RU2414145C1 - Method of pectin production from black walnut coats - Google Patents

Abstract

FIELD: food industry.

SUBSTANCE: invention relates to food industry. The method envisages fruit coat drying and milling, removal of impurities and degreasing with acetone during 24 hours. Removal of polyphenols is performed with a 5% sodium chloride solution,duty of water being 1:10, at a 75-80°C temperature. Then one undertakes four- or five-time rinsing with potable water. Then one proceeds with hydrolytic extraction with a 0.3-0.5% solution of citric acid during 120 minutes at a temperature of 85-90°C, duty of water being 1:20. For pectin substances coagulation acetone is utilised. Then the coagulant is dried and milled to produce the target product.

EFFECT: invention enables processing previously unused secondary raw material resources of black walnut fruits and to ensure a high output of target product with required consumer properties.

1 ex

Description

The invention relates to a technology for the isolation of pectin from plant materials.

A known method of producing pectin from pre-dried fruit shells of the tung, providing for their grinding to a powder state, purification from impurities and metal ions with ethanol, repeated drying and grinding, hydrolysis-extraction, separation of the liquid phase upon completion of the hydrolysis-extraction process, precipitation of pectin from the extract with chloride aluminum, purification from aluminum impurities with ethanol, drying, grinding [Fishman G.M., Dzhabua T.V. Production of pectin from the fruit pulp of the tung. - Proceedings of the Georgian Research Institute of Food Industry, 1971, v.5, p.85-87].

The disadvantage of this method is the low purity of the obtained pectin due to the use of polyvalent metal salts for coagulation, as well as the high cost of ethanol for the purification of pectin coagulate.

A known method of producing pectin from fruit shells of tung, including drying and grinding the fruit shell, removing impurities, degreasing with acetone for one day, purification of polyphenols with 3% sodium chloride solution for half an hour at a temperature of 70-75 ° C, 2-3 multiple washing with water, hydrolysis-extraction with a 0.3-0.5% solution of oxalic acid at a hydraulic module of 1:17 and a process temperature of 80-85 ° C for 90 minutes, separation of the liquid phase after completion of the hydrolysis-extraction process, coagulation of the target product 96% e Anolyte, drying and grinding of the coagulate [Patent №2346465, A23L 1/0524, publ. 02/20/2009].

The disadvantage of this method is the inferiority of purification from polyphenols, as well as the high cost of ethanol for coagulation of pectin from the extract.

The present invention solves the problem of processing secondary raw materials for the production of black walnut kernels not previously used.

The technical result of the invention is to obtain dry pectin of standard quality from the fruit shells of black walnut.

The technical result is achieved in that in a method including drying and grinding the fruit coat, removing impurities, degreasing with acetone for one day, purification of polyphenols with sodium chloride solution for half an hour, repeated washing with water, hydrolysis-extraction, separation of the liquid phase after completion of the process hydrolysis-extraction, coagulation of the target product, drying and grinding of the coagulate, according to the invention, polyphenols are purified by a 5% solution of sodium chloride with a water module of 1:10 and t at a temperature of 75-80 ° C, followed by four to five times washing with drinking water, after which hydrolysis-extraction is carried out with a 0.3-0.5% solution of citric acid for 120 minutes at a temperature of 85-90 ° C and hydromodule 1: 20, and the coagulation of pectin substances is carried out with acetone.

A comparative analysis of the claimed solution with known methods for producing pectin from fruit shells of walnut crops allows us to conclude that the inventive method for producing pectin has a novelty criterion, since it allows to obtain pectin from the shells of black walnut fruit, previously not used.

The inventive method for producing pectin meets the criterion of inventive step, since it allows to obtain pectin of standard quality by using strict purification modes from polyphenols, salt and water soluble proteins and advanced parameters of the hydrolysis-extraction process, and the use of acetone as a coagulating agent eliminates the use of ethanol.

The claimed technical solution meets the criterion of industrial applicability, as it can be used at any pectin production enterprise.

In the inventive method, optimal parameters are proposed for purifying raw materials from polyphenols, the content of which is very high in it, as well as from salt and water soluble proteins. When passing into a solution, and then into a coagulate, polyphenols and proteins adversely affect the physicochemical properties of coagulated pectin and worsen its consumer qualities. Sodium chloride is used as a cleaning agent, as an effective and at the same time cheap and affordable agent, easy to transport, store and use. It is proposed to use a 5% solution of sodium chloride with a water module of 1:10, which guarantees the most profound purification of raw materials from undesirable components. The temperature of the process should be 75-80 ° C, in order to avoid degradation of pectin substances.

Following extraction, a four to five-fold washing of the feed with drinking water allows the maximum removal of excess sodium chloride, polyphenol and protein extract.

The above parameters for the purification of raw materials from polyphenols, salt-and water-soluble proteins are optimal and provide the deepest extraction.

The choice of the described set of parameters for the hydrolysis-extraction of pectin substances is explained by their greatest yield at the optimal cost of basic, auxiliary raw materials and time.

Citric acid, used as a hydrolyzing agent, provides the highest yield of pectin substances from this type of raw material, and a solution concentration of 0.3-05% is optimal for the process.

The optimal yield of pectin substances is detected with a water module of 1:20. With a hydraulic module of 1: 15-1: 17, a porridge-like mass is formed, there is no free movement in the phases, the transition of pectin substances is complicated and is not ensured at the proper level. If the hydromodule increases beyond the optimum, the concentration of the extracted pectin substances in the solution decreases, and although the increase in the pectin substances does not particularly affect the quality of the pectin substances, the acid consumption, the load of containers and equipment, and the energy consumption increase in parallel in the technological cycle.

The optimum temperature of the hydrolysis process is 85-90 ° C. With increasing temperature, the diffusion coefficient increases, since the viscosity of the extract decreases, however, an excessive increase in temperature causes degradation of pectin substances, as a result of which their physicochemical parameters deteriorate. At a temperature of 5-10 ° C below the optimal hydrolysis is slower, which significantly increases the duration of the cycle.

The duration of hydrolysis of 120 minutes is optimal with other accepted optimal process parameters. With a decrease in the duration of the cycle, the amount of extracted pectin substances directly correlates, however, an increase in the duration of the process does not significantly affect the yield of pectin substances, while the energy consumption and equipment load increase.

The use of acetone as a coagulating agent allows to achieve the proper purity of the pectin coagulate and to exclude the consumption of ethanol for its subsequent purification.

The method is implemented as follows. The separated fruit shell of black walnut is dried and crushed, then the impurities are removed, the raw materials are degreased with acetone for one day, and the polyphenols are purified with sodium chloride solution for half an hour. This is followed by repeated washing of the raw materials with water, hydrolysis-extraction, separation of the liquid phase after completion of the hydrolysis-extraction process, coagulation of the target product, drying and grinding of the coagulate.

An example implementation of the proposed method

The fruit shell separated during the processing of black walnut fruit is dried and crushed to a particle size of 1-3 mm, which is degreased with acetone for one day, then polyphenols are cleaned with a 5% sodium chloride solution for 30 minutes at a temperature of 75 ° C and hydromodule 1:10 followed by a fourfold washing of the raw materials with drinking water. Hydrolysis-extraction is carried out with a 0.5% solution of citric acid for 120 minutes at a temperature of 85 ° C and a water module of 1:20. At the end of the hydrolysis-extraction process, the liquid phase is separated and pectin is precipitated from it with acetone; the coagulate is dried and ground to a powder state. The yield of dry crushed pectin coagulate in this case is 21%.

A positive effect in the implementation of the developed method is to solve the problem of processing secondary raw materials for the production of black walnut fruit, not previously used; in increasing the yield of pectin substances from the fruit shells of black walnut as a result of their degreasing with acetone; in giving the target product consumer qualities by purifying raw materials from polyphenols and proteins; in the maximum yield of pectin substances as a result of selection of optimal parameters of the hydrolysis-extraction process, as well as in the use of acetone as a coagulating agent.

The specified positive effect is achieved only by combining the described process parameters, which allows to obtain the claimed technical result.

A production audit of the developed technology was carried out at UNIK “Technolog” (KubSAU) in 2008-2009. Development is recommended for implementation in production.

Claims (1)

A method of producing pectin from the fruit shells of black walnut, including drying and grinding the fruit shell, removing impurities, degreasing with acetone for one day, purification from polyphenols with sodium chloride solution for half an hour, washing with water repeatedly, hydrolysis-extraction, separation of the liquid phase after completion of the process hydrolysis-extraction, coagulation of the target product, drying and grinding of the coagulate, characterized in that the purification from polyphenols is carried out with a 5% solution of sodium chloride with a hydrogen mode f 1:10 and a temperature of 75-80 ° C followed by four to five times washing with drinking water, followed by hydrolysis-extraction with 0.3-0.5% citric acid solution for 120 min at a temperature of 85-90 ° C and a water ratio of 1:20, and coagulation of pectin substances is carried out with acetone.