POLYMER BIOCOMPOSITES WITH IMPROVED ANTIMICROBIAL ACTIVITY BY BEE BREAD AND THEIR PRODUCTION METHOD

Abstract

Disclosed is a biocomposite product with high microbial activity obtained by using bee bread, the method of obtaining this product and using of this biocomposite material for the coating of products like artificial materials, packaging, etc. to be used in areas requiring hygiene or their use as an intermediate raw material.

Claims

1. A method of obtaining biocomposite nanofibers comprising: obtaining an extract by extracting bee bread, lyophilization (freeze-drying) of the extract, turning a thermoplastic polymer into a polymer solution with a magnetic stirrer, adding lyophilized bee bread extract into the polymer solution and obtaining a homogeneous solution with magnetic stirrer, and turning the solution consisting of polymer and bee bread extract into nanofiber (biocomposite) by electrospinning method.

2. The method of obtaining biocomposite nanofiber of claim 1, wherein a mixture of 20-50% bee bread and methanol: water (80:20) is used in the extraction process of bee bread.

3. The method of obtaining biocomposite nanofibers of claim 1, wherein the extraction process of bee bread is carried out at 50° C. for 10 hours in a shaking water bath.

4. The method of obtaining biocomposite nanofibers of claim 1, wherein the bee bread remaining on the filter in the first extraction process, is extracted 2 more times for one hour to obtain a dense bee bread extract.

5. The method of obtaining biocomposite nanofibers of claim 1, wherein bee bread extract obtained at the extraction stage is freezed at −80° C. and then lyophilized by freeze drying in a lyophilizer.

6. The method of obtaining biocomposite nanofibers of claim 1, wherein the thermoplastic polymer is selected from a group consisting of polyurethane, polylactic acid, polyglycolic acid, poly (epsilon-caprolactone), and polyethylene.

7. The method of obtaining biocomposite nanofibers of claim 1, wherein the polymer solution is prepared in a homogeneous structure in the range of 6-15% by weight with magnetic stirrer for 24 hours at room temperature.

8. The method of obtaining biocomposite nanofibers of claim 1, wherein 5-50% by weight lyophilized bee bread extract is added into the total polymer solution.

9. The method of obtaining biocomposite nanofibers of claim 1, wherein polymer solution and lyophilized bee bread extract mixture is subjected to mixing process with magnetic stirrer for 1-2 hours at room temperature to provide a homogeneous structure.

10. The method of obtaining biocomposite nanofibers of claim 1, wherein the thermoplastic polymer solution fortified with bee bread extract prepared at room temperature is filled into a plastic syringe in the range of 10 ml-20 mL and turned into nanofibers by giving it to an electrospinning device through a stainless-steel needle.

11. The method of obtaining biocomposite nanofibers of claim 1, wherein electrospray solution feeding rate is between 1 ml/min-20 ml/min.

12. The method of obtaining biocomposite nanofibers of claim 1, wherein the distance between the tip of the needle and the collector surface is in the range of 5 cm-20 cm in electrospinning.

13. The method of obtaining biocomposite nanofibers of claim 1, wherein the nanofibers obtained in electrospinning are winded on a collector surface, which is covered with an aluminum film and in rotation.

14. Biocomposite nanofiber produced by the method of claim 1.

15. Use of biocomposite nanofiber according to claim 14 as the main or intermediate raw material in areas requiring hygiene such as medical materials, packaging, food coating production, and textile, automotive, furniture and chemistry fields.

16. Use of biocomposite nanofiber according to claim 14, as main or intermediate raw material in the field of health, especially artificial vessels, prostheses, tissue support materials, hemostatic materials, wound care products used in wound infections and open wounds that can be applied locally as well as systemically for stabilizing the immune system in immunosuppressive or transplant patients.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0040] The invention is a polymer biocomposite product with high microbial activity obtained using bee bread, the method of obtaining this product and its use for coating material or as an intermediate raw material for artificial materials, packaging, etc. to be used in areas requiring hygiene.

[0041] The basic steps of the proposed method are as follows: [0042] 1—obtaining an extract by extracting bee bread, [0043] 2—lyophilization of (freeze-drying) extract, [0044] 3—bringing the thermoplastic polymer (preferably polyurethane, polylactic acid, polyglycolic acid, poly(epsilon-caprolactone), polyethylene) into solution with magnetic stirrer, [0045] 4—adding the polymer solution into lyophilized bee bread extract and obtaining a homogeneous solution with magnetic stirrer, [0046] 5—converting the solution consisting of polymer and bee bread extract into nanofibers (biocomposite) by electrospinning method, [0047] 6—using of the obtained biocomposite material as a coating or intermediate raw material for artificial materials, packaging, and etc. products that wanted to gain hygienic properties.

[0048] In the extraction process to be carried out in the first step, 20-50% bee bread is left to extraction with methanol: water (80:20) at 50° C. for 10 hours in a shaking water bath. At the end of the period, it is filtered through Whatman 1 filter. The bee bread remaining on the filter is left to be extracted with the same amount of solvent (methanol: water) for 1 hour under similar conditions, then the extract is removed by filtering through the filter paper. In the last stage, bee bread is left for 1 more hour extraction under similar conditions. The extracts obtained at the end of the three stages are combined. Then the methanol is removed by keeping it in the rotary evaporator under vacuum.

[0049] In the lyophilization stage of the method, the remaining dense extract is frozen at −80° C. and then freeze-dried in a lyophilizer. Lyophilization process is carried out in 3 main stages; [0050] 1. Freezing the Product: The process of completely freezing the product after passing through the appropriate pre-preparation processes, turning it into crystal form. [0051] 2. Sublimation (Primary Drying): Creating the energy required for sublimation to take place in the frozen product and performing sublimation. The stage where the water content is 90-95% removed. [0052] 3. Desorption (Secondary Drying): The process of removing water that cannot be removed in primary drying and is bound to the substance.

[0053] In the third step, the polymer is brought into solution using magnetic stirrer to prepare the polymer. Thermoplastic polymer (preferably polyurethane, polylactic acid, polyglycolic acid, poly (epsilon-caprolactone), polyethylene) is preferred as the polymer here.

[0054] The reason why the mentioned thermoplastic polyurethane material preferred is to have the properties of softening when heated, hardening when cooled, and being easily processed in heat-treatment processes such as extrusion and injection.

[0055] Furthermore, it shows a good performance during processing with its unique molecular structure and it can have different chemical properties and strengths by regulating the chemical structures in its formulation. This structure makes it a good packaging material.

[0056] In the fourth step, lyophilized bee bread extract is added to the polymer solution and a homogeneous solution is obtained with magnetic stirrer.

[0057] In the fifth step, this homogeneous solution (polymer, bee bread extract, solvent used to form the polymer solution) is transformed into nanofibers (biocomposite) by electrospinning method.

[0058] The above thermoplastic polymer solutions can be selected from solvents such as dimethyl sulfoxide or dimethyl formamide, as well as solvents such as tetrahydrofuran, acetone, methyl ethyl ketone, chloromethane, dichloromethane can be used to form the polymer solution.

[0059] In the preferred embodiment of the invention, lyophilized bee bread extract was prepared into a total polymer solution up to 50% by weight, by the following method: In the first step, a homogeneous polymer solution (in the range of 6-15% by weight) is prepared with magnetic stirrer for 24 hours at room temperature. In the second stage, 5-50% by weight of lyophilized bee bread extract is added into the total polymer solution and mixing continues with magnetic stirrer at room temperature for 1-2 hours until a homogeneous structure is obtained.

[0060] Bee bread extract added thermoplastic polymer solutions prepared at room temperature, are filled into a plastic syringe in the range of 10 mL-20 mL and this syringe is attached to a stainless-steel needle as a nozzle. The polymer solution in the syringe is produced in the form of nanofibers by using an electrospinning device (Inovenso-Nanospinner24). Here, the emitter electrode of the high-voltage power supply, which will allow the polymer solution to be drawn into fibers, is charged by connecting it to a conductive jet. The other or grounding electrode of the high-voltage power supply is connected to the conductor collecting device to complete the cycle. To adjust the optimum voltage for each polymer solution, different voltages were applied to the polymer solutions obtained as nanofibers by electrospinning. The feeding rate was set as 1 mL/min-20 mL/min and the distance between the needle tip and the collector surface was set as 5 cm-20 cm. The samples (Nanofibers) are wrapped in a collector surface covered with an aluminum film and in rotation.

[0061] The recommended packaging material is the use of pollen, propolis, honey, brood homogenate, as well as biologically active products including vitamins, food coloring, mineral and medicinal substances in the form of wax. The product also allows for effective oral or sublingual use. The product can be used as food, packaging, medical products (all implant materials remaining in the body) by covering them with appropriate coating techniques. For example, it can be applied locally in artificial vessels, prostheses, tissue support materials, hemorrhage stopping materials, wound infections and wound care products, open wounds, as well as it is used systemically for balancing the immune system in immunosuppressive or transplant patients, textile, automotive, furniture, chemistry fields.