METHOD OF PRODUCING BIOPLASTIC GRANULES FROM OLIVE PIT WASTE (PRINA)

Abstract

A method for producing bioplastic granules includes the steps of subjecting an olive pit waste (prina) from olive oil factories to two different chemical shredding processes, extracting a necessary material for a bioplastic production from a shredded olive pit waste and adding natural polymerizer form holders into the necessary material.

Claims

1. A method for producing bioplastic granules, comprising the process steps of: mixing a dry olive pit waste (prina) with a NaOH solution in a reactor to obtain a first mixture, cooling the first mixture to obtain a cooled mixture, obtaining a solid cellulose by separating the cooled mixture by a filtering method, wherein a hemicellulose structure and a lignin structure are available in a dissolved state in the NaOH solution, the hemicellulose structure and the lignin structure are obtained from olive pits and are available in the cooled mixture, washing the solid cellulose with distilled water, mixing the solid cellulose with H.sub.2SO.sub.4 in the reactor to obtain a second mixture, cooling the second mixture, separating a cellulosic part and a shredded, dissolved cellulose part from each other in the second mixture by using a filtering paper after the cooling to obtain a separated liquid component, wherein the cellulosic part is a pellet part in the second mixture and the shredded, dissolved cellulose part is polymerized, adding glycerin or sorbitol and an antimicrobial agent (oleuropein) to the separated liquid component and placing the separated liquid component in a heater, subjecting the shredded, dissolved cellulose part in the separated liquid component to a polymerization reaction in the heater and obtaining a pulp structure, leaving the pulp structure to cooling at room temperature to obtain a cooled pulp structure, drying the cooled pulp structure.

2. The method according to claim 1, further comprising the process steps of: mixing 4 kg of the dry prina with 0.9 M 16 L of the NaOH solution to obtain the first mixture and transferring the first mixture to the reactor, and increasing a temperature gradually to 150° C., stirring the first mixture by fixing a pressure to 9.5 bars, cooling the first mixture contained in the reactor to obtain a cooled mixture, obtaining the solid cellulose by separating the cooled mixture by a filtering method, wherein the hemicellulose structure and the lignin structure available are in the dissolved state in the NaOH solution, and the hemicellulose structure and the lignin structure are obtained from the olive pits and are available in the cooled mixture, washing the solid cellulose in part with the distilled water, combining the solid cellulose and treating the solid cellulose with 0.52 M 8 L H.sub.2SO.sub.4 with a gradual heating at 150° C. at 10.5 bars in the reactor to obtain the second mixture, cooling the second mixture, separating the cellulosic part and the shredded, dissolved cellulose part from each other in the second mixture by using the filtering paper after the cooling to obtain the separated liquid component, wherein the cellulosic part is the pellet part in the second mixture and the shredded, dissolved cellulose part is polymerized, transferring the separated liquid component to glass beakers with a volume of 2 L, adding 4 ml of the glycerin or 6.5 ml of the sorbitol and the antimicrobial agent (oleuropein) to each liquid component of 2 L and placing the each liquid component in the heater, setting the heater to 300° C. and a mixing speed of 600 Rpm and obtaining the pulp structure as a result of the polymerization reaction of the shredded, dissolved cellulose part after mixing for 2 hours, leaving the pulp structure to cool at the room temperature to obtain the cooled pulp structure, drying the cooled pulp structure in the oven at 65° C. for 24 hours.

3. The method according to claim 1, wherein the oleuropein added into the separated liquid component in polymerization step is obtained by the process steps of: transferring a solution of 50 ml of ethanol-water mixture prepared in 70% ratio to a beaker in a solvent part of a randall system, transferring 10 g of a ground olive leaf or an olive pit powder into a cartridge, operating the randall system in a temperature range of 75 to 100° C. dissolving of folic acid derivatives in ethanol after an extraction, carrying out a distillation to decompose the ethanol and the folic acid derivatives.

4. The method according to claim 1, wherein dried biopolymers are grinded to have a size of 5 microns.

5. The method according to claim 1, wherein biopolymers obtained are used in a plastic sector as a raw material.

6. The method according to claim 2, wherein the oleuropein added into the separated liquid component in polymerization step is obtained by the process steps of: transferring a solution of 50 ml of ethanol-water mixture prepared in 70% ratio to a beaker in a solvent part of a randall system, transferring 10 g of a ground olive leaf or an olive pit powder into a cartridge, operating the randall system in a temperature range of 75 to 100° C. dissolving of folic acid derivatives in ethanol after an extraction, carrying out a distillation to decompose the ethanol and the folic acid derivatives.

7. The method according to claim 2, wherein dried biopolymers are grinded to have a size of 5 microns.

8. The method according to claim 3, wherein dried biopolymers are grinded to have a size of 5 microns.

9. The method according to claim 2, wherein biopolymers obtained are used in a plastic sector as a raw material.

10. The method according to claim 3, wherein biopolymers obtained are used in a plastic sector as a raw material.

11. The method according to claim 4, wherein biopolymers obtained are used in a plastic sector as a raw material.

Description

DETAILED DESCRIPTION OF THE EMBODIMENTS

[0016] The invention is a method for producing bioplastic granules comprising the steps of; [0017] mixing the dry prina obtained from the olive oil factory with NaOH solution in the reactor, [0018] cooling the mixture contained in the reactor, [0019] obtaining solid cellulose by separating, by means of a filtering method, the hemicellulose and lignin structure available in a dissolved state in the NaOH solution that are obtained from olive pits and are available in the cooled mixture, [0020] washing the resulting solid cellulose with distilled water, [0021] mixing cellulose with H.sub.2SO.sub.4 and mixing it in the reactor, [0022] cooling the mixture, [0023] separating the cellulosic part, which is the pellet part in the mixture, and the shredded, dissolved cellulose part, which can be polymerized, from each other, by using filtering paper after the cooling process, [0024] transferring the separated liquid component to glass beakers, adding glycerin or sorbitol and antimicrobial agent (oleuropein) and placing them in the heater, [0025] subjecting the cellulose to polymerization reaction leaving the pulp structure obtained to cooling, [0026] drying the product in an oven after cooling of said product that has been left to cool at room temperature.

[0027] The final end product obtained resists temperatures up to 140° C.

[0028] The process steps in the developed method are described in detail below.

[0029] Raw Material: Olive Pit Waste (Prina):

[0030] As the beginning of the method, 4 kg of dry prina from the olive oil factories is weighed on the scales. Prina, which is called olive pit waste, is the most important raw material source for the invention. Obtaining olive pits from different regions and different districts is important for the yield of the product in terms of cellulosic structure and antioxidant substance in the waste.

[0031] Treating Dry Prina (Olive Pit Waste) with Sodium Hydroxide:

[0032] The weighed dry prina is mixed with 0.9 M 16L NaOH solution and then the next step of processing with the reactor is carried out.

[0033] Obtaining Cellulose in a Reactor Where the Temperature and Pressure are Gradually Observed: 4 kg of prina and 0.9 M 16 L NaOH solution is transferred to the reactor. The temperature in the reactor is gradually increased to 150° C. Pressure increase is observed with the increase in temperature. The pressure is raised to 9.5 bars and is fixed at 9.5 bars. During the entire process, the mixer of the reactor is operated. The reactor is operated at 150° C. and 9.5 bar pressure and cooling is performed after separation. The hemicellulose and lignin structure, that is obtained from olive pits, and that dissolves in NaOH solution is separated from the cellulose in solid form by the filtration method. The reason for this is that, the polymerization degree of hemicellulose is lower than that of cellulose. The solid cellulose portion is washed with distilled water after filtration.

[0034] Providing Degradation of the Obtained Cellulose in the Reactor:

[0035] The resulting solid cellulose part is combined and treated with 0.52 M 8 L H.sub.2SO.sub.4 and processed by gradual heating in the reactor at 150° C., at 10.5 bars and the second separation process is performed. During the entire process, the mixer of the reactor is operated. The structure obtained after the second cooling process applied in the reactor, is separated by the effect of gravity in the filtration system, separation is ensured by paying attention to the conditions of filter paper such as tearing and passing solid particles (filtering).

[0036] Polymerization Reaction of the Cellulose, which is Degraded in the Reactor:

[0037] The liquid component obtained from these processes is transferred to glass beakers in volumes of 2 L. 4 ml of glycerin or 6.5 ml of sorbitol and antimicrobial agent (oleuropein) are added to each 2 L liquid component and the component is placed in the heater.

[0038] Heating:

[0039] In order for the polymerization reaction to occur, 2 ml of cellulosic material, 4 ml of glycerin or 6.5 ml of sorbitol and oleuropein are added into the heater. The heater is set at 300° C. and 600 Rpm mixing speed and stirred for 2 hours. After 2 hours of mixing, a pulp structure is obtained and this structure is left to cool.

[0040] Obtaining Antimicrobial Agent from Olive Pit and Leaf:

[0041] During the heating phase, Oleuropein can be obtained as a whole from the olive itself, the pulp (pomace), the oil and the waste (alperujo) produced in the olive oil production systems with two decanters. Phenolic compounds in olive vary according to the method of agricultural cultivation. In addition, olive leaves prevent hypertension and have hypoglycemic, antiseptic and diuretic properties. The most important compound in olive leaf having these properties is oleuropein. There are very few or underdeveloped methods for extracting biophenols from olive leaves rich in oleuropein. The ethanol/water mixture is used as solvent in the method of randall extraction. Solution of 50 ml of ethanol-water mixture prepared in 70% ratio is transferred to the beaker in the solvent part in the randall system. 10 g of ground olive leaf or olive pit powder is transferred into the cartridge. Afterwards, the randall system is operated in the temperature range of 75-100° C. The extraction process is finished and the folic acid derivatives in the sample are available such that they are dissolved in ethanol. Distillation is then carried out to decompose ethanol and folic acid derivatives. The decomposed oleuropein is added to the heater part during the plasticizing step. All of the ingredients are mixed and left to cool.

[0042] Drying the Product:

[0043] The product, which is left to cool under room temperatures for 2 hours, is left to dry in the oven at 65° C. for 24 hours.

[0044] Grinding:

[0045] The dried biopolymers are placed in the grinder for grinding to be at least 50 microns in size and the particulate structure obtained after grinding is subjected to the screening process. The biopolymers which become particles by sieving are separated, according to their micron levels.

[0046] By the Method Developed: [0047] not only plastic wastes are eliminated, but also environmentally friendly bioplastic granules are produced that utilize olive pit waste and prevent food waste and increase the shelf life of foods, [0048] the bioplastics that are developed begin to disappear in nature within 1 year, [0049] bioplastic cost is reduced by 60%, [0050] with the invention that is antimicrobial, the problem of food waste [0051] use of food preservatives that have negative effect on human health have been reduced by increasing the shelf life of foods, [0052] the bioplastics obtained can provide the desired properties for many products in the plastic industry and can be used in many sectors by means of their resistance to high temperature.