RU2593479C1 - Method of producing pectin - Google Patents

Abstract

FIELD: food industry.

SUBSTANCE: invention relates to food industry. Pectin production method envisages washing before hydrolysis-extraction of milled pectin-containing raw material with drinking water for 0.5-1.5 hour with simultaneous mixing at 10-30 rpm and t = 40-60 °C, separation of the obtained mixture into solid and liquid phases, mixing the solid phase with purified water in the ratio of 1:10-1:40. Herewith the drinking water is preliminarily purified on a two-stage reverse osmosis plant. Mixture obtained after washing is heated up to 50-80°C with simultaneous stirring and circulation, hydrolysis-extraction is performed by cavitation treatment in a rotary-oscillatory apparatus with further separation of pulp into solid and liquid phases in a vacuum drum filter. Obtained liquid phase is centrifuged with the relative centrifugal force of F_R = 2,000-5,000 g followed by microfiltration at P = 0.1-0.3 MPa and V = 0.06-0.16 l/sec, ultrafiltration at P = 0.2-0.6 MPa and V = 0.15-0.30 l/sec, diafiltration at P = 0.2-0.6 MPa and V = 0.1-0.27 l/sec till pectin substances concentration reaches 1-2 %. Herewith ultrafiltration and diafiltration are carried out on tangential filters with ceramic membranes. Then it is thickened in a vacuum-evaporator till dry substances content reaches 3-8 % and spray-dried at the air temperature of 150-200 °C.

EFFECT: output of the pectin is 70-84 % of theoretically possible one.

1 cl, 4 tbl, 3 ex

Description

The invention relates to a technology for the isolation of pectin from plant materials and can be used in the food industry.

A known method of producing pectin from plant materials, including hydrolysis-extraction in an electromagnetic field, separation of solid and liquid phases, concentration, precipitation and drying of pectin, while hydrolysis-extraction is carried out with an aqueous solution of a mixture of citric and succinic acids, taken in a ratio of 3: 2, at a temperature of 80-90 ° C and pH 2 in an electromagnetic field with a frequency of 25-29 Hz for 55-90 minutes, concentration is carried out to a pectin content of 5%, followed by coagulation with 96% ethyl alcohol for 10 minutes, and dryingsuschestvlyayut infrared dryer under vacuum at a pressure of 0.08 ± 0.02 MPa and a temperature of 35-40 ° C until the desired product moisture content is not more than 7% (Patent RF №2495051, publ. 10.10.2013 g).

A known method of producing pectin, including the operation of swelling of plant materials, hydrolysis and extraction using polyharmonic vibration with a frequency of 15-50 Hz, and the processes of swelling and hydrolysis are carried out in one stage with a solution of hydrochloric acid, followed by separation of the solid and liquid phases and the return of the latter for repeated processes of swelling and hydrolysis of plant materials, and the separated solid phase is diluted with water and used for extraction of pectin substances under vibration exposure, then the resulting extract is concentrated and purified on an ultrafiltration unit to obtain pectin concentrate, which is dried on a vacuum dryer (RF Patent No. 2282636, publ. 08/27/2006).

A known method of producing pectin, which consists in the fact that pre-crushed plant materials are treated with a solution of chloroform and ethanol, prepared in a ratio of 1: 3, taken respectively in a ratio of 1: 6, followed by extraction in a water bath at a temperature of 75-80 ° C for 30-40 minutes, followed by filtering the plant material to separate the first extract, the filtered plant material is poured with distilled water at a temperature of 60-70 ° C, respectively, in a ratio of 1:18 and extracted into water drop bath at a temperature of 90-95 ° C for one hour, followed by filtering the plant material to separate the second extract, the filtered plant material is poured with 0.3-0.5% solution of oxalic acid ammonium, respectively, in a ratio of 1:15 and extracted in a water bath at a temperature of 75-80 ° C for 30-40 minutes, followed by filtering the plant material to separate the third extract, the filtered plant material is poured with 0.4-0.5% hydrochloric acid solution and heated at a temperature of 75-80 ° C for one hour and followed by filtering the plant material to separate the fourth extract, which is mixed with the obtained first, second and third extracts, the resulting solution is neutralized with ammonium hydroxide to pH 7, precipitated with 96% ethanol, respectively, in a ratio of 1: 3 at room temperature, the resulting precipitate is squeezed out and dried at a temperature of 4-6 ° C. As plant material, dried sunflower baskets are used. (RF patent No. 2322456, publ. 04/20/2008).

A known method of producing pectin, comprising washing the plant material with water, two-stage acid hydrolysis of the washed material, filtering the obtained hydrolyzate, precipitating pectin from it with alcohol and drying the finished product, using pumpkin pulp as the plant raw material, hydrolysis is carried out with the pulp and paper mixture 1:10 -30, the pH of the mixture is 0.8-1.1 and the process temperature is 65-70 ° C, while the duration of the first stage of hydrolysis is 1.5-2.0 hours, the second 0.5-1.0 hours (RF Patent No. 2055484, published on March 10, 1996).

Known cold technology of pectin from pectin-containing raw materials, including grinding, hydrolysis, extraction in a rotary-cavitation apparatus, microfiltration at P = 0.2 MPa and V = 0.5 m / s with separation of the solid part of the pulp containing pectin, humidity 30-45%, ultrafiltration at P = 0.18 MPa and V = 0.1 m / s with the release of liquid pectin containing 3.0-3.7% solids, drying (http: //www.sergey-osetrov .narod.ru / Projects / Vodka / Pectin / CTP.htm).

A known method of producing pectin, comprising washing the plant material with water, two-stage acid hydrolysis of the washed material, filtering the obtained hydrolyzate, precipitating pectin from it with alcohol and drying the finished product, using pumpkin pulp as the plant raw material, hydrolysis is carried out with the pulp and paper mixture 1:10 -30, the pH of the mixture is 0.8-1.1 and the process temperature is 65-70 ° C, while the duration of the first stage of hydrolysis is 1.5-2.0 hours, the second 0.5-1.0 hours (RF Patent No. 2055484, published on March 10, 1996).

There is a method of producing pectin and dietary fiber from pumpkin pulp, characterized in that when removing pectin from pumpkin pulp, dietary fiber is simultaneously obtained, for which the juice obtained after extraction of pulp is washed with water, pressed and sent to hydrolysis-extraction with a water module of mixture 1: (4 -5), a temperature of 60-65 ° C and a process duration of 60 min, anolyte with a pH20 of 4.0-4.5 is used as an extractant, after separation of the hydrolysis mass by pressing on a pulp and a hydrolyzate, the pulp is extracted with catholyte with a pH20 of 7 5-8.0 at a 1: 3 mixture hydromodule, at a temperature of 60 ° C for 30 minutes, then the extracted pulp is extracted from the extract by pressing, the pulp particles are crushed, dried to obtain dietary fiber, the extract is combined with the hydrolyzate, and after filtration the mixture is sent to precipitation of pectin with alcohol and its drying, moreover, anolyte and catholyte are obtained by processing a solution of sodium chloride in a diaphragm electrolyzer (RF Patent No. 2422044, publ. 06/27/2011).

There is a method of complex processing of pumpkin, involving its preparation, cutting, removing seeds, followed by oil extraction and blanching of the pulp, while the blanched pulp is pressed to produce juice and squeezed, the juice is fermented and distilled to produce bioethanol, and the squeezed extract is extracted in rotary cavitation extractor at a temperature of 75-80 ° C and a cavitation index of 0.7-0.9, followed by phase separation, dried meal to obtain dietary fiber, clean the extract by sequential decantation, microfilter phase, ultrafiltration and diafiltration, concentrate it under vacuum and dried in a fluidized bed to obtain pectin (RF Patent No. 2476090, publ. 02.27.2013).

The main disadvantages of the known technologies include the imperfect stage of the processing of pectin-containing raw materials - hydrolysis and extraction of pectin substances with their considerable duration and high concentrations of mineral acids, which leads to the loss of native properties of pectin biopolymers, in particular, to a decrease in gelling and complexing ability.

For the prototype, a method for producing pectin was selected, including hydrolysis extraction of pectin-containing raw materials by cavitation treatment in a hydroacoustic extractor-disintegrator, separation of the obtained pulp into liquid and solid phases in the field of centrifugal forces and concentration of the liquid phase by ultrafiltration, characterized in that the hydrolysis-extraction of pectin-containing raw materials by cavitation treatment in a hydroacoustic extractor-disintegrator is carried out at a cavitation index K of 0.8-1.9, the separation of the obtained pulp into the liquid and solid phases in the field of centrifugal forces are carried out with a separation factor F _R = 90-100, and after separation, the resulting liquid phase with a suspension of 0.5-0.6% by weight is subjected to additional microfiltration using membranes with pore size (1-10) · 10 ^-6 m to a suspension content of not more than 0.1% of its mass, and concentration by ultrafiltration is carried out using ultrafiltration membranes on a solid substrate and a pore diameter of (1-10) · 10 ^-9 m at the flow rate of the liquid phase of 0.1-2.0 m / s and a pressure of 0.5-3.1 kg / cm ² to content p ectin substances in the resulting concentrate 3.5-4.2%, while after concentration by ultrafiltration, it is further thickened in a vertical two-case direct-flow circulating-film type vacuum evaporator with a vacuum in the condenser 0.09-0.093 MPa, after which the resulting concentrate with a content of 8-14% pectin substances are dried at a temperature of 75-92 ° C. As pectin-containing raw materials use any pectin-containing raw materials of plant origin. Pectin-containing raw materials are used in dry and / or fresh and / or freshly pressed form. Before hydrolysis-extraction, the pectin-containing raw materials are further crushed. To separate the resulting pulp into liquid and solid phases in the field of action of centrifugal forces with a separation factor F _R 90-100, a separation centrifuge is used. As a separation centrifuge, batch or continuous centrifuges are used. Batch centrifuges use semi-automatic or automatic. As separation centrifuges, filter or precipitation centrifuges are used. Microfiltration is carried out mainly on a filter press. When carrying out the ultrafiltration process, a polycarbonate or dacron base is used as a solid substrate of the ultrafiltration membrane. Drying at a temperature of 75-92 ° C is carried out on a roller unit, and / or a pseudo-boiling layer, and / or on pallets, or by spraying.

The task is to increase the yield of pectin from pectin-containing raw materials of plant origin without the use of destructive technologies.

The technical result is the production of pectin from plant materials with a yield of 70-84% of theoretically possible.

The technical result is achieved by a method for producing pectin, including grinding pectin-containing raw materials, hydrolysis extraction by cavitation treatment, separation of the obtained pulp into liquid and solid phases, microfiltration, ultrafiltration, thickening in a vacuum evaporator and drying, while crushed pectin-containing powder is also added before hydrolysis-extraction the raw materials are washed with drinking water for 0.5-1.5 hours while stirring 10-30 rpm and t = 40-60 ° C, the mixture is separated into solid and liquid phases, mix solid phase with purified drinking water in a ratio of 1: 10-1: 40, with simultaneous stirring and circulation are heated to 50-80 ° C, hydrolysis extraction is carried out by cavitation treatment in a rotary pulsation apparatus, followed by separation of the pulp into solid and liquid phase in a vacuum drum filter, centrifuged the liquid phase with a separation factor F _R = 2000-5000 g, microfiltration is carried out at P = 0.1-0.3 MPa and V = 0.06-0.16 l / s, ultrafiltration at P = 0.2-0.6 MPa and V = 0.15-0.30 l / s, diafiltration at P = 0.2-0.6 MPa and V = 0.1-0.27 l / s to pectin concentrations ETS 1-2%, is concentrated to a solids content of 3-8%, dried on a spray dryer at an air temperature of 150-200 ° C.

Salient features that affect the achievement of the claimed technical result are:

- additional washing before hydrolysis-extraction of crushed pectin-containing raw materials with drinking water for 0.5-1.5 hours while stirring 10-30 rpm and t = 40-60 ° C;

- separation of the resulting mixture into solid and liquid phases;

- mixing the solid phase with purified water in a ratio of 1: 10-1: 40, while drinking water is pre-purified at the installation of two-stage reverse osmosis;

- heating the resulting mixture while stirring and circulating to 50-80 ° C;

- carrying out at the achieved temperature hydrolysis extraction by cavitation treatment in a rotary pulsation apparatus, followed by separation of the pulp into solid and liquid phases in a vacuum drum filter;

- centrifugation of the liquid phase with a separation factor F _R = 2000-5000 g;

- microfiltration at P = 0.1-0.3 MPa and V = 0.06-0.16 l / s;

- ultrafiltration at P = 0.2-0.6 MPa and V = 0.15-0.30 l / s;

- diafiltration at P = 0.2-0.6 MPa and V = 0.1-0.27 l / s to a concentration of pectin substances of 1-2%;

- ultrafiltration and diafiltration is carried out on tangential filters with ceramic membranes;

- thickening to a solids content of 3-8%;

- drying in a spray dryer at an air temperature of 150-200 ° C.

The claimed sequence of actions and technological parameters are determined experimentally. Their change in the direction of increase or decrease does not allow to obtain the technical result declared by the applicants.

The step of washing the pulp with drinking water ensures the removal of low molecular weight ballast substances, such as polysaccharides, carotenoids, etc.

Separation into liquid and solid phases allows you to get rid of wash water, which, in turn, contains ballast substances.

The passage of drinking water through a two-stage reverse osmosis purifies water from harmful impurities that affect the quality of the resulting finished product - pectin.

The heating process accelerates the extraction process.

The centrifugation process ensures the removal of suspended particles from the pectin extract and its clarification.

The subsequent microfiltration, ultrafiltration and diafiltration provides a deeper purification of the pectin extract at each subsequent filtration stage: at the microfiltration stage from suspended microparticles remaining after centrifugation, at the ultrafiltration stage - from low molecular weight pectin fractions, at the diafiltration stage - from mineral impurities.

A method of producing pectin from plant material is as follows.

The crushed pectin-containing raw materials are washed with drinking water for 0.5-1.5 hours before hydrolysis-extraction while stirring at 10-30 rpm and t = 40-60 ° C in a container with a stirrer and a jacket. Then the wash water is drained, and the remaining solid phase is filled with purified water in a ratio of 1: 10-1: 40. Purified water is obtained by first passing drinking water through a two-stage reverse osmosis unit. The resulting mixture with simultaneous stirring and circulation is heated to 50-80 ° C, hydrolysis extraction is carried out by cavitation treatment in a rotary pulsation apparatus, followed by separation of the pulp into solid and liquid phases in a vacuum drum filter, the liquid phase is centrifuged with a separation factor F _R = 2000-5000 g. Microfiltration is carried out at P = 0.1-0.3 MPa and V = 0.06-0.16 l / s. Ultrafiltration and diafiltration are carried out on tangential filters with ceramic membranes, respectively, at P = 0.2-0.6 MPa, V = 0.15-0.30 l / s and P = 0.2-0.6 MPa, V = 0 , 1-0.27 l / s. Diafiltration is carried out to a concentration of pectin substances of 1-2%. It is concentrated in a vacuum evaporator to a solids content of 3-8%. Dried on a spray dryer at an air temperature of 150-200 ° C.

Organoleptic characteristics of the obtained pectin are presented in table 1.

Physico-chemical parameters of the obtained pectin are presented in table 2.

The chemical safety of pectin was carried out in accordance with the requirements of the “Unified Sanitary and Epidemiological and Hygienic Requirements for Goods Subject to Sanitary and Epidemiological Surveillance”, approved by Decision of the Customs Union Commission No. 299 of May 28, 2010 and amendments No. 456 of November 18, 2010 of the Technical Regulations of the Customs Union TP TC 029/2012. The data are shown in table 3.

Microbiological safety was carried out in accordance with the requirements for goods subject to sanitary and epidemiological surveillance approved by Decision of the Customs Union Commission No. 290 of May 28, 2010 and amendments No. 456 of November 18, 2010, SanPiN 2.3.2.1078-01. The data are shown in table 4.

Case Studies

Example 1

40 kg of apple raw materials were crushed and washed with drinking water for 0.5 h while stirring at 10 rpm and t = 40 ° C. Then the wash water was drained. Purified drinking water was preliminarily obtained by passing drinking water through a two-stage reverse osmosis unit EKO-80V. Then the washed solid phase was mixed with purified drinking water in a ratio of 1:10 in a container with a stirrer and a jacket. The resulting mixture with simultaneous stirring and circulation was heated to 50 ° C and, at a given temperature, hydrolysis extraction was carried out by cavitation treatment in a rotary pulsation apparatus, followed by separation of the pulp into solid and liquid phases in a G-2.5 vacuum drum filter. The liquid phase was centrifuged in an OGSh-202K-03 centrifuge with a separation factor F _R = 2000 g. Microfiltration was carried out on a V9-VFS filter press at P = 0.1 MPa and V = 0.06 l / s. Diafiltration and ultrafiltration were carried out on tangential filters with ceramic membranes CFKN-20/30, respectively, at P = 0.2 MPa, V = 0.15 l / s and P = 0.2 MPa, V = 0.1 l / s. Diafiltration was carried out to a concentration of pectin substances of 1%. The extract was concentrated in an ELT / S-100 vacuum evaporator to a solids content of 3%. It was dried on a BETA 1C / 25 / UDF spray dryer at an air temperature of 150 ° C. Received pectin with a yield of 70% of theoretically possible.

Example 2

40 kg of pumpkin raw materials were crushed and washed with drinking water for 1.0 h while stirring at 20 rpm and t = 50 ° C. Then the wash water was drained. Purified drinking water was preliminarily obtained by passing drinking water through a two-stage reverse osmosis unit EKO-80V. Then the washed solid phase was mixed with purified drinking water in a ratio of 1:25 in a container with a stirrer and a jacket. The resulting mixture with simultaneous stirring and circulation was heated to 65 ° C and, at a given temperature, hydrolysis extraction was carried out by cavitation treatment in a rotary pulsation apparatus, followed by separation of the pulp into solid and liquid phases in a G-2.5 vacuum drum filter. The liquid phase was centrifuged in an OGSh-202K-03 centrifuge with a separation factor F _R = 3500 g. Microfiltration was carried out on a V9-VFS filter press at P = 0.2 MPa and V = 0.09 l / s. Diafiltration and ultrafiltration were carried out on tangential filters with ceramic membranes CFKN-20/30, respectively, at P = 0.4 MPa, V = 0.2 l / s and P = 0.4 MPa, V = 0.2 l / s. Diafiltration was carried out to a concentration of pectin substances of 1.5%. The extract was concentrated in an ELT / S-100 vacuum evaporator to a solids content of 4%. It was dried on a BETA 1C / 25 / UDF spray dryer at an air temperature of 170 ° C. Received pectin with a yield of 78% of theoretically possible.

Example 3

40 kg of beetroot was ground and washed with drinking water for 1.5 hours while stirring at 30 rpm and t = 60 ° C. Then the wash water was drained. Purified drinking water was preliminarily obtained by passing drinking water through a two-stage reverse osmosis unit EKO-80V. Then the washed solid phase was mixed with purified drinking water in a ratio of 1:40 in a container with a stirrer and a jacket. The resulting mixture with simultaneous stirring and circulation was heated to 80 ° C and, at a given temperature, hydrolysis extraction was carried out by cavitation treatment in a rotary pulsation apparatus, followed by separation of the pulp into solid and liquid phases in a G-2.5 vacuum drum filter. The liquid phase was centrifuged in an OGSh-202K-03 centrifuge with a separation factor of FR = 5000 g. Microfiltration was carried out on a V9-VFS filter press at P = 0.3 MPa and V = 0.16 l / s. Diafiltration and ultrafiltration were carried out on tangential filters with ceramic membranes CFKN-20/30, respectively, at P = 0.6 MPa, V = 0.3 l / s and P = 0.6 MPa, V = 0.27 l / s. Diafiltration was carried out to a concentration of pectin substances of 2%. The extract was concentrated in an ELT / S-100 vacuum evaporator to a solids content of 8%. It was dried on a BETA 1C / 25 / UDF spray dryer at an air temperature of 200 ° C. Received pectin with a yield of 84% of theoretically possible.

Thus, the claimed method for producing pectin from pumpkin pulp provides the possibility of producing pectin with a yield of 70-84% of theoretically possible.

Claims (1)

A method of producing pectin, including grinding pectin-containing raw materials, hydrolysis extraction by cavitation treatment, separation of the obtained pulp into liquid and solid phases, microfiltration, ultrafiltration, thickening in a vacuum evaporation apparatus and drying, characterized in that, in addition to hydrolysis-extraction, crushed pectin-containing raw materials washed with drinking water for 0.5-1.5 hours while stirring 10-30 rpm and t = 40-60 ° C, divide the mixture into solid and liquid phases, mix the solid phase with a cleaner water in a ratio of 1: 10-1: 40, while drinking water is preliminarily purified using a two-stage reverse osmosis unit, the resulting mixture is heated to 50-80 ° С while stirring and circulating, hydrolysis extraction is carried out by cavitation treatment in a rotary pulsation apparatus, followed by separation of the pulp into solid and liquid phases in a vacuum drum filter, centrifuged the liquid phase with a separation factor F _R = 2000-5000 g, microfiltration is carried out at P = 0.1-0.3 MPa and V = 0.06- 0.16 l / s, ultrafiltration at P = 0.2-0.6 MPa and V = 0 , 15-0.30 l / s, diafiltration at P = 0.2-0.6 MPa and V = 0.1-0.27 l / s to a concentration of pectin substances of 1-2%, while ultrafiltration and diafiltration is carried out on tangential filters with ceramic membranes, thicken to a dry matter content of 3-8%, dried on a spray dryer at an air temperature of 150-200 ° C.