SU1286621A1 - Method of producing enotannin from deoiled grist of grape seeds - Google Patents

Abstract

This invention relates to the food industry and relates to methods for producing enotannin. The aim of the invention is to increase the degree of purification and intensification of the process. In order to obtain highly purified zonotanin from grape seed meal, extraction is carried out with alcohol, the extract is concentrated to a density of 1.10-1.12 G / CM, the resulting extract is mixed with diethyl ether and kept for 10-12 minutes to form a precipitate and filtration is carried out; the precipitate of enotannin is dried in a stream of hot air with an air temperature of 40-48 С. 4 tab.

Description

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The invention relates to oil and fat industry, namely to methods for producing oil and enotannin from grape seeds.

The aim of the invention is to intensify the process and increase the purity of enotannin.

The method is carried out as follows.

Grape seeds are separated from the high-oh zipper by sieving, the separated seeds are dried at 90-95 ° C to a residual moisture content of 5-7%. The seeds are crushed, extracted with a hydrocarbon solvent. The extract is treated with activated charcoal, the purified extract is evaporated under vacuum. Hydrocarbon extract reused in the process.

Tannin is extracted from the meal with ethyl alcohol at normal temperature. Extraction is carried out until tannin extraction is terminated, as determined by reaction with vanillin. The enotannin alcohol extract is concentrated under vacuum until a density of 1.10-1.12 is reached, then blended with stirring diethyl ether. The mixture is held up to

25

In terms of its indicators, the radiated oil corresponds to the edible oil from sunflower.

After all the gasoline has evaporated, the enotannin alcohol is extracted. Extraction is carried out with 4 liters of alcohol. Enotannin alcohol extract is condensed in a vacuum apparatus at 45 ° C and a discharge of 650 mm Hg. to a density of 1.10 SRI 650 mm Hg to a density of 1.10 g / cm. The thickened extract is mixed in a 1: 2 ratio with diethyl ether, stirred for 5 minutes, and allowed to stand for 10 minutes until the formation of a pale brown precipitate and compaction. Then the enotunnin section is on the filter. The precipitate of enotannin is additionally washed with a fresh portion of diethyl ether in a ratio of 1:: 0.5. The precipitate of enotannin is dried in a drying oven in a stream of hot air with temperature. The output of enotannin from the weight of seeds of 7.6%, the content of enotannin in the powder is 82.3%,

Example 2. The extraction and squeezing of seeds of a grape variety, their cleaning, grinding and oil extraction with gasoline is carried out as in Example 1. The obtained extract sediment sediment. The precipitate of enotanni-ZO is removed by filtering with activated carbon (AG-3). The precipitate is washed with diethyl ether and dissolved in a flow of 3 g / dm with stirring for 15 minutes. The adsorbent is then separated from the extract by filtration. Gasoline is distilled to form an oil. As a result of the purification of gasoline extract with activated carbon, the light transmission coefficient increases by 43%, and the acidity decreases from 1.68 to 0.76 mg COL (55%). You run oil 15.4%. Gasoline, cleaned

nom air at 40-48 ° C. I P. p. And me R 1. Sweet grape marc varieties Rkatseteli are chopped, seeds are separated by sieving through sieves with a mesh diameter of 6-7 mm. The separated seeds are dried at a residual moisture content of 5%. Repeatly cleaned to remove unwanted at-40 from the coloring and phenolic substances of oQ-mixes. Dried and peeled seeds in the amount of 1 kg are crushed to 0.2-1.5 mm, placed in an extraction column. Grape oil is extracted by extraction with gasoline. An washer-45 was conducted on the extraction with gasoline in the amount of 3 dm. The obtained extract is treated with activated carbon 2 g / dm with stirring for 10 minutes.

activated carbon processing, used Repeatedly in the process cycle.

From the meal extracted enotannin 4 liters of ethyl alcohol. The alcohol extract is concentrated in a vacuum apparatus at a discharge of 650 mm Hg to a density of 1.12 g / cm. The adsorbent is separated from the extract-50 and the tract is displaced in a ratio of 1: 2.

that filtering.

Eluate at 85 ° C

heated in a water bath until the gasoline is completely removed.

O 5

0

five

In terms of its indicators, the radiated oil corresponds to the edible oil from sunflower.

After all the gasoline has evaporated, the enotannin is extracted with alcohol. Extraction is carried out with 4 liters of alcohol. Enotannin alcohol extract is thickened in a vacuum apparatus at 45 ° C and a discharge of 650 mm Hg. to a density of 1.10 SRI 650 mm Hg to a density of 1.10 g / cm. The thickened extract is mixed in a 1: 2 ratio with diethyl ether, stirred for 5 minutes, and allowed to stand for 10 minutes until the pale brown color has formed and settled. The enotannin is then separated on a filter. The precipitate of enotannin is additionally washed with a fresh portion of diethyl ether in a ratio of 1:: 0.5. The precipitate of enotannin is dried in a drying oven in a stream of hot air with temperature. The output of enotannin from the weight of seeds of 7.6%, the content of enotannin in the powder is 82.3%,

Example 2. The extraction of seeds from the squeeze of that grape variety, their purification, grinding and oil extraction with gasoline is carried out as in Example 1. The obtained extract is treated with activated carbon (AG-3)

3 g / dm with stirring for 15 minutes The adsorbent is then separated from the extract by filtration. Gasoline is distilled to form an oil. As a result of the purification of gasoline extract with activated carbon, the light transmission coefficient increases by 43%, and the acidity decreases from 1.68 to 0.76 mg COIL (55%). Oil yield 15.4%. Gasoline, cleaned

from dye and phenolic substances oQpa-

activated carbon processing, used Repeatedly in the process cycle.

From the meal extracted enotannin 4 liters of ethyl alcohol. The alcohol extract is concentrated in a vacuum apparatus at a discharge of 650 mm Hg to a density of 1.12 g / cm. Condensed exe with diethyl ether, mix for 5 minutes and hold for 20 minutes until the precipitate is formed and compacted. Then decant the liquid

As a result of processing the eluate, the activi-55 part, and the precipitate of enotannin is transferred

By the coal content, the light transmission coefficient of the oil is increased by 41%, and the acidity is reduced by 54%. Oil yield from grape seeds 15.6%, Ion filter, sucked off the liquid and washed with a fresh portion of diethyl ether in a ratio of 1: 0.5. After suction of the liquid, the sediment of enotannin

dried in an oven in a stream of hot air at. The pale brown powder contains 81.9% enotannin. The output of enotannin 7.5%.

Example 3. Selection of seeds from the squeeze of the Fetki grape variety, their purification, drying and oil extraction is carried out as in Example 1. Gasoline extract with oil is treated with activated carbon 3 g / dm, then the adsorbent is separated from the extract by filtration, the extractant is distilled off -petrol

10 suck the liquid, additionally washed another precipitate with a fresh portion of diethyl ether in a ratio of 1:: 0.5. The precipitate of enotannin is dried in a drying oven in a stream of hot oil to obtain an oil. As a result

purification of gasoline extract activiro- J-5 spirit at 45 ° C. Enotannin output

Carbon Coefficient Svetopropus-8.1%, and its content in the powder 84.7

Cannas increased by 53%, and acids - When the extract was thickened to a density, it decreased by 59%. The yield of oil below 1.10 g / cm occurs peredrav14, 9%. Diethyl ether in the course of cleaning and

After all the gasoline has evaporated, a precipitate is formed during the precipitation process and the enotannin is extracted. Ex-lenno. Traction is carried out with 4 liters of alcohol. Alcohol data are presented in table. one.

Table 1

When the extract is concentrated to a density of 1.12 g / cm, the product adheres to the heated surface and partially burns it, which reduces its yield and the quality of enotannin. In addition, by thickening the extract above 1.12 g / cn, the time of formation of the precipitate is not accelerated and the amount of diethyl ether does not decrease to form.

The enotannin extract is concentrated in a vacuum apparatus at 48 ° C and a discharge of 650 mm Hg. to a density of 1.12 g / cm. Condensed extract is mixed in a ratio of 1: 2 with diethyl ether, stirred for 5 minutes and incubated for 15 minutes. After formation and compaction of the precipitate, the liquid portion is decanted, and the eno.tannin precipitate is transferred to a filter and the liquid is sucked off, the precipitate is additionally washed with a fresh portion of diethyl ether in a ratio of 1: 0.5. The precipitate of enotannin is dried in a drying oven in a hot stream. When the Bbmie mixture is kept for 20 minutes, the precipitate does not condense and the filtration time is reduced. With a dwell time of less than 10 minutes, no complete precipitate formation occurs. The latter is loose and increases product losses during the filtration process.

Data reflecting the effect of time on the degree of purification are presented in Table. 2

When drying the product in a stream of hot air with a temperature above 48 ° C, a change in color of enotannic and partial losses are observed. In addition, when dissolving the dried product, turbid solutions are formed that require additional filtration.

Indicators of the extract of enotannin, obtained by the prototype and the preTable 2

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At a temperature of less than 40 ° C, the drying time of enotannin increases, and the content of enotannin in the dried product remains constant.

Data reflecting the effect of temperature on the degree of purification are presented in Table. 3

Table 3

Lagged way are presented in Table. four

Thus, the proposed method improves the purification of enotannin (from proteins, amino acids, and other related substances).

The process of obtaining enotannin is intense. it is sified 8-10 times.

Claims (1)

Invention Formula The method of obtaining enotannin from grape seeds meal, which includes the processing of oil with ethyl alcohol from Table 4 by extracting the extract, thickening the extract, filtering and air drying, characterized in that, in order to increase the degree of purification and intensification of the process, thickening the extract is carried out to its relative. the density is 1.10-1.12 g / cm; diethyl ether is introduced into the extract before filtration and this mixture is left for 10-20 minutes, and the drying is carried out at air temperature DO-DZ C.