WO2018101710A1 - Oil palm biomass solid phase extract containing high concentration of fat-soluble physiologically active substance produced from palm oil production by-products and method for producing same - Google Patents

Abstract

The present invention relates to a solid phase extract containing, at a high concentration, a fat-soluble physiologically active substance, such as carotenoid and tocol, produced from by-products generated during a process of producing palm oil, and a method for producing the same. Since a fat-soluble physiologically active substance, which is contained in palm biomass at a low concentration and can only be extracted by using a large amount of solvent, is extracted by using only water and then adsorbed on a small amount of biomass to be solidified, the fat-soluble physiologically active substance subsequently can be extracted and recovered even after extraction with a small amount of solvent, whereby the present invention can produce raw materials useful for the industrial production of various physiologically active substances possessed by palm biomass. In addition, the present invention is a useful method to improve the economic feasibility of biorefinery by increasing the value added of palm oil production by-products.

Description

Oil palm biomass solid extract containing high concentration of fat-soluble physiologically active substance prepared from palm oil manufacturing by-product and its manufacturing method

The present invention is a method for extracting / recovering fat-soluble bioactive substances carotenoids, tocopherols and tocotrienols from the by-products or wastes left after the production of palm oil, and oil palm bio-containing high concentrations of fat-soluble bioactive substances such as carotenoids produced by the method. It relates to mass solid extract.

More specifically, the fat-soluble physiological activity by solvent extraction, including 10 to 30% by weight palm oil containing the fat-soluble bioactive substance, 15 to 40% by weight of solvent-insoluble oil palm biomass and 40 to 70% by weight of water The present invention relates to an oil palm biomass solid extract and a method for preparing the same that can be used for industrial production of materials.

This application claims priority based on Korean Patent Application No. 10-2016-0163850, filed December 2, 2016, and all the contents disclosed in the specification and drawings of the application are incorporated in this application.

Unlike other vegetable oils, palm oil produced from oil palm fruit is composed of saturated fatty acid and unsaturated fatty acid in a ratio of 1: 1, so it shows semi-solid state at room temperature like animal oil or fat. Unrefined palm oil is called crude palm oil (CPO), and 500 to 1,600 mg / kg carotenoids, 600 to 1,000 mg / kg tocopherol and tocotrienol, coenzyme Q10, It contains high value-added bioactive substances such as phytosterol and is red by beta-carotene.

Empty fruit bunch of oil palm (EFB), which is produced as a by-product of palm oil production, accounts for about 23% by weight of palm fruit, and is generally dried to about 40% by weight of moisture. It is used as boiler fuel in manufacturing plants, and the remaining ash and most of the process rooms are used for fertilizers and compost. Part of the palm oil (e.g., 4.6% by weight) is left in the palm fruits in the process of increasing the palm fruit at high temperature to remove the fruits, which causes the palm fruits to contain the various bioactive substances.

Palm pressed fiber (PPF), which is entangled like cobwebs in palm fruits containing palm oil and is released during the extraction process, accounts for 15% of palm fruits and contains a large amount of palm oil. Along with the room, it is used as boiler fuel for palm oil manufacturing plants. This palm pulp fiber contains 5 to 7% by weight of palm oil, 4,000 to 6,000 mg / kg of carotenoids and 2,400 to 3,500 mg / kg of tocols, which are known to contain more bioactive substances than palm oil (Choo etc., JAOCS, 1996, 73, 599-602 .).

In addition, the palm fruit mill waste water (POME, palm oil mill) generated in the process of recovering palm oil by squeezing the nut and separating the liquid from the palm nut by steaming fresh fruit bunch of oil palm with high temperature steam. effluent) contains 95-96% by weight of water, 0.6-0.7% by weight of fat, and 4-5% by weight of solids. Protein, carbohydrates, fats and minerals are present in high concentrations. It can be used for the production of useful substances, but most of them are disposed of in wastewater treatment plants or used as raw materials for biogas production. It also contains a significant amount of palm oil, which contains a large amount of bioactive substances (about 1,500 mg / kg for carotenoids, Ahmad et al., Desalination Water Treat , 2009, 7, 251-256.).

As mentioned above, palm oil production process by-products contain a significant amount of fat-soluble components, and these components also include high value-added bioactive substances such as beta carotene, alpha carotene, tocopherol and tocotrienol. Beta-carotene has an antioxidant activity, has provitamin A activity, and has the characteristics of inhibiting the occurrence of various cancers such as pancreatic cancer, rectal cancer, prostate cancer, breast cancer, melanoma and skin cancer and preventing cataracts. Alpha-carotene also has a cancer preventive effect and antioxidant activity and its activity is superior to beta-carotene, but provitamin A activity represents half of beta-carotene. Tocopherol is an antioxidant that has vitamin E activity. When used in conjunction with other antioxidants, tocopherol prevents macular degeneration and prevents some cancers, cataracts, and Parkinson's disease. It is also used as a food preservative. Tocotrienols are more efficient antioxidants than tocopherols and have vitamin E activity, inhibit cancer formation and inhibit cholesterol formation.

These bioactive materials are high value-added compounds present in a large amount in the by-products of palm oil production, but most of them are not recovered. Currently, fat-soluble substances including such beta-carotene, alpha-carotene, tocopherol, tocotrienol are extracted from palm oil, but the amount is extremely limited. In particular, most beta-carotene is produced by chemical synthesis, which is less effective than natural substances, but the manufacturing cost is known to be 2,000 US dollars per kg. However, if these fat-soluble bioactive substances can be extracted inexpensively from palm oil manufacturing by-products, it is expected that their added value as natural bioactive substances will be more than synthetic materials.

For this reason, researches on extracting physiologically active substances from palm oil by-products discarded until recently have been steadily conducted, but they have not been industrialized yet. As a patented technology, only the extraction of tocopherol and tocotrienol from palm fatty acid distillate has been reported (US Patent No. 5190618, Korean Patent Publication No. 10-1481197). They used organic solvents such as nucleic acids for the extraction of fat-soluble bioactive substances and supercritical water or supercritical carbon dioxide for some extraction studies.

The solvent-based extraction of fat-soluble physiologically active substances contained in such a large amount of biomass at low concentrations is 0.1 g / cm ^{3 for the} bulk density of the biomass. Due to the excessive cost is inevitable, such as the use of an organic solvent and a large extraction equipment more than five times the weight of the biomass weight, more practical extraction methods are required.

The present inventors have found that the fat-soluble physiologically active substance contained in the palm oil by-product is dissolved in palm oil, and this palm oil has the characteristic of emulsifying and eluting in water when friction-pulverizing with water. In addition, emulsion particles containing this fat-soluble physiologically active substance are attached to the biomass fine particles by coagulant, and if necessary, additional flocculant improves sedimentation by coarsening, thereby increasing dehydration efficiency. To solidify through solid-liquid separation. The solid extract prepared in this way can be easily handled because it contains only a 1% of the volume of biomass while containing a high concentration of fat-soluble physiologically active substances of palm by-products. In addition, since the bioactive substance can be extracted at a high concentration even with a small amount of solvent, it is useful for the industrial production of high value-added bioactive substances contained in palm by-products.

The present invention was developed to solve the above problems, and aims to provide a simpler and more economical method for extracting a fat-soluble physiologically active substance containing a low concentration due to the small weight or excessive water content of palm oil production by-products. It is done.

In the present invention, oil palm biomass solid phase extract solidifying emulsion particles containing fat-soluble physiologically active substances that can be easily handled with only about 1% of the volume of biomass while containing a high concentration of fat-soluble physiologically active substances such as carotenoids, and a preparation method thereof. To provide.

In order to solve the above problems, the present invention provides solvent extraction including 10 to 30% by weight of palm oil containing fat-soluble physiologically active substance, 15 to 40% by weight of solvent-insoluble oil palm biomass and 40 to 70% by weight of water. It provides an oil palm biomass solid extract that can be used in the industrial production of fat-soluble physiologically active substances.

According to the present invention, the biomass gruel manufacturing step of manufacturing a biomass gruel containing an emulsion by immersing the byproduct oil by-products in water and friction grinding; Liquid extract manufacturing step of preparing a liquid extract containing biomass fine particles and emulsion particles by solid-liquid separation of the biomass gruel obtained in the biomass gruel manufacturing step; Coagulant, flocculant or coagulant and flocculant are sequentially added to solidify palm oil emulsion particles containing fat-soluble bioactive substances in the liquid extract obtained from the liquid extract preparation step. Preparing agglomerates to adsorb / coagulate / aggregate the biomass particles; And a solid extract preparation step of preparing a solid extract through solid-liquid separation after the agglomerate preparation step; and a process for producing an oil palm biomass solid phase extract, comprising a fat-soluble physiologically active substance from palm oil manufacturing by-products at a high concentration. to provide.

The oil palm biomass solid extract solidifying emulsion particles containing fat soluble bioactive substances according to the present invention can be easily handled because it contains only about 1% of the volume of biomass while containing a high concentration of fat soluble bioactive substances which palm by-products have. have. In addition, since the bioactive substance can be extracted at a high concentration even with a small amount of solvent, it is useful for the industrial production of high value-added bioactive substances contained in palm by-products.

The present invention enables to prepare a solid extract containing a high concentration of high value-added fat-soluble physiologically active substances such as beta-carotene from palm fruits, palm pulp fiber and palm oil plant wastewater, using as a raw material a small amount of organic solvent or supercritical extraction It is useful for industrially preparing fat-soluble physiologically active substances by utilizing various conventional extraction techniques and purification techniques such as chromatography.

1 is a process chart showing the manufacturing step of the oil palm biomass solid extract according to an embodiment of the present invention.

Hereinafter, the present invention will be described in detail. The terms or words used in this specification and claims are not to be construed as limiting in their usual or dictionary meanings, and the inventors may appropriately define the concept of terms in order to best explain their invention in the best way possible. It should be interpreted as meaning and concept corresponding to the technical idea of the present invention based on the principle that the present invention.

As used throughout this specification, the term “lipophilic bioactive substance” is a biochemical that is hardly soluble in water and soluble in organic solvents. Carotenoids such as alpha carotene, beta carotene and gamma carotene, tocopherol and tocotrienol It refers to bioactive substances contained in palm fruits, palm pulp fiber and palm oil plant wastewater such as tocols.

In the present invention, "carotenoid" or "beta carotene" refers to a carotenoid and a beta form of the substance as a generic meaning containing various carotenes, respectively, but refers to other fat-soluble bioactive substances such as tocols. It is also used as a symbolic meaning.

In the present invention, "biomass gruel" refers to a biomass suspension prepared by adding water to biomass and friction grinding, and containing palm oil emulsion particles and biomass powder containing fat-soluble physiologically active substances. This biomass gruel is used as a raw material for primary solid-liquid separation, which separates palm oil emulsions and some fine biomass from most insoluble biomass.

In the present invention, "liquid extract" refers to a liquid substance in which most of the biomass is removed by solid-liquid separation of the biomass contaminants and palm oil emulsion particles and some biomass particles remaining in water. Coagulant, flocculant or coagulant and flocculant is a target material to be aggregated by sequential addition.

In the present invention, "coagulant" refers to a substance used to adsorb / condense suspended particles to biomass particles in a liquid extract, and is a monomolecular inorganic coagulant, a high molecular weight inorganic coagulant, and a low molecular weight. The organic polymer (molecular weight of 1 million or less) of the, the mono-molecular inorganic coagulant is aluminum sulfate (aluminum sulfate), ferrous sulfate (ferrous sulfate, ferric sulfate), ferric chloride (ferric chloride) and the like are representative, polymer type inorganic condensing agents include polyaluminum chloride _{(poly aluminum chloride: [Al 2} (OH) n Cl 6 -n] m), polyaluminum sulfate _{(poly aluminum sulfate: [Al 2} (OH) n (SO 4) 3 - _{n / 2} ] _m ) and the like, and low molecular weight organic polymers include polydicyandiamide, polyamine, and polydiallydimethyldimethylammonium chl. oride: polyDADMAC or polyDDA). Although the coagulant according to the present invention may be in the form of a metal salt or any organic polymer, it is preferable to use an organic polymer in consideration of subsequent processes such as extraction of a fat-soluble physiologically active substance, and in particular, the organic polymer coagulant has a cationic property. It is preferable to use a polymer. The coagulant according to the present invention serves to adsorb / condense the suspended particles to the biomass particles in the liquid extract.

In the present invention, "flocculant" is a flocculant in order to more effectively perform the solidification of the adsorption / flocculation of the emulsion particles and biomass particles formed by the use of a coagulant in the solid-liquid separation step and solid extract form. It is a generic term for materials used to improve sedimentation and increase dehydration efficiency by coarsening, and is a polymer material having a molecular weight of 300 to 5 million or more, and is a nonionic polymer by homopolymerization mainly based on an acrylamide monomer. Anionic polymers prepared by copolymerization with phosphorus polyacrylamide, acrylate (acrylate) monomers or hydrolysis of acrylamide, etc. or cationic polymers by copolymerization with cationic monomers may be used. The flocculant according to the present invention is very effective in coagulating adsorption / coagulum of emulsion particles and biomass particles to improve sedimentation and increase dehydration efficiency to solidify the solid extract form.

In the present invention, the roles of "coagulant" and "flocculant" are defined separately, but only coagulant or coagulant may be used, or more effective when both coagulant and flocculant are used.

In the present invention, the "solid extract" refers to palm oil, insoluble (solvent-insoluble) oil palm biomass, which is mostly produced when water is separated and solid-liquid separated by adding a polymer flocculant to the liquid extract. It means a solid material containing fine particles and a small amount of water.

Palm oil production by-products to extract the fat-soluble physiologically active substances in the present invention are palm fruit bunch (oil palm bunch), palm pressed fiber (palm pressed fiber) and palm oil mill effluent (palm oil mill effluent). Palm fruits contain both fresh fruit bunches at high temperature, dropping off palm fruits and then squeezed to recover the palm oil. do. These palm fruits and palm pulp fibers contain more physiologically active substances such as carotenoids, tocols and polyphenols, but are reduced rapidly as they decay due to the hot and humid environment of the mountain area, so it is desirable to dry them as soon as they are discharged from the factory. Do. Palm oil plant wastewater contains various water-soluble substances such as biomass, such as palm mesocarp in the form of fine particles, palm oil and protein in the emulsion state, and can be used for extraction of the bioactive substance as it is after being cooled to room temperature.

In the present invention, a coagulant or flocculant which serves to facilitate dehydration through filtration by adsorbing / coagulating / aggregating the palm oil in the oil state and the palm biomass in the particulate state is polydicyandiamide and polyacrylamide. It is preferable to use a cationic, anionic or nonionic polymer flocculant comprising a), and other coagulants or flocculants as described above may be added according to the type of biomass and the ratio of the emulsion, and are not limited thereto. Do not.

The solid extract containing a high concentration of a fat-soluble physiologically active substance prepared from the palm oil preparation by-product provided in the present invention is obtained as a solid after separation of the palm oil containing the fat-soluble physiologically active substance to biomass particles insoluble in water. This solid extract consists of palm oil containing 40 to 70% water, 15 to 40% insoluble biomass and 15 to 30% bioactive material. It may also contain a small amount of coagulant or flocculant added during the preparation of the aggregate. This solid extract contains bioactive substances such as alpha-carotene, beta-carotene, gamma-carotene, lycopene, tocopherol, tocotrienol and vegetable sterol, depending on the by-products of palm oil used, and the content of each bioactive substance depends on the type and composition of the raw materials. It is very different accordingly, and is not specifically limited. For example, when the fresh palm pulp fiber is used as a raw material, the concentration of the fat-soluble physiologically active substance of the solid extract is 2 to 5 times higher than that of the raw material, but the solid extract is 1/5 to 1 / by weight containing about 50% water. Decreases to 20 Among these solid extracts, insoluble in water is a biomass of cellulose main components derived from palm fruits, palm pulp or palm pulp.

The present invention

1) a biomass gruel manufacturing step of producing biomass grits containing emulsion by immersion by adding water to palm fruits or palm pulp, which is a by-product of palm oil, and by friction grinding;

2) a liquid extract manufacturing step of preparing a liquid extract containing biomass fine particles and emulsion particles by solid-liquid separation of the biomass gruel obtained in the biomass gruel manufacturing step;

3) Coagulant, flocculant or coagulant and flocculant are sequentially added to solidify palm oil emulsion particles containing fat-soluble bioactive substances in the liquid extract obtained from the liquid extract preparation step. Agglomerating step of adsorbing / aggregating / aggregating the particles with the biomass particles; And

4) The fat-soluble physiologically active substance from palm oil manufacturing by-products includes a solid phase extracting step of preparing a solid extract including high concentrations of carotenoids and tocols through solid-liquid separation after the flocculation step but reducing the water content to about 40 to 70%. It provides a method for producing an oil palm biomass solid extract, characterized in that it contains a high concentration.

In the production method according to the present invention, the friction grinding of the biomass grind production step may be to use the emulsification eluting principle of palm oil from the oil palm biomass.

In the manufacturing method according to the present invention, the trituration of the biomass grind production step may use a twin screw extruder to extract the fat-soluble physiologically active material from the oil palm biomass.

In the production method according to the present invention, the solid-liquid separation in the liquid extract manufacturing step may use a centrifugal separation method or a filtration method.

In the manufacturing method according to the present invention, the step of producing the aggregates using at least one of a cationic, anionic or nonionic polymer flocculant including polydicyandiamide and polyacrylamide as a polymer flocculant It may be.

In the production method according to the present invention, the solid-liquid separation in the solid phase extract manufacturing step may be to use a pressure filtration method including a filter press or a belt press.

Hereinafter, a method for preparing the oil palm biomass solid extract according to the present invention will be described in more detail.

The first step in the method for preparing a solid extract containing a high concentration of carotenoids and tocols from the palm oil production by-products according to the present invention is to add water to the palm oil production by-products and to prepare biomass grits through frictional grinding. The palm bin or palm pulp fiber crushed is first subjected to 1 to 5 times more water than biomass drying and friction grinding. At this time, the friction mill can be used is a twin screw extruder (disc mill) or disc mill (disc mill), in order to reduce the energy consumption and at the same time maximize the friction effect is preferably a twin screw extruder. At this stage, the palm biomass is crushed in water, and the palm oil contained in the biomass is eluted as emulsified particles by emulsification of glycolipids or phospholipids. The efficiency of emulsifying and eluting palm oil may vary depending on the friction grinding conditions. When considering the properties of semi-solid palm oil at room temperature, the frictional grinding temperature is 20 ^o C or more and 100 ^o C or less, and the frictional grinding temperature is 20 to 50 ^o when additionally considering the carotenoid properties that may be altered at high temperature. C is preferred. The operating conditions of the twin screw extruder or the disk mill are not limited to a specific range because they may vary depending on the type of equipment, the combination of screws or the type of the disk.

The second step of the present invention is the solid-liquid separation to prepare an emulsion containing the fat-soluble physiologically active component from the biomass gruel prepared in the first step and a liquid extract containing a small amount of biomass particles. In order to increase the dissolution rate and recovery rate of the palm oil emulsion before solid-liquid separation, first, water is further added to the biomass gruel to contain 10 to 20 times more water than during drying to prepare a uniform gruel. At this time you can use a warm water of room temperature to 50 ^o C or less, or gonjuk can be allowed to warm to the room temperature to 50 ^o C or less in order to enhance the stability of the emulsion particles promote or generate the production of emulsion particles. The solid-liquid separation of this gruel can be used a variety of methods commonly used in the art, and examples thereof include centrifugation, rotary dehydration, suction filtration and pressure filtration. In order to recover the emulsion containing the physiologically active substance in high yield, centrifugal separation using palm oil-containing emulsion particles having a specific gravity smaller than that of water is preferable. That is, some of the biomass particulates (eg, about 1% of the total biomass drying, etc.) are centrifuged at low speed so as to stay in the liquid phase (eg, 1 minute at 200 × g) and then fine biomass particles By recovering the supernatant containing the emulsion can be separated from most of the biomass as a precipitate. However, since the moisture content of the biomass recovered after the solid-liquid separation is large, it may not be suitable for the purpose of using the biomass from which the extractable component is removed. Filtration techniques can be applied directly to separate the emulsion from biomass pellets. This is possible because the size of the emulsion particles is several microns or less, which is smaller than most biomass. At this time, in consideration of the pulverization degree of the biomass, a filter cloth having a pore size of 2.5 microns to 15 microns may be used to allow a small amount of biomass particles and emulsion particles to pass therethrough. It is preferable to select and use a filter cloth having an average pore size through which fine biomass can pass so that the ratio of insoluble biomass in the finally prepared solid extract is 15 to 70% by weight during solid extract extraction. At this stage, both filter press, belt press and centrifugal filtration can be used to separate and recover the emulsion and fine biomass from most biomass.However, filter press or belt press with high energy recovery and high recovery of liquids can be used for solid-liquid separation. Preferably, the filter press having the highest recovery rate of the liquid is most preferred.

The third step of the present invention is to prepare a solid extract by adsorbing and dehydrating a small amount of biomass microparticles containing an emulsion containing a bioactive material. To this end, the liquid extract obtained in the solid-liquid separation of the second step is treated with a polymer coagulant to coagulate the biomass fine particles and the emulsion particles, and thereafter, the coagulant is further treated to coagulate into particles that are hard enough to be filtered under pressure. To this end, the polymer coagulant is made into a high concentration aqueous solution, and is added to the liquid phase and stirred while adsorbing to the suspended particles and the fine biomass. The flocculant is then added and stirred and allowed to stand for at least several minutes so that aggregates can form. At this time, as the polymer coagulant and flocculant, cationic, anionic and nonionic polymer coagulant including polydicyandiamide and polyacrylamide may be used, and solid phase extract may be prepared by solid-liquid separation. The type and amount used are not limited as long as the aggregates are as hard as possible. Once an aggregate is formed, it is subjected to solid-liquid separation using the methods described in Step 2 above to prepare a solid phase extraction having a low water content. At this time, the pressurized filtration which is the lowest the water content of the solid extract obtained as a result of the solid-liquid separation is preferred, and it is more preferable to apply a filter press in terms of low energy consumption and low water content of the solid extract. The solid extract containing high concentration of the bioactive substance prepared in this way is only 2 to 15% of the weight of the raw material biomass when compared to drying, and the water content is low to 40 to 70% by weight, so that a small amount of water-soluble organic solvent or supercritical water, Supercritical carbon dioxide can also extract economically soluble bioactive substances.

In addition, the present invention is 10 to 30% by weight of palm oil containing a fat-soluble bioactive substance such as carotenoids and tocol produced according to the above method; It provides an oil palm biomass solid phase extract that can be used for the industrial preparation of fat-soluble bioactive substances by solvent extraction, including 15 to 40% by weight of solvent-insoluble oil palm biomass and 40 to 70% by weight of water. .

In the oil palm biomass solid extract according to the present invention, the fat-soluble physiologically active substance may be a carotenoid or tocol, and at least one selected from the group consisting of alpha carotene, beta carotene, gamma carotene, lycopene, cotoperol and tocotrienol. Can be.

In the oil palm biomass solid extract according to the present invention, the oil palm biomass palm oil (empty fruit bunch of oil palm), palm pressed fiber (palm pressed fiber) and palm oil plant generated as a by-product in the palm oil manufacturing process It may be at least one of palm oil mill effluent.

Solid extract containing a high concentration of the fat-soluble physiologically active substance of the present invention prepared as described above may then be used to extract carotenoids and tocol using a solvent. That is, the solvent was added at a ratio of 1: 1 (w / v) to 1:10 (w / v) with respect to the solid extract prepared by reducing the water content in step 3, followed by stirring to extract the bioactive material, followed by centrifugation or Filtration yields a solution containing carotenoids and tocols. At this time, the solvent used to extract the fat-soluble physiologically active substance may include a water-soluble organic solvent, a poorly water-soluble organic solvent, supercritical water or supercritical carbon dioxide, and selected in consideration of the solubility and cost of the bioactive substance to be extracted. can do. Examples include water-soluble organic solvents such as alcohols such as ethanol, methanol and isopropyl alcohol, other organic solvents such as tetrahydrofuran, and poorly water-soluble organic solvents such as chloroform, dichloromethane, ethyl acetate, hexane, and other organic solvents. Supercritical water or supercritical carbon dioxide may be used in combination with the solvent, and all solvents and extraction methods available in the art may be used.

The small amount of solid extract containing high concentrations of carotenoids and tocol prepared from palm oil by-products according to the present invention enables economic production of industrial raw materials through solvent extraction and purification of physiologically active substances.

Hereinafter, the preferred embodiment of the present invention will be described in detail with reference to the comparative example so that those skilled in the art can easily carry out. In particular, the technical spirit of the present invention and its core configuration and operation are not limited by this. In addition, the content of the present invention may be implemented in various other forms of equipment, and is not limited to the embodiments and embodiments described herein.

Example 1. Preparation of solid extract containing high concentration of fat-soluble bioactive substance from palm fruit

300 g (empty fruit bunch of oil palm, Indonesia) immersed so that the ratio of biomass to water is 1: 5 during drying. The twin screw extruder (TEK 40 MHS, SM PLATEC, Korea) is equipped with a kneading block and a mixing screw, and is operated at a speed of 20 revolutions per minute at 50 ^o C while injecting palm-based fruits immersed in water. Grinding was carried out. Biomass grits prepared by friction grinding were added with water to a final ratio of 1:20 (biomass: water) and stirred, followed by a small filter press with 6 micron filter cloth (manufactured by Korea Research Institute of Chemical Technology, Korea). ) Was separated and recovered as a liquid extract containing an emulsion and biomass particles and a large amount of biomass, respectively (A). Polydicyandiamide (polydicyandiamide, DC-400, SNF Korea, Korea) was treated to this liquid extract at a concentration of 3,000 mg / L and stirred at a slow rate to allow the adsorbed particles to adsorb to the biomass particles. Cationic polyacrylamide (C-211, SNF Korea, Korea) aqueous solution was added thereto at a concentration of 20 mg / L, and stirred for 60 minutes at room temperature to form aggregates. After the aggregate was formed, the solid extract was prepared by solid-liquid separation using a small filter press (Korea Institute of Chemical Research, Korea) attached to the 6 micron filter cloth. The solid extract was weighed, taken in small amounts and lyophilized to determine the moisture content. In addition, 2 g of this solid extract was taken in a 50 ml falcon tube, followed by ultrasonic extraction with 9 ml of ethanol, followed by centrifugation to prepare a supernatant. Carotenoids were quantified as indicators of fat-soluble bioactive substances by a spectrophotometer (Benchmark Plus microplate spectrophotometer, BIO RAD, USA, 450 nm). The ethanol remaining in the falcon tube was decanted and blown with air to remove the ethanol by volatilization. 50 ml of hexane (n-hexane) was added thereto, followed by ultrasonic extraction, centrifugation and supernatant removed. Air was blown to remove hexane, dried under reduced pressure for 24 hours, and weighed to calculate the weight of the solid extract from which the fat-soluble component was removed. The composition and yield of the palm fruit fruit solid extract from the experimental values were calculated and shown in Table 1.

Example 2. Preparation of solid extract containing high concentration of fat soluble bioactive substance from palm pulp fiber

300 g of palm pressed fiber (from Indonesia) (during drying, 6.4% ethanol extractable ingredient) was immersed so that the ratio of biomass and water was 1: 5. A twin screw extruder (TEK 40 MHS, SM PLATEC, Korea) is equipped with a kneading block and mixing screw, and is operated at a rate of 20 revolutions per minute at 50 ^o C. Grinding was carried out. Biomass grits prepared by friction grinding are mixed by adding water and stirring to make a final ratio of 1:20 (biomass: water) with water (small chemical press with 6 micron filter cloth) , Korea) were separated and recovered as a liquid extract containing the emulsion and biomass particles and a large amount of biomass (A). Polydicyandiamide (polydicyandiamide, DC-400, SNF Korea, Korea) was treated in a liquid extract at a concentration of 3,000 mg / L and stirred at a slow rate to cause the emulsion particles to coagulate in the fine biomass. Cationic polyacrylamide (polyacrylamide C-211, SNF Korea, Korea) was added thereto at a concentration of 30 mg / L, and stirred for 60 minutes at room temperature to form an aggregate. After the aggregate was formed, the solid extract was prepared by solid-liquid separation using a small filter press (Korea Institute of Chemical Research, Korea) attached to the 6 micron filter cloth. The solid extract was weighed, taken in small amounts and lyophilized to determine the moisture content. In addition, 2 g of this solid extract was taken in a 50 ml falcon tube, followed by ultrasonic extraction with 9 ml of ethanol, followed by centrifugation to prepare a supernatant. Beta-carotene was quantified as an indicator of fat-soluble bioactive substance by high performance liquid chromatography (Waters, USA) with an absorbance detector. The ethanol remaining in the falcon tube was decanted and blown with air to remove the ethanol by volatilization. 50 ml of hexane (n-hexane) was added thereto, followed by ultrasonic extraction, centrifugation and supernatant removed. Air was blown to remove hexane, dried under reduced pressure for 24 hours, and weighed to calculate the weight of the solid extract from which the fat-soluble component was removed. The composition and yield of palm pulp fiber solid extract were calculated from the experimental values, and are shown in Table 1.

Example 3. Preparation of solid extract containing high concentration of fat-soluble bioactive substance from palm oil factory wastewater

1,000 g of palm oil mill effluent (including palm pulp, Indonesia) was treated with polydicyandiamide (polydicyandiamide, DC-400, SNF Korea, Korea) at a concentration of 3,000 mg / L and stirred at a slow rate. The emulsion particles were allowed to coagulate in the fine biomass. Cationic polyacrylamide (polyacrylamide C-211, SNF Korea, Korea) was added thereto at a concentration of 40 mg / L, and stirred for 60 minutes at room temperature to form an aggregate. After the aggregate was formed, the solid extract was prepared by solid-liquid separation using a small filter press (Korea Institute of Chemical Research, Korea) attached to the 6 micron filter cloth. The solid extract was weighed, taken in small amounts and lyophilized to determine the moisture content. In addition, 2 g of this solid extract was taken in a 50 ml falcon tube, followed by ultrasonic extraction with 9 ml of ethanol, followed by centrifugation to prepare a supernatant. Carotenoids were quantified as indicators of fat-soluble bioactive substances by a spectrophotometer (Benchmark Plus microplate spectrophotometer, BIO RAD, USA, 450 nm). The ethanol remaining in the falcon tube was decanted and blown with air to remove the ethanol by volatilization. 50 ml of hexane (n-hexane) was added thereto, followed by ultrasonic extraction, centrifugation and supernatant removed. Air was blown to remove hexane, dried under reduced pressure for 24 hours, and weighed to calculate the weight of the solid extract from which the fat-soluble component was removed. The composition and yield of the palm oil plant wastewater solid extract were calculated from the experimental values and are shown in Table 1.

Comparative Example 1. The estimated total amount of the fat-soluble physiologically active substance contained in the palm ball rooms, and pulp fiber palm and palm oil Waste Water

The dried palm fruits and palm pulp fibers were cut and pulverized with a cutter mill (manufactured by Korea Powder Machinery, Korea) to prepare a powder of 20 mesh or less. Palm oil plant wastewater was lyophilized and ground to a powder of 20 mesh or less. 5 g (during drying) of these samples were taken and placed in a Soxhlet wobble, followed by Soxhlet extraction using ethanol as a solvent. The volume of the extract was measured and a portion was taken and centrifuged. Take supernatant and measure absorbance at 450 nm to quantify carotenoids (for palm fruits and palm oil plant wastewater) or high performance liquid chromatography (absorption detector 450 nm) with high performance liquid chromatography, Waters, USA Beta carotene was quantified as an indicator of fat-soluble physiologically active substance, and the recovery rate of each example was calculated by comparing this value with the amount of carotenoid or beta carotene obtained in Examples, and the results are shown in Table 1.

Palm By-Products	Composition (g)
	Example 1 (palm fruits and vegetables)	Example 2 (palm pulp fiber)	Example 3 (palm oil factory wastewater)
Total amount	35.5	32.1	32.9
water	20.5	17.4	19.4
Insoluble Biomass	8.6	8.4	4.5
Fat-soluble ingredients	6.4	6.3	9.0
Beta-carotene or carotenoids (mg) in biomass (300g)	10.5 (carotenoids)	19.8 (beta carotene)	14.5beta carotene)
Beta-carotene or carotenoids (mg) in solid extract	4.8	10.1	12.3
Carotene or carotenoid recovery rate (%)	45	51	85

As shown in Table 1 above, 300 g of the palm oatmeal and palm pulp fiber during drying were prepared as a solid extract using the technique of the present invention, and the raw material biomass was reduced to 10% of the weight of the raw biomass. More than 30% of the fat-soluble bioactive substance contained in the mass can be recovered. In addition, it is possible to recover 85% of the fat-soluble physiologically active substance contained in the wastewater as a solid extract prepared at 4% or less by weight of the palm oil factory wastewater. This is a result of using a sample in which the content of fat-soluble physiologically active substance is extremely low after a long time after the preparation of the raw biomass. Thus, as can be seen in the literature, the technique of the present invention will be able to recover the fat-soluble physiologically active material in a higher yield when using a fresh material from a mountain region having a high content of fat-soluble physiologically active ingredients.

Claims (10)

1. 10 to 30% by weight of palm oil containing fat-soluble bioactive substance;

   15 to 40% by weight of solvent-insoluble oil palm biomass; And

   Oil palm biomass solid phase extract that can be used in the industrial production of fat-soluble bioactive substances by solvent extraction, including 40 to 70% by weight of water.
2. The method according to claim 1,

   The fat-soluble physiologically active substance is an oil palm biomass solid extract, characterized in that the carotenoid or tocol.
3. The method according to claim 1,

   The fat-soluble bioactive substance is oil palm biomass solid extract, characterized in that any one or more selected from the group consisting of alpha carotene, beta carotene, gamma carotene, lycopene, cotoperol and tocotrienols.
4. The method according to claim 1,

   The oil palm biomass may be any one or more of an empty fruit bunch of oil palm, palm pressed fiber, and palm oil mill effluent generated as a by-product during the production of palm oil. Oil palm biomass solid extract.
5. Biomass gruel manufacturing step of preparing biomass gruel containing an emulsion by immersing palm oil by-products in water and then by friction grinding;

   Liquid extract manufacturing step of preparing a liquid extract containing biomass fine particles and emulsion particles by solid-liquid separation of the biomass gruel obtained in the biomass gruel manufacturing step;

   Coagulant, flocculant or coagulant and flocculant are sequentially added to solidify palm oil emulsion particles containing fat-soluble physiologically active substances in the liquid extract obtained from the liquid extract preparation step. Preparing agglomerates to adsorb / coagulate / aggregate the biomass particles; And

   The method of producing an oil palm biomass solid phase extract, characterized in that it contains a fat-soluble physiologically active substance from palm oil production by-products, including a solid phase extracting step of preparing a solid extract through solid-liquid separation after the flocculation step.
6. The method according to claim 5,

   Friction pulverization of the biomass porridge production step is a method for producing an oil palm biomass solid phase extract, characterized in that using the palm oil emulsification eluting principle from the oil palm biomass.
7. The method according to claim 5,

   Friction pulverization of the biomass gruel manufacturing step is a method for producing an oil palm biomass solid phase extract, characterized in that to use a twin screw extruder (twin screw extruder) to extract the fat-soluble bioactive material from the oil palm biomass.
8. The method according to claim 5,

   Solid-liquid separation in the liquid extract manufacturing step is a method for producing an oil palm biomass solid extract, characterized in that using centrifugal separation or filtration.
9. The method according to claim 5,

   The agglomerate preparation step is an oil palm biomass solid phase, characterized in that using at least one of a cationic, anionic or nonionic polymer including polydicyandiamide and polyacrylamide as a polymer flocculant. Method of Preparation of Extracts.
10. The method according to claim 5,

    Solid-liquid separation in the solid phase extract manufacturing step is a method for producing an oil palm biomass solid phase extract, characterized in that using a pressure filtration method including a filter press or belt press.

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