KR830000401B1 - Solid-liquid extraction method - Google Patents

Abstract

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Description

Solid-liquid extraction method

The figure is a schematic sectional view of the extractor by this invention.

* Explanation of symbols for main parts of the drawings

1: extraction solvent supply line 2: solid material supply line

3: extraction solvent extraction line 4: supply line of new solvent

5: discharge line of treated solid material 6: filter element

7: Passive prevention film 8: Stirrer

PI: Pressure gauge Me: Motor

The present invention relates to a method of extracting several components of a solid material by treating a solid material with a single solvent or a mixture of two or more solvents using n containers arranged in series. During the extraction process, each vessel is kept in constant stirring.

At this time, a solvent is supplied to each container at a specific flow rate and taken out. This flow rate is selected in the range of 2 to 15 m 2 / hour / m 2 and is a continuation of the flow through n containers.

In practice, each container is filled with a suitably pulverized solid material, then the solvent is filled and stirring is started.

Subsequently, fresh solvent is supplied to the first extractor (container). As a result, the solvent contained therein can be diluted and effectively extracted.

The solvent removed from this vessel is fed to the next extractor, where the same operation is repeated, followed by the same operation for all subsequent n extractors.

Immediately after the extraction from the solids of the first extractor, the extraction solvent is removed and a new solvent is supplied to clean the solids and then the solids are extracted. On the other hand, the solvent after washing is used as the extraction solvent of the next extractor. This container is then filled with fresh solid material and connected to the end of the series of containers. In this way, the supply position of the new solvent is transferred from the first vessel to the next vessel and then changed to the supply position of the new solvent for each operation (rotation).

In each vessel, 10% of the solids (micromolecules) move as the solvent flows, requiring filtering means in addition to extractors in series, thus separating the solids carried by the solvent and making the extraction complete.

The practicality and efficiency of this method are strictly correlated by a number of variables, while these variables themselves are also correlated.

As a basic barometer, as mentioned above, the ratio at the time of supplying or extracting the solvent as each extractor from the extractor must be in the range of 2-15 m <3> hours // m <2>. The ratio of the height to the diameter of the vessel, the geometry of the filtration member, the size of the holes (mesh) of the filtration member, the type of material constituting the filtration member, the thickness of the filtration member, the viscosity of the slurry, And the like are appropriately selected.

It is natural for a person skilled in the art to properly select the barometers described above, along with all other variables depending on the solids to be processed, their size, solvent and oral, in order to ensure the highest operating and extraction efficiency.

In this specification, it demonstrates with reference to the case where powder and a concentrate are obtained by extracting a lipid and unnecessary substance from the edible plant for demonstrating this invention. In addition, the detailed description about the operation mentioned later does not limit the objective of this invention, and it is clear that the extraction method mentioned above can be applied to the solid-liquid extraction of another case.

Oily seeds, such as sunflower seeds, peanuts and cottonseeds, and low contents such as soybeans, grape varieties and sesame seeds are mainly used in the food industry as a source of lipids. It is known to be used as a nutrient for humans.

Oily seeds are an important plant resource for proteins of high biological value and are therefore highly available in human nutrition.

The use of proteins present in plant seeds as nutrients is likely to reduce the solubility of proteins, and to reduce the solubility of proteins between sugars and proteins due to the presence of harmful and / or unnecessary substances such as phenols, fermentable sugars, digestive substances and lignin. It was strictly forbidden because of exogenous treatment by treatment techniques such as the Mayrad reaction and the condensation reaction between phenols and proteins.

Generally speaking, it was not possible to remove unnecessary and / or fluids in any of the seeds used to prepare the protein product.

In other words, protein materials from sunflowers prepared by deoiling plants (seeds contain oil at high concentrations) are not used as human foods for the two reasons mentioned above. In the past, a method of extracting toxic and / or insoluble substances from degreasing foods has been proposed. However, in order to exclude foreigners who lose some basic properties in the product after extraction, an improvement of such an oil extraction method is required.

In fact, the extraction cakes obtained by conventional oil extraction methods are, in principle, high in crude fiber, low in NSI (nitrogen solubility index) and low in biological value of protein selection due to treatment at high temperatures.

The first problem that must be solved to obtain protein cakes that can be used as raw materials when converting from soluble seeds to products used as a nutrient source is that seeds with low crude fiber content require lower operating temperatures than protein denaturation temperatures. It is to degrease.

At present, a treatment method that satisfies the above two conditions and at the same time economically tolerates is not used.

The extraction of lipids is generally done as follows. That is, compression, extraction with a percored solvent, extraction by immersion in a solvent, extraction with a solvent after compression, and the like.

Degreasing methods, including compression degreasing and extraction with picoring solvents, require the presence of inerts (crude fibers) in the material to be degreased, in order to achieve a technically viable treatment. Is carried out.

In the extraction operation, the seed which has been completely removed from the outer skin is degreased with a solvent, and the same amount of residual content can be used as the same amount of solvent as the conventional method. This method is also used when seed or skim powder is extracted with a solvent. This method is also possible to extract oil and toxic substances and / or insoluble substances using a suitable solvent mixture even when the seed is completely removed from the shell.

When carrying out the method, the extraction device is provided with a stirrer and a filtration member as described above, whereby the number of containers that are internally cleaned by the swinging movement caused by stirring during the extraction operation is achieved.

Thus, the filtration member functions as a liquid for liquid rather than a general function.

The material to be treated is fed to each vessel at regular intervals and held in this vessel as necessary for extraction. Such a substance is supplied in the form of a slurry prepared by mixing the extracted solvent with the extracted solvent.

The solvent flows serially in a series of vessels to be kept agitated, while the supply of fresh solvent is rotated from any other vessel to the next vessel at regular intervals.

The discharge of treated solids is rotated in turn from each container. Shifts in the supply and withdrawal positions for solids and solvents can cause apparent movement of the solids with respect to the extraction solvent. In fact, the material to be treated is first contacted with a solvent taken out of the container immediately before it, followed by contact with a clean solvent (that is, the solvent is leaving extractability) and then washed with fresh solvent almost completely after extraction. That is, the progress of the process is continuous for the solvent and discontinuous for the solid material. Since the filter member serving as the scrim is employed to keep the solvent pressure decrease through the vessels, the particulate solid material is filtered out. It is washed with an extraction solvent. This is done by regularly reducing the concentration of the extraction solvent from maximum to minimum.

Each time the particulates are collected and washed, the resulting solid cake is recycled into a container containing solids.

In the application of the method, the barometers described above are set to the following values.

Raw Material

Sunflower seeds (Cultivar Uniflor 70) were obtained from ISEA and their shells were removed industrially by hand or Buhler method.

Shelled soybean (CultiVar ADA) was obtained from Oliie Risi. It was ground with a soluble seed Difenbach and (model L2 / 30/30) used for extraction of lipids.

Ethanol (grade of drinkable grade) was obtained from Orka from Tokanomal Nucleic Acid from Ruka Pont from Chroroic Acid with purity greater than 97% from Fluka. Pure chemical reagents were used.

[Way]

Chemical analysis of the raw materials and products to be extracted was carried out according to a conventional method.

The Association Official Analytical Chemists (AOAC) method (12th edition 1975) used for each component is as follows.

The measurement of the whole sugar was carried out according to Mr Dubois' method (Anadical. Chemistry Anal. Chem. 28,350).

The residual content of nucleic acid and ethanol was measured according to the method of Mr. Wan et al. Using gas chromatography HP model 5840A (J.A.O.C.S. 54,542 (1977)).

For the measurement of lipids, AACC (American Association of Cereal Chemiste) 1962 NO 30-36 was used. The measurement of lignin was carried out by the standard method of Chemical Analysis 6th edition II B volume, 1937 pages. The content of cellulose was calculated from the difference between crude fiber and cellulose.

The content of chromogenic acid (as phenol) (for solid and liquid matters) was measured according to the method of Bittoni et al. (Rivista Italiana Sostanze Grasse, 54, 421, 1977). The nitrogen solubility index (NSI) for solids was measured at pH 9.5 (and pH 7.0) according to the Analytical Oil Chemists Society (AOCS) 1969 Ba 11-65 method. Protein Dispersion Index (PDI) (for solids) was measured according to the AOCS 1969 Ba 10-65 method.

Another object of the present invention is to provide an extractor shown in the accompanying drawings. The device comprises a container with a separator 6 for the solid material to be extracted. This separator may have various shapes (plug, cylinder, star, sphere, etc.). Holes of varying dimensions must be provided to maintain the highest amount of solid material without damaging the free flow of fluid solvent therethrough.

In other words, it acts as a shaker, and some of the solid material is transferred through the shaker as it flows through the solvent. The inside of the vessel is equipped with a single plate type or many plate type agitators 5, so that the rotation speed r.p.m is variable. The solvent is generally supplied from the bottom side, and the discharge is made through the filtering member (ie screen member). Solid material supply and discharge ports are provided at the respective container faucets and bottoms. Moreover, the film | membrane 7 for preventing a wave is provided in the inside of a container. The pore diameter and material of the screen vary depending on the type of extraction to be performed, the type of solvent used and the particle size of the solid material.

In the schematic diagram of the extractor, reference numeral 1 denotes an extraction solvent supply line, 2 a solid material supply line, 3 an extraction solvent extraction line, 4 a fresh solvent supply line, 5 a solid material discharge line after treatment, 6 is a filtering member, 7 is a wave preventing film, 8 is a stirring paper, PI is a pressure gauge, and Me is a motor.

Example 1

Extraction of Lipid from Shelled Sunflower Seeds (Uniflor 70 Cultivar)

Preparation of Seed Powders Stripped

The outer skin of the sunflower (Uniflor 70 Cultivar) seed having the chemical composition shown in Table 1 was peeled off and then ground to 0.25 mm with a Diefenbach mill. Such material was extracted with a solvent without further treatment.

Extraction of lipids

It extracted using the extractor shown in drawing. The operating conditions are as follows.

Supply of material: 2.5 kg of flakes of sunflower seeds were fed to an extractor of volume 15 l.

Extraction Solvent: Nomal Nucleic Acid

Stirring Strength: 0.8kw / ㎥

Temperature: 35 ℃

Extraction time: 6 hours

Flow Rate of Extraction Solvent: 12.5ℓ / hour

Recirculating solvent flow rate: 12.5ℓ / hour

Filter element: Stainless steel gauze with a hole diameter of 25 microns

The slurry constant amount of the extract raw material flakes prepared as described above was supplied rotationally to each extractor at 1 hour intervals. The number of extractors used was six. Under stable conditions, 1 kg of sunflower seeds flakes were extracted with 5 L of solvent. About 10% of the material to be extracted having a particle size of 25 microns or less was passed through the hole of the filtering member and transferred by the extraction solvent. In this way, the material from the extractor was recycled to the reservoir with the corresponding degreasing material. The solvent was removed by the depressurization furnace of 25 degreeC with respect to the degreasing sunflower powder collect | recovered from the discharge | emission of each extractor. Samples of degreasing powder taken out during 48 hours of treatment were analyzed twice for proteins, lipids, moisture, crorogenic acid (as phenol), lignin, cellulose, sugars and ash according to the method described previously. According to the analysis results shown in Table 1, the residual lipid content was 2% or less and the NSI (nitrogen dissolution index) was 77.5% at pH 9.5.

TABLE 1

Example 2

Preparation of Extracted Seeds from Partly Skinned Soybeans

Partly shelled soybeans of the ADA variant were obtained from Olii and Risi. The chemical composition of this soybean is shown in Table 2. Soybeans were heated at 70 ° C. for 30 minutes prior to extraction of the substrate and ground into flakes of 0.25 mm thickness by Difenbach.

Extraction of lipids

Extraction was carried out using an extractor as in Example 1 under the following conditions.

Raw material: 5 kg of the soybean flakes prepared as described above were fed to an extractor with a volume of 15 L.

Extraction Solvent: Nomal Nucleic Acid

Stirring Strength: 1.0KW / ㎥

Temperature: 35 ℃

Extraction time: 3 hours

Flow of Extraction Solvent: 20ℓ / hour

Flow of Recirculating Solvent: 22ℓ / hour

Filter element: Gauze of stainless steel with a hole of 125 microns

A predetermined amount of the flakes to be extracted as described above was supplied at intervals of 30 minutes while rotating the supply position to each extractor. The number of extractors is six. Under stable conditions, 1 kg of flakes (soybean) was extracted with 2 liters of solvent. Ten percent of the raw material of the particle size of 125 microns or less was passed through the hole of the filtering member and transferred by the solvent.

The material from the extractor was recycled to the reservoir with the corresponding degreasing supplement. The degreasing soybean powder collect | recovered from the discharge | emission of each extractor was dried under reduced pressure in the furnace at 25 degreeC. Samples of the degreasing powder obtained during the 72-hour treatment were analyzed twice for protein, lipids, moisture, croroic acid (as phenol), lignin, cellulose, sugars and ash according to the method described above.

According to the analysis results shown in Table 2, the residual lipid content was 1.3% or less, and the NSI was 6.7% at pH 9.5.

TABLE 2

Example 3

Preparation of Protein Concentrates by Extraction of Chroroic Acid and Soluble Sugars from Sunflower Skim Powder

Preparation of sunflower skim powder

According to Example 1, the skim powder of the sunflower was prepared using the seed which peeled off the shell by the Buhler method. The chemical composition of the powder is shown in Table 3.

Extraction of Insoluble Ingredients

It extracted under the following conditions using the extractor shown in drawing.

Supply of raw materials: 1.0 kg of skim powder of sunflower was supplied with the volume of 15 L extractor.

Extraction Solvent: Ethanol-Water Mixture (72: 28)

Stirring Strength: 1.0KW / ㎥

Temperature: 25 ℃

Extraction time: 3 hours

Flow of Extraction Solvent: 20ℓ / hour

Filtration element: 44 micron hole stainless steel gauze

의 압축건조로에서 건조했다. 48시간 처리하는 동안 얻어진 단백질 응축물의 샘플에 대해 전술한 방법에 따라 단백질, 크로로겐산(페놀로서), 조섬유, 당류, pH 9.5에 있어서의 NSI에 관한 함량을 두번 측정했다.A certain amount of powder to be extracted was fed at intervals of 30 minutes while rotating the feed position to each extractor. Six extractors were used. Under stable conditions, 1 kg of powder prepared from sunflower seeds was extracted with 7.5 solvents. About 10% of the extract raw material with a particle size of 44 microns or less was passed through the pores of the filtering member and transferred by the solvent. The material from the extractor was recycled to the storage container with significant auxiliary powder from which the insoluble components were removed. The product thus obtained (referred to as protein condensate with high protein content) is 25

Dried in a compression drying furnace. Samples of protein condensate obtained during the 48-hour treatment were measured twice in terms of protein, chromogenic acid (as phenol), crude fibers, sugars, NSI at pH 9.5.

The analysis results are shown in Table 3. According to this, the content of chromogenic acid (as phenol) was 0.29%, the protein content (N × 6.25) 67%, and NSI was 71.5% at pH 9.5.

Extraction of lipids and insolubles using other seeds such as cottonseed, sesame seeds, grape seed, seeds of hawthorn (Simmondsia Californica), peanuts, safflower seeds and bruner seeds as raw materials was also carried out.

TABLE 3

Example 4

Production of Protein Concentrates by Extraction of Oligosaccharides from Defatted Soybeans

Preparation of skim soybeans

According to Example 2, skim soybeans were prepared. The chemical composition of this defatted soybean is shown in Table 4.

Extraction of Insoluble Ingredients

Extraction was performed under the following conditions by the extractor shown in the figure.

Supply of raw materials: 1.5 kg of skim soybeans were fed to an extractor of volume 15 l.

Extraction vessel: Ethanol-water mixture (volume ratio 75: 25)

Stirring Strength: 1.0KW / ㎥

Extraction temperature: 25 ℃

Extraction time: 6 hours

Flow rate of extraction solvent: 15ℓ / hour

Filter element: Stainless steel gauze with a hole of 125 microns

A certain amount of raw material to be extracted was supplied at intervals of 1 hour while rotating the feed position to each extractor. Six extractors were used. Under stable conditions, 1 kg of the raw material prepared from soybean was extracted with 10 L of solvent. Particle Size About 10% of the extraction material of 125 microns or less was passed through the pores of the filter element and transferred by the solvent.

The material from the extractor was recycled to the reservoir with the corresponding auxiliary component which removed the insoluble components. Protein extract was obtained, which was dried in a dryer (Viani model DEVI 4VE OI).

Samples of protein extracts obtained during 32 hours of treatment were subjected to protein, lipid, moisture, lignin, cellulose, ash, sugars (measured according to Dubois method) and NSI at pH 9.5 and pH 7.0 according to the method described above. The content was measured twice.

The analysis results are shown in Table 4. According to this, the content of all sugars was 0.95%, and NSI at protein content (N × 6.25) 70.5%, pH 9.5 and pH 7.0 was 66.0% and 43.6%, respectively.

TABLE 4

Example 5

Extraction of Chroroic Acid and Sugars from Aqueous Acid pH Solution from Degreased Sunflower Seeds

Preparation of sunflower de-support fee

According to Example 1, the skim powder of sunflower was prepared using the seed which removed the shell by the Buhler method. The chemical composition of the liquid is shown in Table 5.

Extraction of Insoluble Ingredients

Extraction was performed under the following conditions using the extractor shown in the figure.

Supply of raw materials: 1.0 kg of skim powder of sunflower was supplied to the extractor of 15 L of volumes.

Extraction solvent: water adjusted to pH 3.5 by 4N formic acid

Stirring Strength: 1.0KW / ㎥

Temperature: 25 ℃

Extraction time: 3 hours

Flow rate of extraction solvent: 20ℓ / hour

Filter element: Hole size 44 micron gauze in stainless steel

A certain amount of powder to be extracted was fed at 30 minutes intervals while rotating the feed position to each extractor. Six extractors were used. Under stable conditions, 1 kg of powder prepared from sunflower seeds was extracted with 7.5 solvents. About 10% of the particle size of the extract raw material of 44 microns or less was passed through the hole of the filtering member and transferred by the solvent. The material from the extractor was recycled to the storage vessel with the corresponding co-powder with pH adjusted to 5.0 with 2N NaOH. The product thus obtained (referred to as protein concentrate because of its high protein content) was ground with a Fryma cordoid mill and dried with a spray dryer. Samples of protein concentrates obtained during the 32 hour treatment were measured twice in terms of protein, lipids, moisture, crude fiber, ash, sugars and NSI at pH 9.5 according to the method described above.

The analysis results are shown in Table 5. According to this, the content of chromogenic acid (as phenol) was 0.45%, the protein content (N × 6.25) 64%, and the NSI at pH 7.0 were 58%.

TABLE 5

Claims (1)

A solid-liquid extraction method for treating solid materials with solvents or mixed solvents in a plurality of interconnected extractors, wherein the solid materials to be extracted periodically and cyclically and continuously at the beginning of the extraction process and when the pretreated solid material is discharged from the extractor. Is supplied to each extractor, and the solvent is continuously circulated through the extractor interconnected for extraction of the solid substance in each extractor, and the solvent is discharged from the extractor containing mostly pretreated solid substance, and the filtration member extended into the extractor. The solids-liquid in each extractor is kept in the extractor so that the filtered solid substance remains in the extractor when the solvent containing residual solid matter is discharged from one side extractor through the filtering member and circulated to the next extractor. The solid material is filtered from the solvent by the filtration member during the extraction process. And stirring the solvent and the solid material by the stirring device in each extractor to sweep the solid material filtered out of the filtering member by the rotational movement of the solid material and the solvent by stirring, and periodically circulating the pretreated solid material from the extractor periodically. Solid-liquid extraction method characterized in that the discharge bin.

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