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Pectin- and chitosan-based biodegradable film

Pectin- and chitosan-based biodegradable film
IPC classes for russian patent Pectin- and chitosan-based biodegradable film (RU 2458077):
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Method for production of pectin material / 2250220
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Method for production of pectin material / 2250219
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Polymer composition for moulding biodegradable articles from molten mass Polymer composition for moulding biodegradable articles from molten mass / 2446191
Invention relates to chemical and food industry, particularly to production of biodegradable plastic materials and can be used to make moulded or film articles for various purposes, including food purposes. The polymer composition for moulding biodegradable articles from molten mass contains polyolefins, biodegradable filler - starch and a process additive, which is a protein phosphatide concentrate (or fuzz) - a by-product of production of unrefined sunflower or rapeseed oil.

FIELD: chemistry.

SUBSTANCE: biodegradable film contains pectin, chitosan, water, 1N hydrochloric acid, a plasticiser - glycerine and a structure-forming agent - 3% methyl cellulose solution.

EFFECT: obtaining a uniform biodegradable film without structural defects, which similar to household packaging polyethylene films on homogeneity, plasticity and strength.

2 dwg, 1 tbl

 

The invention relates to compositions of biodegradable films containing pectin for use in pharmaceuticals, medicine, veterinary medicine, food or cosmetic industry and for the manufacture of wrapping food film capsules.

Known taken as the prototype of a highly elastic layered film made of chitosan and pectin. As the plasticizer can be added glycerine or lactic acid, and pectin or chitosan solution used for the manufacture of the film, may be added to the starch. The resulting layered film is biodegradable and made from renewable agricultural raw materials (U.S. patent No. 5919574).

The disadvantage of the prototype is the considerable complexity of manufacturing the layered film, as it is necessary separately to produce a layer of pectin and chitosan layer film, in addition, the juxtaposition of these films to each other can be associated with the appearance of air bubbles between the layers, which is almost impossible to remove because the layers of the film sufficiently firmly stick together among themselves.

Object of the invention is the simplification and acceleration of the process of making films of pectin and chitosan, obtaining biodegradable film with characteristics similar to plastic packaging films.

Technical resultativity is to obtain homogeneous biodegradable films based on pectin and chitosan without flaws patterns, similar homogeneity, plasticity, strength for packaging plastic films domestic use.

The technical result is achieved by the fact that in biodegradable film obtained from pectin, water, chitosan, odnomomentnoe hydrochloric acid and plasticizer according to the invention as a plasticizer use glycerin, and the film contains the amendment a three percent solution of methyl cellulose in the following ratio, wt.%:

pectin 35-37
chitosan 35-37
water 7-8
odnomomentna hydrochloric acid 7-8
glycerin 5-6
a three percent solution of methyl cellulose the rest of it.

The figure 1 shows pictures of biodegradable films based on pectin and chitosan according to the invention. The figure 2 shows photographs of the decomposition proposed film for 8 days.

In the biodegradable film according to the invention, the optimum ratio of pectin and chitosan should be closer the ina 1:1. This ratio allows the films according to the invention to be strong (pectin gives the film studentsT), the lack of pectin structure of the film becomes too loose and liquid, the film may not harden. And when the excess pectin film becomes inflexible, at the same time the decomposition of the film increases, which is due to the greater density of the films.

Chitosan is responsible for compatibility with animal tissue. Exposed to natural fungi, films containing chitosan, have a built-in source of nitrogen to increase biodegradation. I.e. the lack of chitosan significantly increases the period of decomposition films, reduced their degree of safety for the body. When excess chitosan film is opaque, will have a cloudy white color.

Glycerin is responsible for the plasticity and flexibility of the films. When his lack of film is not stretched, bending cracks. With an excess of glycerol film is poorly separated from the surface becomes sticky, viscous.

A three percent solution of methyl cellulose makes the film stronger. In excess of this component of the film becomes fragile. The lack - delicate, fragile.

Biodegradable film according to the invention was prepared as follows. Pectin is dissolved in distilled water. Then Lu is the better dissolution of the components of the solution are placed in a thermostat for 1 minute at a temperature of 37-38°C. Chitosan was dissolved in 1 BC (odnomomentnoe) hydrochloric acid. For better dissolution of the components of the solution are placed in a thermostat for 1 minute at a temperature of 37-38°C. Then the obtained solutions of pectin and chitosan preferably in equal proportions poured and stirred until complete dissolution of the formed clots. In order for the film was solid and uniformly separated from the substrate after stirring clots in the resulting solution add the plasticizer and the amendment.

The mixture is carefully poured into a Petri plate. Film formed on the glass substrate (in the Petri plate) for 20-24 hours at a temperature of from 0 to 25°C.

The result is a homogeneous, transparent (depending on the thickness of the film is transparent or slightly turbid) film. The film is flexible, so that, when folded, does not form cracks during extension, the film takes its original state. The film has no colour, smell. It can be painted various dyes, such as food, since they are harmless to humans. The film may take various forms depending on the shape of the vessel into which is poured a solution: in the bowl Petri - round film (figure 1), in square container - square film. Change the color and shape of the films had no effect on their properties.

The strength of biopolymer films was determined in accordance with Shasta 17035-86 using a universal testing machine with an Electromechanical drive (GOST 7855-84). Strength σr, MPa (H/mm2) was calculated by the formula:

,

where σr- tensile strength (MPa) N/mm2),

Fr- tensile force (N),

And0- the cross-sectional area (mm2).

The strength of the obtained film are shown in table 1, where also the values of the indices of the films according to the invention in comparison with the similar indicators of polyethylene. As one of the main objectives of the present invention was to get a decent analog plastic packages, the most important properties of the resulting polymer films are shown in the table with the same properties of polyethylene films for domestic use (packaging). Based on these data we can conclude that the strength of polymer films is close to the strength of the polyethylene, but their safety and ability to undergo biodegradation expands the scope of their application.

Table 1 shows the composition obtained according to the invention the film: its thickness is h, the length of the circumference is taken of the fragment - 1, the stretchability of the material in width in one direction - σwidththe stretchability of the material in the length in the other direction - σlength.

Table 1
h, mm l0mm σwidth, MPa σlength, MPa
The composition of the obtained film:
the methylcellulose 0,06 15 12,2 13,8
pectin
chitosan
glycerin
water
1 N. HCl
Plastic film 0,04 15 13,7 14,7

The film thickness was measured using a micrometer ELECTRO MS DIGITAL MICROMETER. She was 0,074 mm At different instances made film thickness ranged from 0,075 up to 1 mm.

Evaluation of biodegradation of the films was carried out in the soil environment. Fresh film from a mixture of chitosan - pectin were fully biodegradable for 8 days (figure 2). After three-month storage film is decomposed, for 15 days, after half a year for 23 days.

The invention is illustrated by example.

10 mg Apple Petina dissolved in 2 ml of distilled water. For a better solution was placed a solution in thermostat for 1 minute at a temperature of 37-38°C.

10 mg molefractions of chitosan from crustacean shell (manufacturer - JSC "Bioprogress") dissolved in 2 ml of 1 N. (odnomomentnoe) HCL. For a better solution was placed a solution in thermostat for 1 minute at a temperature of 37-38°C.

Then merge the resulting solutions of pectin and chitosan. During draining of the solution of pectin with an equal volume of chitosan solution is the formation of clots at the contact interface of the two liquids. The clots have a gel-like structure. When defending going on the t slow deposition of clots at the bottom of the vessel without the formation of a homogeneous mass. Clots or removed from the solution, or stir until smooth. In order for the film was solid and uniformly separated from the substrate after stirring clots in the resulting solution add the plasticizer and the amendment. To impart plasticity add 1.5 ml of the plasticizer is glycerin. To give the film strength is added by amendment 2 ml of 3% solution of methylcellulose (3 g of methylcellulose + 100 ml water).

Film formed on the glass substrate (in the Petri plate) for 20-24 hours at 20-25°C. After drying the film it is separated from the substrate. The film thickness was measured using a micrometer ELECTRO MS DIGITAL MICROMETER, she was 0,074 mm

Biodegradable film obtained from pectin, water, chitosan, odnomomentnoe hydrochloric acid and plasticizer, characterized in that it contains as a plasticizer glycerin, as well as the amendment - a three percent solution of methyl cellulose in the following ratio, wt.%:

pectin 35-37
chitosan 35-37
water 7-8
odnomomentna hydrochloric acid 7-8
glycerin 5-6
a three percent solution of methyl cellulose rest

 

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