Publication No. WO 03/031134 A1, published April 17, 2003, Imerys Minerals Limited.

U.S. Patent Application Publication No. 2004/0105942 A1, published June 3, 2004.

U.S. Patent No. 4183893, issued Jan. 15, 1980.

U.S. Patent No. 4870122, issued Sept. 26, 1989.

U.S. Patent No. 6391411 B1, issued May 21, 2002.

1. Barrier film, including:
a) a polyolefin base resin; and
b) a polyolefin carrier resin mixed with caso3;
at the same time, caso3and the carrier resin are present in a mass ratio of 15/85 to 80/20, where caso3present in the film in a total concentration of from 5 to 35 wt.%.

2. The film according to claim 1, in which the base resin and the carrier resin are different resins and preferably differ in molecular weight, density, melt index and/or index polydispersity.

3. The film according to claim 1, in which the th carrier resin has a melt index from 4 to 10 DG/min

4. The film according to claim 1, in which the carrier resin has a density from 0,958 to 0,963 g/cm3.

5. Barrier film, including:
a) a polyolefin base resin having a melt index of from 0.05 to 2.0 g/cm3and the density of 0,958 to 0,963 g/cm3;
b) a polyolefin carrier resin for caso3while the carrier resin has a melt index from 4 to 10 DG/min and density of 0,958 to 0,963 g/cm3;
(c) caso3;
moreover, caso3present in the film with a total concentration of from 5 to 35 wt.%.

6. The film according to claim 5, in which caso3and the carrier resin are present in a mass ratio of 15/85 to 80/20.

7. Multilayer barrier film, in which at least one first layer of a multilayer film includes one or more of such compounds as ethylene vinyl acetate (ETI), ethylenethiourea (EEA) and ethylenically acid, and at least one second layer of the multilayer film includes a polyolefin and calcium carbonate (caso3), and in which caso3is present in a total concentration of from 5 to 35 wt.%.

8. Multi-layer film according to claim 7, in which layers of a film including a polyolefin and calcium carbonate (caso3)include polyolefin carrier resin, and in which caso3and polyolefin carrier resin are present in a mass ratio of 15/85 to 80/20, and possibly polyolefin carrier resin has a suffix is melt from 4 to 10 DG/min

9. The film according to claim 1, including:
a) a base resin of high density polyethylene (HDPE), HDPE base resin has a melt index of from 0.05 to 2.0 DG/min and density of 0,958 to 0,963 g/cm3;
b) HDPE carrier resin for calcium carbonate (caso3), while HDPE carrier resin has a melt index from 4 to 10 DG/min and density of 0,958 to 0,963 g/cm3;
(c) caso3and caso3has a median particle size of from 0.7 to 2.5 μm, the upper section d98 from 4 to 15 microns, a surface area of from 3.3 to 10.0 m2/g and the total concentration in the film is from 5 to 35 wt.%, at the same time, caso3was processed by the agent for the surface treatment with the level of processing from 0.3 to 2.3 wt.%, and caso3and HDPE carrier resin are present in a mass ratio of 15/85 to 80/20.

10. The film according to claim 9, in which caso3crushed in a wet condition and/or in the dry state prior to introduction caso3in the film, and preferably milled in the wet state in the presence or absence of tools for grinding, and more preferably milled in the wet state in the presence of tools for grinding, including salt polyacrylic acid and/or salt of a copolymer of acrylic acid, where the calcium carbonate may be dried after grinding, and possibly caso3processed by the agent for the surface treatment before and/or during the wedding ceremony is, and/or after the grinding, preferably with the level of processing from 1.5 to 3 mg of the agent for surface treatment/m2Caso3.

11. The film according to claim 1, where the base resin and the carrier resin are the same, including:
a) high density polyethylene (HDPE)having a density of 0,958 to 0,963 g/cm3and
b) calcium carbonate (caso3) with median particle size of from 0.7 to 2.5 μm, preferably from 1.4 to 2.0 μm, and more preferably 1.4 µm, upper cut d98 from 4 to 15 μm, preferably from 8 to 10 microns and more preferably 8 μm, a surface area of from 3.3 to 10.0 m2/g, preferably from 3.3 to 5.5 m2/g and more preferably 5.5 m2/g, and a total concentration in the film is from 5 to 35 wt.%.

12. The film according to any one of claims 1 to 11, in which caso3was processed by the agent for the surface treatment with the level of processing from 0.3 to 2.3 wt.%, preferably from 0.8 to 1.1 wt.%, and more preferably 1.1 wt.%, and where is agent for the surface treatment may be one or more fatty acids having from 8 to 24 carbon atoms, and preferably one or more of such acids as arachnid, Bekenova, capric, zerotinova, ezoterikova, lauric, myristic, montanosa, palmitic and stearic acid, and more preferably the agent for the surface treatment contains stearic what iSlate.

13. Multi-layer film comprising the film according to any one of claims 1 to 12.

14. The method of obtaining uterine composition based on calcium carbonate (caso3) and polyolefin to obtain component (b) of the barrier film according to claim 1, comprising mixing caso3with a polyolefin carrier resin, preferably a high density polyethylene (HDPE), and caso3and the carrier resin are present in a weight ratio of from 15/85 to ≤60/40.

15. The method of obtaining uterine composition based on calcium carbonate (caso3) and high density polyethylene (HDPE) to obtain a film, comprising mixing caso3and HDPE carrier resin, and caso3and the carrier resin are present in a mass ratio of 15/85 to 80/20.

16. The method according to 14 or 15 in which the carrier resin has a melt index from 4 to 10 DG/min

17. The method according to 14 or 15, in which caso3has a median particle size of from 0.7 to 2.5 μm, preferably from 1.4 to 2.0 μm, and more preferably 1.4 µm.

18. The method according to 14 or 15, in which caso3has an upper cutoff d98 from 4 to 15 μm, preferably from 8 to 10 microns and more preferably 8 μm.

19. The method according to 14 or 15, in which caso3has a surface area of from 3.3 to 10.0 m2/g, preferably from 3.3 to 5.5 m2/g and more preferably 5.5 m2/year

20. The method according to 14 or 15, in which CAC is 3was processed by the agent for the surface treatment with the level of processing from 0.3 to 2.3 wt.%, preferably from 0.8 to 1.1 wt.% and more preferably 1.1 wt.%, and where is agent for the surface treatment is one or more fatty acids having from 8 to 24 carbon atoms, preferably one or more of such acids as arachnid, Bekenova, capric, zerotinova, ezoterikova, lauric, myristic, montanosa, palmitic and stearic acid, and more preferably the agent for the surface treatment contains stearic acid.

21. Uterine composition with calcium carbonate to obtain the component (b) of the barrier film according to claim 1, comprising 50 wt.% calcium carbonate with a median particle diameter of 1.4 μm, with a particle size of 8.0 μm on the top slice d98, when a surface treatment 1.1 wt.% stearic acid, 50 wt.% the carrier resin of high density polyethylene (HDPE) with a density of 0,962 g/cm3and a melt index of 6.5 DG/min

22. A method of producing a film according to claim 1, containing a polyolefin and calcium carbonate (caso3), comprising mixing (a) uterine composition according to item 21 or uterine composition obtained by the method according to p-20, and (b) a polyolefin base resin.

23. The method according to item 22, in which caso3present in the film in a total concentration of from 5 to 35 wt.%.

24. Uterine composition is, obtained by the method according to any of p-20.

25. The film obtained by the method according to any of PP and 23.

26. The film according to any one of claims 1 to 11, 13, and 25, or obtained by the method according to any of PP-20, and 22 and 23, where the carrier resin is high density polyethylene with an average molecular mass (hmm-HDPE).

27. The film according to any one of claims 1 to 11 or 13 and 25, or obtained by the method according to any of PP-20, and 22 and 23, where the concentration of caso3in the film ranges from 20 to 30 wt.%, preferably 25 wt.%.

28. The film according to any one of claims 1 to 11, or 13 and 25, or obtained by the method according to any of p-20 or 22 and 23, where the carrier resin has a melt index from about 6.5 to 8.0 DG/min and preferably about 6.5 DG/min

29. The film according to any one of claims 1 to 11 or 13 and 25, or obtained by the method according to any of p-20 or 22 and 23, where the mass ratio caso3/carrier resin is from 40/60 to 80/20, preferably from 40/60 to ≤60/40, more preferably from 45/55 to 55/45, and most preferably 50/50.

30. The film according to any one of claims 1 to 11 or 13 and 25, where the rate of penetration of moisture vapour (SPV) reduced in comparison with the film, in which there is no caso3.

31. The film according to item 30, where the rate of penetration of moisture vapour (SPV) reduced by 10-30%, preferably 20-30%, and more preferably 25-30% in comparison with sppv film, in which there is no caso3.

32. The film according to any one of claims 1 to 11 or 13 and 25, where MSE is the awn penetration of moisture vapour (SPV) is 0,213-0,230 grams of water vapor-mil/100 inch 2film/day at 37,5°C and at 100% relative humidity and preferably is 0,213 grams of water vapor-mil/100 inch2film/day at 37,5°C and 100% relative humidity.

33. Packaging film containing film according to any one of claims 1 to 13 and 25-32, where the film is a packaging film preferably for materials sensitive to moisture, such as packaging film for food for animals or the packaging material for a pharmaceutical product, and more preferably for dry food products, such as air cereals cereals or crackers.



 

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1 tbl

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2 tbl, 7 ex

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FIELD: chemistry.

SUBSTANCE: rubber mixture based on ethylene propylene diene rubber SKEPT-40 contains the following, pts. wt: SKEPT-40 100, sulphur 2, zinc oxide 5, stearic acid 1, technical carbon P-234 100, tetramethylthiuram disulphide 1.5, mercaptobenzthiazole 0.5, modifier 2. The modifier is preferably obtained from reacting epoxy diane resin ED-20, epichlorohydrin and aniline in weight ratio 4:1:2.5, respectively, at temperature 150°C.

EFFECT: invention increases rubber adhesion when gluing with chloroprene adhesives 88CA and 88H, improved physical and mechanical properties.

3 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to polymer-based construction materials used in making chemical-resistant, high-strength articles and structures. The polymer-concrete mixture contains the following in wt %: low molecular weight polybutadiene 8-11; sulphur 4.0-5.5; thiuram 0.15-0.35; captax 0.04-0.12; diphenylguanidine 0.04-0.12; zinc oxide 1.0-2.4; calcium oxide 0.45-0.60; thermal power plant flue ash 8-10; quartz sand 22-25; crushed granite stone 44.91-56.32.

EFFECT: invention enables to obtain a composite with high heat resistance with shorter polymer-concrete vulcanisation time.

3 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: rubber mix is prepared from butadiene-nitrile rubber BNKS-18 AMN with addition of powdered ultra-high-molecular-weight polyethylene (UHMWPE) in the following ratio of components, wt %: BNKS-18 AMN butadiene-nitrile rubber 40-46.3; SKMS-10 RKP rubber 19.0; stearine 0.54; zinc white BT-M 1.63; sulphur 0.54; diaphene FP 0.54; paraffin 0.54; dibutylphthalate 3.2; technical rubber P-701 25-31.3; UHMWPE 1.63; sulfenamide T 0.54; thiuram 0.54.

EFFECT: high oil and moisture resistance and frost resistance of cushion pads.

1 tbl

FIELD: chemistry.

SUBSTANCE: modifying composition contains carbon-chain rubber, sulphur and quinol ether in the following ratio, pts. wt: rubber 100, sulphur 8-12, quinol ether 6-10. The modifying composition enables utilisation of rubber wastes of different composition. The product obtained using the modifying composition is used independently as a commercial-grade rubber mixture and as an additive to other rubber mixtures.

EFFECT: improved environmental friendliness due to utilisation of rubber wastes of different composition, wide range of modifiers for utilising rubber wastes.

6 tbl, 57 ex

FIELD: chemistry.

SUBSTANCE: method involves: (A) putting a product in a packing article, containing a multilayer wrapping film welded onto itself, (B) heat sealing the closed product so that the product is surrounded by the multilayer wrapping film; (C) heating the packed product to temperature of at least 212°F for at least approximately 0.5 hours, where heating takes place in the presence of vapour under pressure. The multilayer wrapping film contains: (1) a cross-linked first outer layer which serves as an insulating layer and the in contact with the product, and (2) a cross-linked O2-impermeable layer containing a mixture of: (i) 50-95 wt % in terms of the weight of the mixture of amorphous polyamide, which contains at least one polyamide selected from a group comprising PA-6I/6T; PA-MXD,I/6,I; PA-6/6,T; PA-6/6I; PA-6,6/6,I; PA-6,6/6,T; and (ii) polycrystalline polyamide which contains at least one polyamide selected from a group consisting of (a) 5-50% of the weight of the PA-MXD,6/MXD,I mixture and (b) 5-15% of the weight of the mixture, polyamide with or without a nucleating agent, having reduced viscosity measured in accordance with the ISO 307 test method from 150 ml/g to 245 ml/g.

EFFECT: obtaining a packed food product sterilised in an autoclave and having a long shelf life.

11 cl, 2 ex, 2 tbl, 2 dwg

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