Biodegradable thermoplastic composition

FIELD: chemistry.

SUBSTANCE: invention relates to a biodegradable thermoplastic composition for producing materials and articles which are biodegradable in natural conditions. The biodegradable thermoplastic composition contains lignocellulose filler, a binding agent and polyethylene as a polymer base. The binding agent is a copolymer of ethylene and vinyl acetate. The lignocellulose filler used is in form of cheap manufacturing wastes with no food and feed value and natural materials selected from flax shive, sunflower husks, sodium lignosulphonate, leaves and straw.

EFFECT: composition is characterised by high biodegradability and meets requirements for materials for processing using conventional processes and equipment.

5 cl, 3 tbl, 1 dwg

 

The invention relates to a biodegradable thermoplastic compositions, and in particular to compositions containing lignocellulosic materials, and can be used to create materials and products, is able to biodegradation in natural conditions. The problem of waste disposal at the present time is particularly acute. One of the major problems is the high resistance of synthetic polymeric materials to the physical, chemical and biological degradation. Giving synthetic polymers properties Biodegradability microorganisms and natural-climatic factors, such as the action of light, oxygen, moisture, corrosive environments, etc. can significantly reduce the amount of polymer waste and improve the environment. First of all, to biodegradation must be capable of polymeric materials used for the manufacture of goods with small term usage, such as packaging films, bags, disposable tableware etc. of the Existing biodegradable polymers, such as polylactide - biodegradable, biocompatible, thermoplastic polymer based on lactic acid, polyhydroxybutyrate and its analogues, are significantly more expensive than traditional polymers. The possibility of obtaining cheaper biodegradable materials with asana using polymer compositions, including, along with traditional thermoplastic synthetic polymers, biodegradable fillers of natural origin. Known biodegradable polymer compositions containing as filler starch. As the polymer base they may contain cellulose derivatives [RU 96112905 AND, publ. 27.09.1998, EN 2174132 C1, publ. 27.09.2001, EN 2404205 C1, publ. 20.11.2010], polyamides [EN 97121172 AND, publ. 27.08 1999], a copolymer of ethylene and vinyl alcohol [EN 2073037 C1, publ. 10.02.1997] and other polymers. However, starch is a valuable food product, so production on the basis of which the bulk of the material intended for the manufacture of products for short-term use, economically justified. Known biodegradable composition containing as a polymeric bases up to 70-80% of a copolymer of ethylene and vinyl acetate (CMEA), and as fillers of natural origin - waste technological production processing cocoa beans dry cocoa (20,0-40,0 wt.%) [EN 2349612 C1, publ. 20.03.2009] or rye flour (30-48,7 wt.%) [EN 2318006 C1, publ. 27.02.2008]. To improve the compatibility of the ingredients in the composition of the injected surfactant and other processing AIDS. The disadvantage of this technical solution is used as the polymer base is relatively expensive copolymer of ethylene and vinylic the Tata, which increases the cost of the finished product. In addition, the cocoa and rye flour is also relatively expensive fillers and can be used in feed or in food industry. Given the high volume and short time use products from biodegradable polymeric materials, to create compositions, it is advisable to use the cheapest polymer thermoplastics suitable, including, for use in contact with food products as well as cheap, not representing the food and nutritional value fillers. According to the invention [EN 2363711 C1, publ. 10.08.2009], selected as a prototype, biodegradable thermoplastic composition as the polymer base includes industrial and/or household waste polyethylene (67-76 (in Russian), 5 wt.%), as fillers of natural origin, the waste of the food industry - rice husk (20-30 wt.%), as well as technological additives - oligomeric dye (1-2 wt.%) and titanium dioxide (0.5 to 1 wt.%). However, products made from this composition are characterized by low rates of water absorption and physical-mechanical characteristics, which, apparently, is connected with insufficient adhesion between filler and polymer matrix, only due to adsorption interactions. This is ricine biodegradation of the composition occurs due to absorption by microorganisms fragments filler, while the polymer matrix is almost destroyed, which is confirmed by the data of IR spectroscopy. The present invention is the creation of a thermoplastic, biodegradable polymer composition comprising the polymer as component of cheap synthetic polymeric materials, and as a natural filler - cheap, do not pose a food or nutritional value fillers, with the resulting composition should exhibit a high ability to biodegradation under the action of natural factors, but also to meet the requirements of materials for processing using known processes.

The problem is solved, we offer a biodegradable composition comprising polyethylene, lignocellulosic filler and compatibilizer (binding agent), which is used as a copolymer of ethylene and vinyl acetate, in the following ratio of components, wt.%:

Lignocellulosic filler15-60
A copolymer of ethylene and vinyl acetate3-12
PolyethyleneRest

Optionally, the composition may be what led technological additives. Polyethylene, which is a polymeric based composition can be represented by the various brands of polyethylene high and low density, as well as containing polyethylene waste. Currently, the market offers many grades of polyethylene, you can use each of them, however, preferred brands of high-pressure polyethylene (LDPE) (low density), since they are suitable for contact with food products and their supramolecular structure allows optimal to impose a fine filler. It contains polyethylene waste includes waste recycling polyethylene products and waste consumption. Waste recycling are the Gating system and the defective product, waste consumption include packaging, non-food goods, machine parts, instruments, etc. Containing polyethylene waste, generally more oxidized than the original polymer, this property can lead to a better adhesion with the filler and more rapid biodegradation of the polymer part. For use in accordance with the invention, waste consumption must first be cleaned, dried and sorted. Made of composite materials based on plastic waste, it is recommended to make products non-critical purposes and consumer goods, ex the of toys, products in contact with food products, and medical products. As lignocellulosic filler can be used in a wide range of objects of natural origin containing cellulose and/or lignin, however, from an economic point of view it is preferable to use cheap, not representing food and fodder value of technological waste or natural materials, such as fire linseed, sunflower seed husk, sodium lignosulphonate and vegetable objects, such as leaves or straw. The cost of these fillers is substantially lower than the cost of the fillers used in the models and the prototype. For example, the waste product of flax - fire flax - 10 times cheaper rye flour, 30 times cheaper cocoa-Vell and almost 60 times cheaper than starch.

Table 1 shows the content of carbohydrates and/or lignin in the objects, which, in accordance with the present invention, used as a lignocellulosic filler.

Table 1
Lignin-carbohydrate composition of fillers in accordance with the invention
FillersCellulose, wt.%Lignin, wt.% Pentosans, wt.%
Fire flax47-4925-2721-23
Sunflower husks34-3626-2825-27
Birch leaves24-2633-3517-19
Straw cereal46-4817-1923-25
Sodium lignosulphonate-100-

In accordance with the invention, the content of the lignocellulosic filler in the composition may be in the range of from 15 to 60 wt.%. The choice of a particular value within a specified range depends on the type of products for which the composition is intended and how the technological processing of the material. For thin films (less than 100 μm), obtained by extrusion through a flat head, the content of the filler in the composition should be in the range of from 15 to 20 wt.%. At higher filler contents may cause defects in the film due to release on the of omnitele to the surface. Lower filler content is not economically feasible. In the case of thicker films to reduce the cost of the material obtained and the efficiency of biodegradation quantitative content of the filler should be increased. For example, for films with a thickness of 100-250 μm filler content can be increased to 40 wt.%, for films thicker than 250 μm to 50 wt.%. Higher filler contents can lead to the deterioration of the quality of the films. Upon receipt of the films or sheets by pressing the quantitative content of the lignocellulosic filler in the composition, as well as to obtain films by extrusion, does not exceed 50 wt.%. In the manufacture of articles by injection molding or molding (disposable tableware, Cutlery, trays and so on), having a greater thickness than the film, the content of the filler can be increased to 60 wt.%.

A copolymer of ethylene and vinyl acetate (CMEA) plays the role of a binder. Various brands of CMEA, manufactured, which contain from 5 to 30% of vinyl acetate (TU 6-05-1636-97 JSC "Neftehimsevilen", Kazan). Preliminary experiments have shown that the use of brands CMEA, containing about 18% vinyl acetate, is optimal. Compatible with CMEA polymer matrix and the filler due to the presence of acetate groups and et is lenovich links, provides improved interfacial adhesion between the polymer base and the filler by adding to the adsorption mechanism of chemical interaction.

Improved adhesion contributes to improving the accessibility of the polymer matrix for the integrated impact of climatic factors and microorganisms, leading to fracture of the material in the natural environment. This is reflected in the increase in the water absorption of the claimed compositions, and the changing dynamics of biodegradation and character bioreserves impact of natural factors obtained from these products.

As an illustration, in Table. 2 shows the effect of the content of CMEA to reducing weight is subjected to the influence of nature films obtained from compositions containing HDPE and dry birch leaves, and Table. 3 shows the influence of the content of the CMEA on water absorption and reducing the mass subjected to the influence of nature films obtained from compositions containing HDPE and straw of cereals.

Table 2
The change in mass of the sample films containing as a natural filler dry birch leaves, depending on the content of the CMEA
No. The compositionReducing the mass of sample, %
after 2 monthsafter 8 months
1HDPE 70% + birch leaves 30%1,29,1
2HDPE 66,5% + CMEA 3,5% + birch leaves 30%2,39,1
3HDPE 59,5% + CMEA 10,5% + birch leaves 30%4,39,2

Table 3
The change in mass and water absorption of samples of films containing as a natural filler straw cereals depending on the content of the CMEA
No.The compositionWater absorption, wt.%Reducing the mass of sample, %
after 4 monthsafter 8 monthsafter 12 months
1P is VD 70% + straw cereals 30% 8,17,915,1of 17.5
2HDPE 66,5% + CMEA 3,5% + straw cereals 30%11,28,8of 17.018,4
3HDPE 59,5% + CMEA 10,5% + straw cereals 30%14,010,418,920,8

The table shows that the rate of destruction of the sample increases with the introduction of the composition of the CMEA, and the more, the higher the content of compatibilizer.

The changing nature of biodegradable impact of natural factors is illustrated by figure 1, which shows the change in the content of Oh-groups corresponding to the carbohydrate component of the composition in the samples are given in Table. 2. The content of Oh-groups characterized by the area of the peaks in the IR spectra in the region 3100-3590 cm-1corresponding to the content of hydroxyl groups of lignocellulosic filler. Curve number corresponds to the sample number in Table 2.

As can be seen from the figure, in the case of a sample that does not contain CMEA, the maximum reduction of the content of Oh-groups during the first two IU azev with a minimum reduction of weight of the sample (see Table 2) suggests that the fracture is exposed, mainly natural filler. Introduction CMEA changes the nature of the impact of natural factors on the composition: the content of hydroxyl decreases slightly while significantly reducing the mass of the sample, which indicates the polymer component.

Preliminary studies showed that the tensile strength and elongation at break of the films obtained from the compositions, which included CMEA, about 15% higher than for films obtained from compositions not containing compatibilizer.

The quantitative content of the CMEA in the composition should provide a high efficiency of binding of the polymer substrate with a filler at the minimum expense. On this basis, the use of the binder in the amount less than 3 wt.% ineffective, and more than 12 wt.% it is not economically feasible.

The invention is as follows.

Preparation of filler.

Dried at 105°C for 2-3 hours filler is crushed, then diffuse through the sieve analyzer, sieving, or rumble. Directly before mixing with the other components of the filler additionally dried in the same conditions.

Size fractions of filler depends on the method further processing of the resulting company shall stand. For more films by extrusion through a flat head use a fraction of filler, 20-30 μm smaller than the thickness of the finished film. When using extrusion fraction of the filler may be only 10 microns less than the thickness of the resulting films or sheets. In the manufacture of articles by injection molding or molding (disposable tableware, Cutlery, trays and so on), having a greater thickness than the film, it is recommended to use a fraction of filler to 200 microns.

A composition.

Polyethylene is mixed with the required amount of CMEA and the resulting mixture contribute in co-rotating twin screw extruder for melting and homogenization at 140-160°C, after which the mixture make prepared as described above, the filler and continue stirring until complete homogenization of the mixture. The wiring coming out of the head of the extruder, cut into pellets, which are used for subsequent processing and receiving biorazlagaemykh materials one of the known methods.

From the obtained granules can be produced in the film by extrusion using an extruder with a slot die at the same temperature. Pellets can be used for the manufacture of products using injection molding, for which the mixture is subjected to melt in the molding with subsequent injection of the obtained melt wpress form under pressure. You can also get products by molding, for which the granules are poured into the extruder with a flat slotted head, get a tape of a thickness of from 0.1 mm to 3 mm, which is then fed into the molding machine, where it is heated and blown into a mold.

In Table 4 examples of implementation of the claimed invention, is not exhaustive of all the possibilities of its implementation. As the polymer base used high-pressure polyethylene brand 15803-020 in the form of granules. As compatibilizer used CMEA brand 11607-040 containing 18% vinyl acetate.

The ability of materials to biodegradation under the action of natural factors characterized by water absorption for 24 hours (according to GOST 4650-80) and weight loss of the sample in the soil prepared in accordance with GOST 9.060-75, when the exposure for 8 months at a temperature of 25°C.

For comparison, the table shows the characteristics of a pure LDPE (example 1), not having the property of Biodegradability.

Examples 2-5 describe biodegradable thermoplastic composition obtained by using as filler fires linen, received at the primary processing of flax and represents the woody part of flax stalks. The content of carbohydrate and ligninases fraction of the filler shown in table 1. Fire is a waste of textile production is, as a rule, is burned. Flax shive dried at 105°C for one hour, then sieved through a sieve with a mesh size of 200 μm. Just before the introduction into the composition of the sifted dry fire again within 2 h at 105°C.

The mixture is calculated quantities of HDPE and CMEA contribute in a twin screw extruder and homogenized at 150°C for several minutes. In the molten mass is added the appropriate amount prepared as described above, fires linen and continue mixing at a temperature of 150°C for several minutes. Coming from the head of the extruder, the strands are cut into pellets, which are, depending on the content of the filler, a film by extruder with a slot die (examples 2 and 3) or products using injection molding (example 4).

Examples 6 and 7 characterize the biodegradable thermoplastic composition obtained in a similar way using as filler sunflower. The sunflower is the waste oil industry. Typically, the husk is burned, using it as a cheap fuel for boilers. The husk is also used as a feed additive in animal husbandry, but the share of its use is negligible.

Example 8 describes a biodegradable thermoplastic composition obtained as opisanie, using as filler of sodium lignosulphonate. The lignosulfonates are a byproduct of wood processing and represent a mixture of salts of lignosulfonic acids (mixed with reducing and minerals). For the manufacture of polymer compositions in accordance with the invention, use powder sodium lignosulphonate.

Examples 9-11 characterize the biodegradable thermoplastic composition obtained in a similar way using as filler dried birch leaves. For the manufacture of the inventive biodegradable compositions may use any of the leaves, as on the structure and chemical composition of leaves of different plants vary slightly. For example, the content of cellulose and lignin in birch leaves and spruce needles is almost the same. In these examples, the filler used dried birch leaves.

Examples 12-15 characterize the biodegradable thermoplastic composition obtained in a similar way using straw as filler. Straw is a remaining after threshing dry stalks of cereal and legume crops. As raw material for biodegradable composite materials suitable all kinds of straw. The main advantage of straw as mA is eriala are high availability and low cost. In these examples, the filler used straw mixture of cereals.

20,1
Table 4
Characteristics of samples of the compositions obtained in accordance with the invention
# exampleThe composition, wt.%Water absorption, wt.%Weight loss, wt.%Products manufactured from the composition
HDPECMEAFiller
1100--0,020,0Film extrusion
266,53,5Fire flax 307,810,3Film extrusion
359,510,5the sharp linen 30 10,213,2Film extrusion
438,0to 12.0Fire flax 5010,2to 12.0Shovel method of injection molding
528,0to 12.0Fire flax 6011,9a 12.7Shovel method of injection molding
666,53,5Sunflower husks 3011,0the 13.4Film extrusion
759,510,5Sunflower husks 3011,213,5Film extrusion
859,510,5Sodium lignosulphonate 3022,4Film extrusion
966,53,5Birch leaves 307,78,3Film extrusion
1059,510,5Birch leaves 307,99,2Film extrusion
1148,0to 12.0Birch leaves 408,911,2Film extrusion
1282,03,0Straw cereal 15,07,27,5Film extrusion
1366,53,5Straw cereal 30,011,2of 17.0Film extrusion
59,510,5Straw cereal 30,011.618,9Film extrusion
1548,0to 12.0Straw cereal 40,015,420,7Film extrusion

These data show that, compared with polyethylene not containing additives, the samples have a high ability to biodegrade. As technological characteristics contributing to the processing of the materials obtained by the known methods used material density and the melt flow index at a temperature of 190°C., determined in accordance with GOST 15139-69 and GOST 11645-73 respectively. As shown by measurements, the density of the samples is 1.03-1.06 g/cm3that is comparable to the density of HDPE is 0.92 g/cm3. The value of melt flow index, depending on the nature and quantity of filler, ranging from-0.15 to 2.70 g/10 min, which allows the use of materials received for processing by various known methods. Change the content of the components is tov in the composition in the claimed limits can vary physico-chemical characteristics while maintaining a high ability to biodegrade the obtained materials.

1. Biodegradable thermoplastic composition comprising polyethylene, lignocellulosic filler and a binder agent is a copolymer of ethylene and vinyl acetate in the following ratio, wt.%:

Lignocellulosic filler(15-60)
A copolymer of ethylene and vinyl acetate(3-12)
PolyethyleneRest

2. The composition according to claim 1, characterized in that polyethylene is used, preferably, the high-pressure polyethylene.

3. The composition according to claim 1, characterized in that the lignocellulosic filler is a technological waste or natural material containing cellulose and/or lignin.

4. The composition according to claim 3, characterized in that the technological waste or natural material containing cellulose and/or lignin, which are selected from the group: fire linseed, sunflower seed husk, sodium lignosulphonate, foliage, straw.



 

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