WO2023182610A1 - Method for mass production of fulvic acid from humus soil - Google Patents

Method for mass production of fulvic acid from humus soil Download PDF

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WO2023182610A1
WO2023182610A1 PCT/KR2022/018813 KR2022018813W WO2023182610A1 WO 2023182610 A1 WO2023182610 A1 WO 2023182610A1 KR 2022018813 W KR2022018813 W KR 2022018813W WO 2023182610 A1 WO2023182610 A1 WO 2023182610A1
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fulvic acid
aqueous solution
extracting
large amount
acid aqueous
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French (fr)
Korean (ko)
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박태철
김홍식
김아람
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주식회사 네오맥스연구소
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    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P17/00Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms
    • C12P17/02Oxygen as only ring hetero atoms
    • C12P17/06Oxygen as only ring hetero atoms containing a six-membered hetero ring, e.g. fluorescein

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  • the present invention relates to a method for mass producing fulvic acid from humus soil, and more specifically, an extraction method for obtaining a large amount of high-quality aqueous fulvic acid solution from humus material using enzymes and a ceramic separator. It's about.
  • Natural humic substances are attracting attention as excellent natural substances that have various pharmacological activities while being significantly effective in improving water quality and fish farm environment. These natural humic substances are formed as a product of erosion of organic substances in the soil. It is usually found in soil, water, sediment, coal, and peat in the natural environment.
  • Natural humic substances are dark-colored, amorphous complexes with a three-dimensional structure, and contain high molecular weight phenolic substances that can chelate metals and inorganic substances. Natural humic substances play an important role in connecting inorganic and organic compounds in the natural environment. It is presumed that this is because the surrounding chains of natural humic substances contain aromatic, hydroxyl, carbonyl, carboxyl, amine, and sulfhydryl groups, and thus have various properties and structures.
  • Natural humic substances which are alkaline aqueous solutions, can be separated into fulvic acid and humic acid due to differences in solubility in acids. Fulvic acid is soluble in acids, but humic acid is insoluble in strong acids.
  • fulvic acid is a low molecular weight acid produced by the action of useful microorganisms as a part of humic substances accumulated in the soil. It has high biological activity, easily combines with minerals and elements in its molecular structure, and has excellent penetration due to its low surface tension. Fulvic acid is rich in minerals and has a strong anti-sulfur antioxidant effect. When savoring fulvic acids, astringent, bitter, and sour tastes are mentioned as characteristic tastes. Meanwhile, fulvic acid is being developed as an ingredient for food, medicine, and cosmetics. There is a problem in that fulvic acid is not easy to purify because it has the property of being soluble in all acidic, neutral, and basic solutions.
  • fulvic acid can generally be purified with high purity through a strong base/strong acid treatment extraction method specified by the International Humic Substances Society (IHSS), an international academic society. Extraction and purification methods (strong base/strong acid treatment methods, etc.) of these fulvic acids are well established in Korea, and these details are detailed in Korean Patent Application Nos. 10-2011-0027154 and 10-2011-0027117. .
  • IHSS International Humic Substances Society
  • fulvic acid extraction uses an alkaline-acid extraction method.
  • humic substances When the humic substances are precipitated using an aqueous solution of sodium hydroxide (NaOH) at pH 13.5 for 4 to 48 hours, they are separated into precipitate and supernatant.
  • the separated supernatant was again acidified to pH 0.5 using hydrochloric acid (HCl) and allowed to precipitate again for about 12 hours. Accordingly, humic acid precipitates, and the supernatant may be composed of fulvic acid.
  • humic substances Humic Substances, or Humus
  • humic substances are formed as the components of dead bodies such as wetlands, swamps, lake bottoms, plants, algae, and seaweed undergo pressure and temperature changes over hundreds to tens of millions of years, causing bacteria, etc. It exists in humus soil created through decomposition/polymerization by microorganisms, and most of it is a collection of organic acids, namely humic acid, fulvic acid, and minerals. Fulvic acid, which exists in smaller amounts among these organic acids, is a humic substance that is highly soluble in water regardless of pH concentration and has a (dark) brown or light blackish brown color.
  • humic acid or fulvic acid can be collected and extracted anywhere where corrosion has progressed to a certain degree, such as water, soil, peat, and sedimentary layers.
  • fulvic acid can be obtained by fermenting tangerines or plants to artificially reproduce the 'humic acid process' and generate humic acid.
  • Fermented, matured, purified various minerals, amino acids, vitamins, enzymes, sulfur, iodine, and chilating fulvic acid complexes present in humic substances have the power to provide energy while maintaining biological balance.
  • scientists who studied the properties of electrolytes in amoeba as animal cells confirmed through experiments that the vitality of cells was revived through these electrolytes, and reported that it was a surprising and beautiful phenomenon.
  • Humic substances are electrolyte mixtures with various organic compound structures, and their chemical molecular structures are not constant because they vary depending on the country's topography and geological environment.
  • Humus has a high affinity for metal ions exposed to the soil environment and forms a humic colloid that acts like a soluble ion exchange material, and the distribution and behavior of metal ions in soil particles and soil water (Migration behavior) ) plays an important role in
  • These humic substances are divided into Fulvic Acid (FA), Humic Acid (HA), and Humin, depending on the difference in molecular weight and solubility depending on pH in aqueous solution. It has very diverse compositions and physical and chemical properties depending on the vegetation, climate, geological characteristics, and soil depth of the area where it was formed.
  • Humic substances are distributed in many countries such as Russia, Canada, the United States, India, China, and Japan, but substances containing a lot of fulvic acid are believed to be mainly distributed in islands and swamps such as the Philippines, Southeast Asia, and Japan.
  • the areas where humic substances are discovered in Korea are Gangneung, Pyeongtaek, the lower reaches of Hallasan Mountain, Goesan, and it is known that humic substances are distributed in geological layers located within 10km from the coastline near the southeastern coast.
  • Humic substances or humus are not only structurally unstable, but are also substances that have existed in water for a considerable period of time without being well decomposed by microorganisms.
  • McCarthy an American corrosive material researcher, commented on the characteristics of corrosive materials that do not decompose easily, saying, 'The structure of the central (nucleus) part that determines the properties of corrosive materials does not change, but the outer structure of the materials undergoes a decomposition process. Because this changes slowly, it takes quite a long time to decompose.'
  • aqueous fulvic acid solution which is a natural substance derived from humic substances and has strong reducing/oxidizing power, through the promoting action of enzymes.
  • the technical problem to be solved by the present invention is to provide a method for extracting a large amount of natural fulvic acid aqueous solution with strong reducing/oxidizing power from corrosive substances.
  • the present invention provides a method for extracting a large amount of natural fulvic acid aqueous solution from humic substances, comprising the following steps:
  • (S2) fermentation by adding at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin to the mixed suspension prepared in (S1);
  • step (S3) First separation and extraction of the supernatant of the fermentation broth fermented in step (S2), removal of sedimented and precipitated corrosive material sludge that has settled on the bottom, and secondary separation using a hydraulic press or centrifuge. Then, extracting and recovering the filtrate from the sludge and combining it with the first extraction supernatant;
  • step (S4) maturing fulvic acid by injecting oxygen-containing bubbles from the ceramic filter membrane of the aerobic tank while maintaining the temperature of the supernatant obtained in step (S3) at 11 to 16°C;
  • step (S5) removing fine residual floating matter from the aged liquid aged in step (S4) using a ceramic separator
  • step (S6) A step of producing fulvic acid by subjecting the aged liquid from which residual suspended matter was removed in step (S5) to antibacterial and sterilization filtration using a ceramic filter of 0.01 to 0.5 ⁇ m.
  • step (S1) 150 to 300 kg of humus soil is added to 500 to 800 L of water.
  • the water in step (S1) is groundwater or purified water.
  • the groundwater or purified water is characterized in that the chlorine component has been removed.
  • the chlorine removal is characterized by using activated carbon or ion exchange resin adsorbent.
  • step (S2) the enzyme is added in an amount of 1,500 to 3,000 mg per 1 kg of humus soil.
  • a ceramic filter of 0.01 to 0.5 ⁇ m is used to generate bubbles of 100 to 200 ⁇ m in size to facilitate oxygen supply.
  • step (S2) the water temperature is maintained at 36-44°C.
  • the supernatant is separated by injecting air from the outside from bottom to top through ultra-fine ceramic pores of 0.01-0.5 ⁇ m to generate ultra-fine oxygen bubbles of 100-200 ⁇ m in the suspension. It is characterized in that the supernatant is separated by inducing corrosive substances in the suspension to float.
  • the process further includes the step of drying the humus sludge remaining after the secondary extraction in step (S3) to produce humus powder with a moisture content of 18 to 22%.
  • the humus powder is used as a rooting agent to help the roots of seedlings grow well in agriculture, as an additive/supplement to antibiotic feed for livestock/livestock, or as a natural antibiotic feed for farmed fish in the fisheries industry.
  • step (S4) the aging process is performed for 70 to 90 days while generating oxygen bubbles.
  • step (S6) antibacterial and sterilizing filtration are performed while stirring the aged liquid.
  • the fulvic acid obtained in step (S6) is further subjected to a low-temperature sterilization process.
  • the pasteurization is characterized by maintaining the temperature of the aqueous solution at 63°C for 30 minutes and then gradually cooling it.
  • the method of extracting fulvic acid from humus soil removes humic substances, which are humus soil, by using at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP, and biotin and a ceramic separator.
  • humic substances which are humus soil
  • at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP, and biotin and a ceramic separator Not only can activation shorten the overall extraction time of fulvic acid, but it also has the advantage of increasing the extraction yield of fulvic acid compared to when the enzyme is not used.
  • fulvic acid in a state with strong reduction-oxidation power (inert) can be obtained without adding any chemical components.
  • the present invention is a material with strong reduction and oxidation power, and has effects such as virus inactivation, antioxidant effect, preservative and deodorizing action, surfactant action, heavy metal dissolution action, and harmful chemical substance dissolution and neutralization action in addition to antibacterial and sterilizing action. It is expected to be very useful as an activator, antioxidant, and supplement in the fields of agriculture, fisheries, and livestock farming.
  • Figure 1 is a water tank diagram showing a method for extracting natural material fulvic acid as one of the embodiments of the present invention, showing the raw material input and dilution step, enzyme addition step, floating material flotation and stirring step, supernatant extraction step, and fulvic acid extraction step.
  • (a) it is a process of floating and agitating suspended matter by installing a ceramic separator and generating bubbles here
  • Figure 2 shows the process in which a suspension is made from humic substances, fermented and aged, and minerals are formed on the surface of the supernatant. Calcium, sulfur, etc. are condensing on the surface of the water tank from the initial stage (a) through the intermediate stage (b) to stage (c). The fermentation process is complete when a dark gray film is formed on the surface of the supernatant, as shown in (c).
  • Figure 3(b) is a photograph showing the surface and vertical section (lower layer of the yellow surface) where minerals and sulfur components (yellow) are clearly revealed as moisture evaporates.
  • Figure 4 shows the process of levitating suspended matter in the supernatant and stirring and maturing, where a white mineral saponin bubble film (a) begins to form thinly on the surface of the water. After a certain period of time, these bubbles begin to gather together (b) and disappear after a gradual disappearance stage (c).
  • a white mineral saponin bubble film (a) begins to form thinly on the surface of the water. After a certain period of time, these bubbles begin to gather together (b) and disappear after a gradual disappearance stage (c).
  • the part that looks like a curved pipe at the bottom or the eaves at the end of a slate roof is a ceramic separator. It shows ultrafine bubbles floating through the pores of the ceramic separator.
  • Figure 5(b) shows ultrafine bubbles floating and combining with floating sediment particles to form a brown suspended particle film (layer) on the water surface, and the side is a transparent polycarbonate tank. This is a photo taken from an angle viewed from above.
  • Figure 6 shows an aqueous solution of fulvic acid (NEOMAX), a natural substance, that was separated and extracted from the supernatant, subjected to final filtration processes, and then placed in a transparent container and a brown container, respectively.
  • NOMAX fulvic acid
  • Figure 7(a) shows the growth of garlic roots grown for more than 3 weeks with fulvic acid (Neomax) stock solution diluted 750:1 to 500:1.
  • Figure 7(b) shows that the roots of garlic were finely developed in all directions as a result of cultivating garlic with the diluted solution.
  • Figure 8(a) shows a dark purple stem obtained by growing 1-year-old ginseng seedlings in hydroponic cultivation for 30 to 35 days with Neomax diluted solution (diluted stock solution 750:1 to 500:1), showing saponin Re. It is ginseng in which the main ingredient is expressed.
  • Figure 8(b) shows ginseng with the main component saponin F1 expressed, forming dark purple stems by diluting fulvic acid Neomax stock solution to 750:1 to 500:1 and growing 5-year-old ginseng seedlings in hydroponics for 45 days. am.
  • Figure 9(a) shows the results obtained by diluting Neomax stock solution from 750:1 to 500:1 and spraying the leaves four times when cultivating sweet potatoes, resulting in mass production of more than 2.5 times the normal harvest amount.
  • Figure 9(b) shows that as a result of hydroponic cultivation of sweet potatoes for a total of 80 days (one month longer than usual), several short and large leaf stems were formed, like potato leaf stems.
  • Figure 9(c) shows that humic material sludge (hereinafter referred to as MM soil), which precipitated during the process of extracting Neomax crude solution, was used for pepper cultivation. 5 g per head of pepper was mixed into the soil and watched as the peppers grew in pesticide-free conditions. As a result, the stems of each pepper grew to an average of more than 2.5 m and reached the ceiling of the greenhouse.
  • MM soil humic material sludge
  • the present invention provides a method for extracting a large amount of natural fulvic acid aqueous solution from humic substances, comprising the following steps:
  • (S2) fermentation by adding at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin to the mixed suspension prepared in (S1);
  • step (S3) First separation and extraction of the supernatant of the fermentation broth fermented in step (S2), removal of sedimented and precipitated corrosive material sludge that has settled on the bottom, and secondary separation using a hydraulic press or centrifuge. Then, extracting and recovering the filtrate from the sludge and combining it with the first extraction supernatant;
  • step (S4) maturing fulvic acid by injecting oxygen-containing bubbles from the ceramic filter membrane of the aerobic tank while maintaining the temperature of the supernatant obtained in step (S3) at 11 to 16°C;
  • step (S5) removing fine residual floating matter from the aged liquid aged in step (S4) using a ceramic separator
  • step (S6) A step of producing fulvic acid as transparent natural drinking water by subjecting the aged liquid from which residual suspended matter has been removed in step (S5) to antibacterial and sterilization filtration using a ceramic filter of 0.01 to 0.5 ⁇ m.
  • fulvic acid a natural substance
  • humic substances can be easily extracted from humic substances through an activated fermentation process using enzymes and a ceramic membrane, and by using a simple, inexpensive ceramic membrane in the manufacturing process, the precipitate is converted into a pure aqueous solution. It is possible to produce in large quantities an aqueous solution of fulvic acid, a natural substance that does not occur at all, has a good water content and has strong reducing and oxidizing power.
  • step (S1) is characterized by adding humus to water to prepare a mixed suspension while maintaining pH 6.0 to 8.0 and temperature 36 to 44 ° C.
  • a ceramic filter membrane with a bubble supply device is installed on the bottom of the water tank containing the suspension.
  • the raw water used for extraction must be purified water from which chlorine has been removed.
  • a common method of removing chlorine components is to use adsorbents such as activated carbon or ion exchange resin. After removing chlorine in this way, the water is allowed to stand at room temperature for 3 to 5 days before proceeding with the next process.
  • step (S2) is fermented by adding one or more enzymes selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin to the mixed suspension prepared above.
  • one or more enzymes selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin to the mixed suspension prepared above.
  • the water temperature in the tank is maintained at 36 to 44°C, preferably 38 to 42°C, more preferably 40°C, so that the enzymes are well activated in the water tank, and the pH is 5.5 to 5.5°C. It is characterized by maintaining it at 7.5. It is advisable to allow a rest period in the fermentation process by drastically lowering the temperature of the workplace and supplying and ventilating fresh air so that the water temperature in the water tank reaches 25-27°C at an appropriate time during the process. Afterwards, the temperature of the water in the water tank is raised to 36 ⁇ 44°C to activate the enzyme again, and the initial working conditions are continuously maintained.
  • the decomposition enzyme in the humus suspension is not activated well, and if the temperature is above 44°C, there is a problem in that the decomposition enzyme is denatured by heat and its activity is reduced.
  • the concentration of the enzyme is usually expressed as the number of enzyme units in 1 ml.
  • the appropriate dosage of enzyme(s) is 1,500 to 3,000 mg per 1 kg of humus soil. It is efficient not to exceed this.
  • humic substances are already mixed with a large amount of various types of naturally occurring microorganisms, such as Bacillus subtilis, photosynthetic bacteria, filamentous bacteria, Bacillus bacteria, algae, yeast, etc.
  • a suspension as a mixture is used. It is not absolutely necessary to add additional microorganisms, etc.
  • a specific enzyme is added, and the enzyme, a type of protein, acts as a catalyst to activate and promote the overall fermentation reaction.
  • Enzyme(s) are generally proteins with a molecular weight of 15,000 to several million Daltons, and catalytic reactions by enzymes have high activity at low temperatures, low pressure, and near neutral pH.
  • reaction temperature and pH have a great influence on the activity of the enzyme.
  • the activity of the enzymes mentioned above usually increases with increasing temperature up to about 40-44°C, but above that, denaturation due to heat occurs and most of them lose their activity.
  • the optimal pH is strongly acidic around 2, such as pepsin that acts in the stomach, but the enzyme activity in the present invention has a neutral pH (5.5 to 7.5), as in the case of most other enzymes. It appears that the vicinity is most suitable for fermentation of humic substances.
  • the above enzyme(s) play a catalyst role in all biochemical reactions involving proteins, metal ions, minerals, amino acids, etc.
  • the activity of the enzyme(s) in humic substances is maximized at 36-44°C, so when the temperature rises beyond this optimal temperature range, the enzyme(s) are denatured by heat and the activity decreases.
  • the enzyme(s) plays the role of a catalyst, lowering the activation energy of the reaction by combining with the substrate to form an enzyme-substrate complex.
  • these substances In order for certain substances to come together and have a chemical reaction, these substances must have enough energy to combine or collide with each other, and the minimum energy required to achieve this state is called the activation energy of the substance. Enzymes lower this activation energy. , promotes chemical reactions within living organisms.
  • step (S3) is to first separate and extract the supernatant of the fermented broth, and remove the sedimented and precipitated corrosive material sludge that has settled on the bottom, using a hydraulic press or After secondary separation using a centrifuge, the filtrate is extracted and recovered from the sludge and combined with the first extraction supernatant.
  • the Solid-Liquid Separation method involves installing a ceramic filter membrane on the bottom of the water tank and allowing air to float from the outside, which allows air from the outside to flow from bottom to top through ultra-fine ceramic pores of 0.01 to 0.5 ⁇ m. This is a method of levitating corrosive substances in the suspension by injecting them and inducing the generation of ultra-fine oxygen bubbles of 100 to 200 ⁇ m in the suspension. If proper agitation is performed during this process, the microorganisms are activated and the desired supernatant can be obtained in a short period of time.
  • the pH value of the suspension was 5.0 to 6.0, but when the extraction progresses as described above and the pH value drops to about 2.3 to 2.9, the primary supernatant from the water tank is transferred to a pump and the supernatant is collected from the ceramic membrane tank.
  • the humus soil (called MM soil, moisture content of 18-22%) made by drying the humus sludge generated at this time is used as an additive to rooting agents in agriculture to help the roots of seedlings grow well, and as an antibiotic for livestock/livestock use.
  • MM soil moisture content of 18-22%
  • step (S4) maintains the temperature of the supernatant obtained in step (S3) at 11 to 16°C and injects oxygen-containing bubbles from the ceramic filter membrane of the aerobic tank to produce fulvic acid. This is the stage of maturing.
  • the supernatant extracted through the primary filtration above is placed in a separate 1-ton capacity water tank with a ceramic filter separator installed on the bottom while maintaining a temperature of 11 to 16°C in a well-ventilated room in the dark. Pour it.
  • step (S5) is a step of removing fine residual suspended matter from the aged liquid by floating it using a ceramic separator.
  • the supernatant is poured into a water tank, and then the separation membrane is operated to supply oxygen bubbles to the supernatant and stirred to ensure proper maturation to float and remove fine insoluble impurities.
  • step (S6) the aged liquid from which residual suspended solids have been removed is subjected to antibacterial and sterilization filtration using a ceramic filter of 0.01 to 0.5 ⁇ m to produce fulvic acid as transparent natural drinking water. This is the step.
  • the fulvic acid solution is aged for 1 to 3 years while maintaining the internal temperature at 8 to 15°C for long-term storage using a warehouse-type underground space, an abandoned mine tunnel, or an unused road tunnel.
  • the natural substance fulvic acid can be obtained by subjecting the fulvic acid aqueous solution that has reached the mature stage to antibacterial and sterilization filtration through a 0.01-0.5 ⁇ m membrane filter.
  • the floating ultrafine bubbles collide with and adhere to the settled/suspended particles (Flocs) in the corrosive material, thereby reducing the specific gravity of the combination between Flocs and bubbles. It floats well on the surface of the water.
  • contaminants are filtered out from the suspension through the pores of an ultra-fine filter of about 0.01 to 0.5 ⁇ m. Once the supernatant is formed, it is aged at a certain temperature for a certain period of time and then the completed fulvic acid is processed. Can be extracted efficiently.
  • the fulvic acid extracted in this way is transferred to a vertical rectangular water tank with two outlet valves attached in a vertical direction at the lower part of the tank.
  • a ceramic filter separator is installed on the bottom of the water tank and air is injected through it to float and remove ultrafine impurities floating in the fulvic acid. Then, the valves mounted on the water tank are sequentially opened from top to bottom. Put it in another container and store it in a cold storage.
  • a low-temperature sterilization process when using the fulvic acid aqueous solution as drinking water, a low-temperature sterilization process is additionally performed.
  • This low temperature long time sterilization (LTLT) is a process in which the temperature of the aqueous solution is first maintained at 63°C for 30 minutes and then gradually cooled.
  • LTLT long time sterilization
  • the air in contact with the solution must be vented out before the process begins.
  • acidity is a major criterion that determines the range of survival of bacterial organisms, and most toxic bacteria are unable to function in strong acid solutions below pH 4.5.
  • Fulvic acid Neomax acts on taste cells to produce an astringent (astringent) taste, and this taste is known to be caused by tannin.
  • Representative tannin components that provide an astringent taste include flavonoids and catechins. These components strengthen human capillaries and are effective in preventing high blood pressure, arteriosclerosis, and stroke.
  • catechin is known to have an antioxidant effect that is more than 50 times higher than that of vitamin C or vitamin E. These antioxidant substances have the function of removing free radicals in the body. Therefore, if you consistently drink fulvic acid, which contains a lot of vitamins, flavonoids, minerals, and amino acids, it is beneficial and effective for physical health and disease prevention, including delaying aging through antioxidants.
  • the fulvic acid produced in the present invention is a dark brown or brown aqueous solution depending on the raw material and its properties, the pH value was 2.2 to 2.8 at 25°C, and the specific gravity was 1.00 to 1.03.
  • E. coli, general bacteria, and heavy metals are not detected in the aqueous solution, and the aqueous solution has a very strong and astringent taste when expressed sensuously and appreciatively, but also has some sweetness.
  • the total solid content in the solution is 0.85 ⁇ 1.25%, of which The content of pure fulvic acid was 0.30-0.55% of the total weight of the aqueous solution.
  • the present invention as a result of a sensory test on the aqueous solution of fulvic acid extracted in the present invention, it is a bright and pale brass-colored aqueous solution that hardly generates any precipitate, and remains in a stable state without any change even when stored for a long period of time. Maintaining.
  • the taste can be described as an aqueous solution of fulvic acid, a natural substance that is soft and refreshing and easy to drink, with a sour taste, an astringent taste, and a subtle sweet taste.
  • a stock solution of fulvic acid aqueous solution named NEOMAX brand name
  • NEOMAX brand name
  • an aqueous solution of fulvic acid consisting only of natural substances was administered to animals as drinking water for 18 to 21 days for the purpose of using it as a livestock feed additive.
  • fulvic acid consisting only of natural substances
  • an aqueous solution of fulvic acid diluted at 750:1 to 500:1 was administered to housed laying hens as drinking water from the beginning, and immediately before laying eggs began, 500:1 to 300: Fulvic acid drinking water was prepared and fed at a dilution ratio of 1. After one month, we carefully observed the movements of the 4,000 chickens being raised in the cage, and found that despite the intrusion of strangers, the chickens not only responded docilely, but even approached people and remained silent for quite some time. Judging by the fact that it was looking at the intruder for a long time, it was found that it was being raised in a comfortable condition without stress.
  • the chickens responded calmly without being agitated, and it was reported that the workers did not notice any unpleasant odors such as excrement while collecting eggs for a long time in the cage. .
  • the shells were thick and there was no fishy smell.
  • the nutrients were vitamin C 8.78mg/kg, tannin 6.22mg/100g, vitamin D3 9,295.35 IU/kg, polyphenol 16.86mg/100g, flavonoid 1.75mg/100g. , a value such as 1.931.11mg/kg of sulfur was confirmed.
  • Neomax fullvic acid aqueous solution
  • a ratio of 750:1 to 500:1 was diluted at a ratio of 750:1 to 500:1, and then supplied as a nutrient to one-year-old ginseng seedlings during hydroponic cultivation for one month. .
  • the stems of 1-year-old ginseng developed into a dark purple color.
  • the stem of ginseng has a light green color during the early growth period.
  • Re the main component of ginseng
  • Neomax when a person drinks Neomax, an aqueous fulvic acid solution, it enters the body and reaches the intestines through the stomach. Due to the action of organic acids present in Neomax, beneficial bacteria increase and harmful bacteria decrease in the intestines, making the intestinal flora sound and healthy. As a result, the odor of stool, etc. is weakened (deodorizing effect) and, depending on the person, the odor component from the blood is reduced, thereby reducing body odor and bad breath.
  • the method of extracting fulvic acid from humus soil removes humic substances, which are humus soil, by using at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP, and biotin and a ceramic separator.
  • humic substances which are humus soil
  • at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP, and biotin and a ceramic separator Not only can activation shorten the overall extraction time of fulvic acid, but it also has the advantage of increasing the extraction yield of fulvic acid compared to when the enzyme is not used.
  • fulvic acid in a strong (inactive) redox state can be obtained without adding any chemical components.
  • the present invention is a material with strong oxidation-reduction power, and has effects such as virus inactivation, antioxidant effect, preservative and deodorizing effect, surfactant activity, heavy metal dissolution effect, and harmful chemical substance dissolution and neutralization effect in addition to antibacterial and sterilizing effect. It is expected to be very useful as an activator, antioxidant, and supplement in the fields of agriculture, fisheries, and livestock farming.

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Abstract

The present invention relates to a method for mass production of fulvic acid from humus soil. A method for extracting fulvic acid from humus soil according to the present invention employs at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP, and biotin, and a ceramic separator to activate humic matter, which is humus, whereby not only can the overall extraction time of fulvic acid be shortened, but also the extraction yield of fulvic acid is higher than when no enzymes are used. In addition, according to the present invention, fulvic acid in a state having a strong redox potential (in an inactive state) can be obtained without adding any chemical components. Therefore, having the effects of virus inactivation, antioxidative action, antiseptic, deodorizing, and anticorrosive action, detergent action, heavy metal dissolution, and harmful chemical substance dissolution and neutralization in addition to antibacterial and sterilizing actions, the fulvic acid with a strong redox potential according to the present invention is expected to be advantageously used as an activator, an antibiotic, and a supplement in the agriculture, fishery, and livestock industries.

Description

부식토로부터 풀빅산을 대량 생산하는 방법Method for mass producing fulvic acid from humus soil
본 발명은 부식토로부터 풀빅산(fulvic acid)을 대량 생산하는 방법에 관한 것으로, 보다 구체적으로는 부식물질(腐植物質)에서 효소와 세라믹 분리막을 이용하여 고품질의 풀빅산 수용액을 대량으로 수득하는 추출방법에 관한 것이다.The present invention relates to a method for mass producing fulvic acid from humus soil, and more specifically, an extraction method for obtaining a large amount of high-quality aqueous fulvic acid solution from humus material using enzymes and a ceramic separator. It's about.
천연 휴믹물질이라 하여 수질환경 및 양어장 환경개선에 상당한 효과를 이루면서도 다양한 약리 활성을 가지는 우수한 천연물질이 각광을 받고 있는데, 이러한 천연 휴믹물질(Natural Humic substance)은 토양에서 유기물질의 침식 생성물로 형성되며, 보통 자연환경의 토양, 물, 퇴적물, 석탄, 이탄 등에서 발견된다.Natural humic substances are attracting attention as excellent natural substances that have various pharmacological activities while being significantly effective in improving water quality and fish farm environment. These natural humic substances are formed as a product of erosion of organic substances in the soil. It is usually found in soil, water, sediment, coal, and peat in the natural environment.
천연 휴믹물질은 진한 색을 가진 3차원 구조의 무정형 복합물로, 금속과 무기물질을 킬레이트 할 수 있는 고분자 페놀 물질을 포함한다. 천연 휴믹 물질은 자연환경에서 무기, 유기 화합물을 연결하는 중요한 역할을 한다. 천연 휴믹 물질의 주변 사슬에 방향족, 하이드록실기, 카르보닐기, 카르복실기, 아민기, 설프히드릴기 등이 포함되어 있어 다양한 성질과 다양한 구조를 갖기 때문이라고 추측된다.Natural humic substances are dark-colored, amorphous complexes with a three-dimensional structure, and contain high molecular weight phenolic substances that can chelate metals and inorganic substances. Natural humic substances play an important role in connecting inorganic and organic compounds in the natural environment. It is presumed that this is because the surrounding chains of natural humic substances contain aromatic, hydroxyl, carbonyl, carboxyl, amine, and sulfhydryl groups, and thus have various properties and structures.
알칼리 수용액인 천연 휴믹 물질은 산에서의 용해성 차이에 의해서 fulvic acid(풀빅산)와 humic acid(휴믹산)로 분리할 수 있다. 풀빅산은 산에서 녹으나 휴믹산은 강산에서 녹지 않는 특성이 있다. Natural humic substances, which are alkaline aqueous solutions, can be separated into fulvic acid and humic acid due to differences in solubility in acids. Fulvic acid is soluble in acids, but humic acid is insoluble in strong acids.
이중에서 풀빅산은 토양에 많이 축적되어 있는 부식물질의 일부로 유용미생물의 작용에 의하여 만들어진 저분자량의 산으로 생물활성이 높고 분자구조 중에 미네랄과 요소와 쉽게 결합하며, 표면장력이 낮아 침투력이 우수하다. 풀빅산은 미네날이 풍부하고 강력한 황항산화 작용이 있으며, 풀빅산들을 음미하면 특징적인 맛들로 떫은맛, 쓴맛, 시큼한 맛들이 언급된다. 한편 풀빅산은 식품 의약품이나 화장품 원료들로 개발되고 있다. 풀빅산은 산성 용액, 중성 용액 및 염기서 용액에서 모두 용해되는 특성이 있기 때문에 정제하는 것이 쉽지 않다는 문제가 있다.Among them, fulvic acid is a low molecular weight acid produced by the action of useful microorganisms as a part of humic substances accumulated in the soil. It has high biological activity, easily combines with minerals and elements in its molecular structure, and has excellent penetration due to its low surface tension. Fulvic acid is rich in minerals and has a strong anti-sulfur antioxidant effect. When savoring fulvic acids, astringent, bitter, and sour tastes are mentioned as characteristic tastes. Meanwhile, fulvic acid is being developed as an ingredient for food, medicine, and cosmetics. There is a problem in that fulvic acid is not easy to purify because it has the property of being soluble in all acidic, neutral, and basic solutions.
그러나 풀빅산은 일반적으로 국제적인 학회인 International Humic Substances Society (IHSS, 국제부식학회)에서 정한 강염기/강산 처리 추출법을 통해서 고순도의 정제물을 얻을 수 있다. 국내에서도 이러한 풀빅산의 추출 및 정제방법(강염기/강산 처리법 등)이 잘 정립되어 있으며, 이러한 내용은 대한민국 특허 출원번호 제10-2011-0027154호, 제10-2011-0027117호 등에 자세히 수록되어 있다.However, fulvic acid can generally be purified with high purity through a strong base/strong acid treatment extraction method specified by the International Humic Substances Society (IHSS), an international academic society. Extraction and purification methods (strong base/strong acid treatment methods, etc.) of these fulvic acids are well established in Korea, and these details are detailed in Korean Patent Application Nos. 10-2011-0027154 and 10-2011-0027117. .
종래의 풀빅산 추출은 알칼리-산성 추출법을 사용한다. 부식물질을 pH 13.5의 수산화나트륨(NaOH) 수용액을 이용하여 4 내지 48시간 동안 침전시키면, 침전물과 상층액으로 분리된다. 분리된 상층액을 다시 염산(HCl)을 사용하여 pH 0.5로 산성화시키고, 다시 약 12시간 동안 침전시킨다. 그에 따라 휴믹산은 침전되고, 상층액은 풀빅산으로 구성될 수 있다.Conventional fulvic acid extraction uses an alkaline-acid extraction method. When the humic substances are precipitated using an aqueous solution of sodium hydroxide (NaOH) at pH 13.5 for 4 to 48 hours, they are separated into precipitate and supernatant. The separated supernatant was again acidified to pH 0.5 using hydrochloric acid (HCl) and allowed to precipitate again for about 12 hours. Accordingly, humic acid precipitates, and the supernatant may be composed of fulvic acid.
한편, 부식물질(腐植物質, Humic Substances, or Humus)은 습지, 늪지, 호수바닥면, 식물, 조류, 해조류 등의 사체 구성요소들이 수억~수천만 년에 걸쳐 압력 및 온도변화를 겪으면서, 세균 등 미생물 작용에 의한 분해/중합작용을 거쳐 생성된 부식 토양에 존재하는데, 그 대부분은 유기산들 즉, 휴믹산(Humic acid)과 풀빅산(Fulvic acid) 그리고 미네랄들의 집합체이다. 이들 유기산들 중에서 보다 적게 존재하는 풀빅산(Fulvic acid)은 pH 농도와 관계없이 물에 잘 용해되는 부식물질이며 (짙은) 갈색이나 옅은 흑갈색을 띄고 있다. 또한 이러한 부식물질은 조성되는 과정 중에 이미 천문학적 숫자의 미생물들에 의하여 분해가 되어져 있는 상태이다. 이와 같이 천연의 휴믹산이나 풀빅산은 물, 흙, 이탄, 퇴적층 등 부식이 어느 정도 진행된 곳에서는 어디서나 채취하고 추출할 수 있다. 또한 귤이나 식물 등을 발효시켜 인공적으로 '부식화 과정'을 재현하면서 부식산을 발생시켜 풀빅산을 얻을 수도 있다.On the other hand, humic substances (Humic Substances, or Humus) are formed as the components of dead bodies such as wetlands, swamps, lake bottoms, plants, algae, and seaweed undergo pressure and temperature changes over hundreds to tens of millions of years, causing bacteria, etc. It exists in humus soil created through decomposition/polymerization by microorganisms, and most of it is a collection of organic acids, namely humic acid, fulvic acid, and minerals. Fulvic acid, which exists in smaller amounts among these organic acids, is a humic substance that is highly soluble in water regardless of pH concentration and has a (dark) brown or light blackish brown color. Additionally, these corrosive substances have already been decomposed by an astronomical number of microorganisms during the process of their composition. In this way, natural humic acid or fulvic acid can be collected and extracted anywhere where corrosion has progressed to a certain degree, such as water, soil, peat, and sedimentary layers. In addition, fulvic acid can be obtained by fermenting tangerines or plants to artificially reproduce the 'humic acid process' and generate humic acid.
부식물질 안에 존재하는 발효 숙성 정제된 다양한 미네랄들, 아미노산, 비타민, 효소, 유황, 요오드 성분들과 Chilating(착화) 되어있는 풀빅산 복합체들은 생물학적 균형을 유지하면서, 에너지를 공여할 수 있는 힘을 가진, 세상에서 가장 정교하게 만들어진 천연의 유기 전해질(powerful organic electrolytes)들이다. 동물세포로서 아메바를 대상으로 전해질이 가진 특성을 연구했던 과학자들은, 실험을 통하여 이러한 전해질을 통해 세포의 생명력이 되살아난 현상을 확인하고, 놀랍고 아름다운 현상이라고 보고하였다.Fermented, matured, purified various minerals, amino acids, vitamins, enzymes, sulfur, iodine, and chilating fulvic acid complexes present in humic substances have the power to provide energy while maintaining biological balance. , are the world's most sophisticated natural organic electrolytes (powerful organic electrolytes). Scientists who studied the properties of electrolytes in amoeba as animal cells confirmed through experiments that the vitality of cells was revived through these electrolytes, and reported that it was a surprising and beautiful phenomenon.
부식물질은 이렇듯 다양한 유기화합물 구조를 갖는 전해질 혼합물로서, 그 나라 지형 및 지질 환경에 따라 차이가 생기기 때문에 그의 화학적 분자구조는 일정하지 않다. 부식토는 토양 환경에 노출된 금속 이온들에 대해 높은 친화력을 가지고 가용성의 이온교환물질처럼 행동하는 휴믹 콜로이드(colloid)를 형성하며, 토양입자와 토양수 내에서의 금속이온의 분포와 거동(Migration behavior)에 중요한 역할을 한다. 이러한 휴믹물질은 그 자체가 갖는 분자량의 차이, 그리고 수용액에서의 pH에 따른 용해도 차이에 따라 풀빅산(Fulvic Acid: FA), 휴믹산(Humic Acid: HA), 및 휴민(Humin) 등으로 나뉘며, 토양이 형성된 지역의 식생, 기후, 지질특성이나 토양층의 깊이 등에 따라 매우 다양한 조성(compositions)과 물리화학적 특성을 지닌다. 휴믹물질들은 러시아, 캐나다, 미국, 인도, 중국, 일본 등 여러 국가에 분포되어 있으나 풀빅산이 많이 함유된 물질들은 주로 필리핀, 동남아, 일본 등 도서 지역이나 늪지에 주로 분포되어 있는 것으로 파악되고 있다. 국내의 휴믹물질 발견 지역은 강릉, 평택, 한라산 하류, 괴산, 그리고 서남해안 인근 해안선에서 10Km 이내에 위치한 지질층에 휴믹물질이 분포하는 것으로 알려져 있다.Humic substances are electrolyte mixtures with various organic compound structures, and their chemical molecular structures are not constant because they vary depending on the country's topography and geological environment. Humus has a high affinity for metal ions exposed to the soil environment and forms a humic colloid that acts like a soluble ion exchange material, and the distribution and behavior of metal ions in soil particles and soil water (Migration behavior) ) plays an important role in These humic substances are divided into Fulvic Acid (FA), Humic Acid (HA), and Humin, depending on the difference in molecular weight and solubility depending on pH in aqueous solution. It has very diverse compositions and physical and chemical properties depending on the vegetation, climate, geological characteristics, and soil depth of the area where it was formed. Humic substances are distributed in many countries such as Russia, Canada, the United States, India, China, and Japan, but substances containing a lot of fulvic acid are believed to be mainly distributed in islands and swamps such as the Philippines, Southeast Asia, and Japan. The areas where humic substances are discovered in Korea are Gangneung, Pyeongtaek, the lower reaches of Hallasan Mountain, Goesan, and it is known that humic substances are distributed in geological layers located within 10km from the coastline near the southwestern coast.
부식(휴믹)물질 또는 부식토는 구조적으로 그 자체가 불안정할 뿐 아니라 미생물에 의해서 잘 분해되지 않은 상태로 상당히 오랜 기간 물 속에 존재하였던 물질이다. 미국의 부식물질 연구자인 매카시는 이와 같이 잘 분해되지 않는 부식물질의 성격에 대해 '부식물질의 성질을 결정짓는 중심(핵) 부분의 구조는 변함이 없으나, 분해과정을 통하여 그 물질들의 바깥쪽 조직이 서서히 변화되기 때문에, 분해되는데 상당히 오랜 시간이 소요된다'라는 가설을 주장하였다. Humic substances or humus are not only structurally unstable, but are also substances that have existed in water for a considerable period of time without being well decomposed by microorganisms. McCarthy, an American corrosive material researcher, commented on the characteristics of corrosive materials that do not decompose easily, saying, 'The structure of the central (nucleus) part that determines the properties of corrosive materials does not change, but the outer structure of the materials undergoes a decomposition process. Because this changes slowly, it takes quite a long time to decompose.'
이에 본 발명자들은 효소의 촉진작용을 통해 부식물질에서 유래된 천연물질로 환원/산화력이 강한 풀빅산 수용액을 대량으로 추출함으로써 본 발명을 완성하였다.Accordingly, the present inventors completed the present invention by extracting a large amount of aqueous fulvic acid solution, which is a natural substance derived from humic substances and has strong reducing/oxidizing power, through the promoting action of enzymes.
본 발명에서 해결하고자 하는 기술적 과제는 부식물질로부터 환원/산화력이 강한 천연 풀빅산 수용액을 대량으로 추출하는 방법을 제공하기 위한 것이다.The technical problem to be solved by the present invention is to provide a method for extracting a large amount of natural fulvic acid aqueous solution with strong reducing/oxidizing power from corrosive substances.
상기한 기술적 과제를 해결하기 위하여, 본 발명에서는 하기 단계를 포함하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법을 제공한다:In order to solve the above technical problems, the present invention provides a method for extracting a large amount of natural fulvic acid aqueous solution from humic substances, comprising the following steps:
(S1) 부식토를 물에 첨가하여 pH 6.0~8.0 및 온도 36~44℃를 유지시키면서 혼합 현탁액을 제조하는 단계; (S1) adding humus to water to prepare a mixed suspension while maintaining pH 6.0-8.0 and temperature 36-44°C;
(S2) 상기 (S1)에서 제조된 혼합 현탁액에 NAD, NADP, FAD, CoA, ATP, GTP, TPP 및 비오틴으로 이루어진 군에서 선택된 하나 이상의 효소를 첨가하여 발효시키는 단계;(S2) fermentation by adding at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin to the mixed suspension prepared in (S1);
(S3) 상기 단계 (S2)에서 발효시킨 발효액의 상등액을 1차 분리 추출하고, 바닥면에 가라앉은 침강 및 침전상태의 부식물질 슬러지(Sludge)를 걷어내어 유압기 또는 원심분리기를 이용하여 2차 분리한 다음 그 슬러지에서 여액을 추출 및 회수하여 상기 1차 추출 상등액과 합치는 단계;(S3) First separation and extraction of the supernatant of the fermentation broth fermented in step (S2), removal of sedimented and precipitated corrosive material sludge that has settled on the bottom, and secondary separation using a hydraulic press or centrifuge. Then, extracting and recovering the filtrate from the sludge and combining it with the first extraction supernatant;
(S4) 상기 단계 (S3)에서 수득된 상등액의 온도를 11~16℃로 유지하면서 호기조의 세라믹 필터 분리막으로부터 산소가 들어있는 기포를 주입시켜 풀빅산을 숙성시키는 단계;(S4) maturing fulvic acid by injecting oxygen-containing bubbles from the ceramic filter membrane of the aerobic tank while maintaining the temperature of the supernatant obtained in step (S3) at 11 to 16°C;
(S5) 상기 단계 (S4)에서 숙성된 숙성액을 세라믹 분리막을 이용하여 미세 잔류 부유물을 부상시켜 제거하는 단계; 및(S5) removing fine residual floating matter from the aged liquid aged in step (S4) using a ceramic separator; and
(S6) 상기 단계 (S5)에서 잔류 부유물을 제거한 숙성액을 0.01~0.5μm의 세라믹 필터를 사용하여 항균 및 멸균여과를 실시하여 풀빅산을 생산하는 단계.(S6) A step of producing fulvic acid by subjecting the aged liquid from which residual suspended matter was removed in step (S5) to antibacterial and sterilization filtration using a ceramic filter of 0.01 to 0.5 μm.
바람직하게, 상기 단계 (S1)에서 물 500~800 L에 대하여 부식토 150~300 kg을 넣는 것을 특징으로 한다.Preferably, in step (S1), 150 to 300 kg of humus soil is added to 500 to 800 L of water.
바람직하게, 상기 단계 (S1)에서 물은 지하수 또는 정제수인 것을 특징으로 한다.Preferably, the water in step (S1) is groundwater or purified water.
상기 지하수 또는 정제수는 염소 성분이 제거된 것임을 특징으로 한다.The groundwater or purified water is characterized in that the chlorine component has been removed.
상기 염소 제거는 활성탄 또는 이온교환수지 흡착제를 사용하는 것을 특징으로 한다.The chlorine removal is characterized by using activated carbon or ion exchange resin adsorbent.
바람직하게, 상기 단계 (S2)에서 효소는 부식토 1Kg당 1,500~3,000 mg의 양으로 첨가하는 것을 특징으로 한다.Preferably, in step (S2), the enzyme is added in an amount of 1,500 to 3,000 mg per 1 kg of humus soil.
바람직하게, 상기 단계 (S2)에서 세라믹 필터 0.01~0.5㎛ 분리막을 이용하여 100~200㎛ 크기의 기포를 발생시켜 산소공급을 원활하게 하는 것을 특징으로 한다.Preferably, in the step (S2), a ceramic filter of 0.01 to 0.5 μm is used to generate bubbles of 100 to 200 μm in size to facilitate oxygen supply.
바람직하게, 상기 단계 (S2)에서 수온을 36~44℃ 상태로 유지하는 것을 특징으로 한다.Preferably, in step (S2), the water temperature is maintained at 36-44°C.
바람직하게, 상기 단계 (S3)에서 상등액 분리는 0.01~0.5㎛의 초미세한 세라믹 기공을 통해 외부로부터 공기를 아래에서 윗방향으로 주입시킴으로써 현탁액 속에서 100~200㎛의 초미세한 산소 기포를 발생시키도록 유도시켜 현탁액 수중의 부식물질들을 부상시킴으로써 상등액을 분리시키는 것을 특징으로 한다.Preferably, in step (S3), the supernatant is separated by injecting air from the outside from bottom to top through ultra-fine ceramic pores of 0.01-0.5 ㎛ to generate ultra-fine oxygen bubbles of 100-200 ㎛ in the suspension. It is characterized in that the supernatant is separated by inducing corrosive substances in the suspension to float.
바람직하게, 상기 단계 (S3)에서 2차 추출이 진행된 후에 남은 부식물 슬러지를 건조하여 수분함량 18~22%의 부식토 분말을 제조하는 단계를 추가로 포함하는 것을 특징으로 한다.Preferably, the process further includes the step of drying the humus sludge remaining after the secondary extraction in step (S3) to produce humus powder with a moisture content of 18 to 22%.
상기 부식토 분말은 농업에서 모종의 뿌리가 잘 자라도록 돕는 발근제, 축산/가축용으로는 항생제 사료의 첨가/보조제, 또는 수산업에서 양식 어류의 천연 항생제 사료용으로 사용하는 것을 특징으로 한다.The humus powder is used as a rooting agent to help the roots of seedlings grow well in agriculture, as an additive/supplement to antibiotic feed for livestock/livestock, or as a natural antibiotic feed for farmed fish in the fisheries industry.
바람직하게, 상기 단계 (S4)에서 산소 기포를 발생시키면서 70~90일 동안 숙성공정을 진행하는 것을 특징으로 한다.Preferably, in step (S4), the aging process is performed for 70 to 90 days while generating oxygen bubbles.
바람직하게, 상기 단계 (S6)에서 숙성액을 교반시키면서 항균 및 멸균여과를 수행하는 것을 특징으로 한다.Preferably, in step (S6), antibacterial and sterilizing filtration are performed while stirring the aged liquid.
바람직하게, 상기 단계 (S6)에서 수득된 풀빅산을 저온살균공정을 추가로 실시하는 것을 특징으로 한다.Preferably, the fulvic acid obtained in step (S6) is further subjected to a low-temperature sterilization process.
상기 저온살균은 수용액의 온도를 63℃에서 30분 유지시킨 다음 서서히 냉각시키는 것을 특징으로 한다.The pasteurization is characterized by maintaining the temperature of the aqueous solution at 63°C for 30 minutes and then gradually cooling it.
이와 같이, 본 발명에 따른 부식토로부터 풀빅산을 추출하는 방법은 NAD, NADP, FAD, CoA, ATP, GTP, TPP 및 비오틴으로 이루어진 군에서 선택된 하나 이상의 효소 및 세라믹 분리막을 사용함으로써 부식토인 부식물질을 활성화시켜 풀빅산의 전체적인 추출시간을 단축시킬 수 있을 뿐만 아니라 효소를 사용하지 않았을 때보다 풀빅산의 추출 수율이 더욱 높아지는 이점이 있다. 또한, 본 발명에 따르면 환원 산화력이 강한(불활성의) 상태의 풀빅산을 일체의 화학성분의 첨가없이 수득할 수 있다. 따라서, 본 발명에 따르면 환원 산화력이 강한 물질로서 항균 및 살균 작용 외에도 바이러스 불활화 작용, 항산화 작용, 방부 방취 방식작용, 계면활성작용, 중금속 용해작용, 유해화학물질 용해 및 중화작용 등의 효과를 가지는 바, 농업, 수산업, 축산업 분야에서 활성제, 항상제, 보조제로 매우 유용하게 사용될 수 있을 것으로 기대된다. As such, the method of extracting fulvic acid from humus soil according to the present invention removes humic substances, which are humus soil, by using at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP, and biotin and a ceramic separator. Not only can activation shorten the overall extraction time of fulvic acid, but it also has the advantage of increasing the extraction yield of fulvic acid compared to when the enzyme is not used. In addition, according to the present invention, fulvic acid in a state with strong reduction-oxidation power (inert) can be obtained without adding any chemical components. Therefore, according to the present invention, it is a material with strong reduction and oxidation power, and has effects such as virus inactivation, antioxidant effect, preservative and deodorizing action, surfactant action, heavy metal dissolution action, and harmful chemical substance dissolution and neutralization action in addition to antibacterial and sterilizing action. It is expected to be very useful as an activator, antioxidant, and supplement in the fields of agriculture, fisheries, and livestock farming.
본 명세서에 첨부되는 다음의 도면들은 본 발명의 바람직한 실시예를 예시하는 것이며, 전술한 발명의 내용과 함께 본 발명의 기술사상을 더욱 이해시키는 역할을 하는 것이므로, 본 발명은 그러한 도면에 기재된 사항에만 한정되어 해석되어서는 아니 된다.The following drawings attached to this specification illustrate preferred embodiments of the present invention, and serve to further understand the technical idea of the present invention along with the contents of the above-described invention. Therefore, the present invention is limited to the matters described in such drawings. It should not be interpreted in a limited way.
도 1은 본 발명의 실시예 중 하나로 천연물질 풀빅산 추출방법을 도시한 수조그림으로, 원료투입 및 희석단계, 효소제 첨가단계, 부유물 부상 및 교반단계, 상등액 추출단계, 풀빅산 추출단계를 보여준다. 여기에서, (a) 세라믹 분리막을 장착하고, 여기에 기포를 발생시킴으로 부유물의 부상 및 교반하는 공정이고, (b) Drain 꼭지를 위 중간 밑에서부터 아래 순서로 틀어 천연물 풀빅산을 추출하는 공정의 개념도이다. Figure 1 is a water tank diagram showing a method for extracting natural material fulvic acid as one of the embodiments of the present invention, showing the raw material input and dilution step, enzyme addition step, floating material flotation and stirring step, supernatant extraction step, and fulvic acid extraction step. Here, (a) it is a process of floating and agitating suspended matter by installing a ceramic separator and generating bubbles here, and (b) a conceptual diagram of the process of extracting natural product fulvic acid by turning the drain tap in the order from the bottom of the top to the bottom. am.
도 2는 부식물질로부터 현탁액이 만들어지고 발효 숙성되어 상등액의 표면에 미네랄들이 형성되는 과정을 보여준다. 초기단계 (a)에서 중간단계인 (b)과정을 지나 (c)단계까지 수조 표면에 칼슘, 유황 등이 응집되어 가고 있다. (c)와 같이 상등액의 표면에 짙은 회색의 막이 생성되면 발효공정이 완료된 것이다. Figure 2 shows the process in which a suspension is made from humic substances, fermented and aged, and minerals are formed on the surface of the supernatant. Calcium, sulfur, etc. are condensing on the surface of the water tank from the initial stage (a) through the intermediate stage (b) to stage (c). The fermentation process is complete when a dark gray film is formed on the surface of the supernatant, as shown in (c).
도 3(a)는 현택액이 발효 숙성된 다음 그대로 정치(定置)시키면, 도 2의 (c)에서 형성된 미네랄 막의 미립자 부유물들이 하부로 침강된다. 이어서 상등액을 추출해 낸 다음, 수조 바닥에 쌓인 슬러지의 표면을 촬영한 사진이다. 수분이 많이 포함되어 진갈색을 띄고 있다. In Figure 3(a), when the suspension is left to stand after fermentation and maturation, the suspended fine particles of the mineral film formed in Figure 2(c) settle to the bottom. This is a photo taken of the surface of the sludge accumulated on the bottom of the tank after extracting the supernatant. It contains a lot of moisture and is dark brown in color.
도 3(b)는 수분이 증발함에 따라, 미네랄 및 유황성분(황색)이 뚜렷하게 드러난 표면과 수직단면(황색 표면의 하부층)을 보여주는 사진이다.Figure 3(b) is a photograph showing the surface and vertical section (lower layer of the yellow surface) where minerals and sulfur components (yellow) are clearly revealed as moisture evaporates.
도 3(c)는 표면의 황색은 수분이 거의 증발함에 따라, 밝은 노란색으로 변하였고, 짙은 회색의 하부 수직층도 건조가 진행되면서 회색으로 밝아졌다.In Figure 3(c), the yellow surface changed to bright yellow as most of the moisture evaporated, and the dark gray lower vertical layer also became light gray as drying progressed.
도 4는 상등액에서 부유물을 부상시키고 교반 숙성하는 공정으로, 표면 위에 하얀 미네랄 사포닌 거품막(a)이 수면에 전체적으로 엷게 형성되기 시작하는 모습이다. 일정 시간 경과 후 이 거품은 서로 모이기 시작하면서(b), 서서히 소멸되어가는 단계(c)를 지나 없어진다. Figure 4 shows the process of levitating suspended matter in the supernatant and stirring and maturing, where a white mineral saponin bubble film (a) begins to form thinly on the surface of the water. After a certain period of time, these bubbles begin to gather together (b) and disappear after a gradual disappearance stage (c).
도 5(a)는 아래부분에 굴곡이 있는 파이프(pipe) 또는 슬레이트 지붕 끝 처마같이 보이는 부분이 세라믹 분리막이다. 세라믹 분리막 기공을 통해서 초미세 기포가 부상하는 모습을 보여준다. In Figure 5(a), the part that looks like a curved pipe at the bottom or the eaves at the end of a slate roof is a ceramic separator. It shows ultrafine bubbles floating through the pores of the ceramic separator.
도 5(b)는 초미세 기포가 부상하면서, 부유하고 있던 침전입자와 결합, 수면 위로 갈색의 부유입자 막(층)을 형성한 모습이며 옆면은 투명한 폴리카보네이트 수조이다. 위에서 비스듬히 내려다 본 각도의 사진이다. Figure 5(b) shows ultrafine bubbles floating and combining with floating sediment particles to form a brown suspended particle film (layer) on the water surface, and the side is a transparent polycarbonate tank. This is a photo taken from an angle viewed from above.
도 6은 상등액을 분리 추출하여 최종 여과공정들을 진행한 다음 각각 투명용기와 갈색용기에 담은, 천연물질인 풀빅산 수용액(네오맥스, NEOMAX)의 모습이다.Figure 6 shows an aqueous solution of fulvic acid (NEOMAX), a natural substance, that was separated and extracted from the supernatant, subjected to final filtration processes, and then placed in a transparent container and a brown container, respectively.
도 7(a)는 풀빅산(네오맥스) 원액을 750:1~500:1로 희석하여 3주 이상 재배한 마늘 뿌리의 성장한 모습이다.Figure 7(a) shows the growth of garlic roots grown for more than 3 weeks with fulvic acid (Neomax) stock solution diluted 750:1 to 500:1.
도 7(b)는 상기 희석액으로 마늘을 재배한 결과 그 뿌리가 사방으로 미세하게 잘 발달된 모습이다. Figure 7(b) shows that the roots of garlic were finely developed in all directions as a result of cultivating garlic with the diluted solution.
도 7(c)는 마늘 뿌리 (b)를 확대하여 자세히 살펴보면, 뿌리의 끝부분 외에도 중간의 부분 부분에 갈색의 점과 같이 색깔이 다른 부분이 보이는데, 이곳에 있는 세포들을 통해 영양분이 흡수되는 것으로 보인다. In Figure 7(c), if you zoom in and look closely at the garlic root (b), you can see parts of different colors, such as brown dots, in the middle of the root in addition to the tip of the root. This indicates that nutrients are absorbed through the cells there. see.
도 8(a)는 네오맥스 희석액(원액을 750:1~500:1로 희석)으로 묘삼 1년근을 30~35일간 수경재배로 성장시켜 얻은, 짙은 자색의 줄기대를 갖는 모습으로, 사포닌 Re 주성분이 발현된 인삼이다. Figure 8(a) shows a dark purple stem obtained by growing 1-year-old ginseng seedlings in hydroponic cultivation for 30 to 35 days with Neomax diluted solution (diluted stock solution 750:1 to 500:1), showing saponin Re. It is ginseng in which the main ingredient is expressed.
도 8(b)는 풀빅산 네오맥스 원액을 750:1~500:1로 희석하여 5년근 묘삼을 45일 동안 수경재배로 성장시켜 짙은 자색 줄기대를 형성한 사포닌 F1 주성분이 발현된 인삼의 모습이다.Figure 8(b) shows ginseng with the main component saponin F1 expressed, forming dark purple stems by diluting fulvic acid Neomax stock solution to 750:1 to 500:1 and growing 5-year-old ginseng seedlings in hydroponics for 45 days. am.
도 9(a)는 고구마를 재배할 때 네오맥스 원액을 750:1~500:1로 희석시켜 4회 엽면살포하여 얻은 결과로서, 일반적인 수확량의 2.5배 이상의 대량 생산된 결과이다.Figure 9(a) shows the results obtained by diluting Neomax stock solution from 750:1 to 500:1 and spraying the leaves four times when cultivating sweet potatoes, resulting in mass production of more than 2.5 times the normal harvest amount.
도 9(b)는 고구마를 총 80일 동안 수경재배(보통보다 1개월 더 경과)한 결과, 마치 감자의 잎줄기처럼 짧고 크게 여러 개가 형성되어진 모습이다.Figure 9(b) shows that as a result of hydroponic cultivation of sweet potatoes for a total of 80 days (one month longer than usual), several short and large leaf stems were formed, like potato leaf stems.
도 9(c)는 네오맥스 원액을 추출하는 과정에서 침전된, 부식물질 슬러지[이하 MM토(土)라고 칭함]를, 고추 재배에 사용하였다. 고추 1포기당 5 g을 토양에 섞어 투입하여, 무농약 상태에서 고추가 성장하도록 지켜 본 결과, 고추 각 포기의 줄기가 평균 2.5m 이상으로 성장하여 비닐하우스 천정에 닿은 모습이다.Figure 9(c) shows that humic material sludge (hereinafter referred to as MM soil), which precipitated during the process of extracting Neomax crude solution, was used for pepper cultivation. 5 g per head of pepper was mixed into the soil and watched as the peppers grew in pesticide-free conditions. As a result, the stems of each pepper grew to an average of more than 2.5 m and reached the ceiling of the greenhouse.
이하 본 발명을 좀 더 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명에서는 하기 단계를 포함하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법을 제공한다:The present invention provides a method for extracting a large amount of natural fulvic acid aqueous solution from humic substances, comprising the following steps:
(S1) 부식토를 물에 첨가하여 pH 6.0~8.0 및 온도 36~44℃를 유지시키면서 혼합 현탁액을 제조하는 단계; (S1) adding humus to water to prepare a mixed suspension while maintaining pH 6.0-8.0 and temperature 36-44°C;
(S2) 상기 (S1)에서 제조된 혼합 현탁액에 NAD, NADP, FAD, CoA, ATP, GTP, TPP 및 비오틴으로 이루어진 군에서 선택된 하나 이상의 효소를 첨가하여 발효시키는 단계;(S2) fermentation by adding at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin to the mixed suspension prepared in (S1);
(S3) 상기 단계 (S2)에서 발효시킨 발효액의 상등액을 1차 분리 추출하고, 바닥면에 가라앉은 침강 및 침전상태의 부식물질 슬러지(Sludge)를 걷어내어 유압기 또는 원심분리기를 이용하여 2차 분리한 다음 그 슬러지에서 여액을 추출 및 회수하여 상기 1차 추출 상등액과 합치는 단계;(S3) First separation and extraction of the supernatant of the fermentation broth fermented in step (S2), removal of sedimented and precipitated corrosive material sludge that has settled on the bottom, and secondary separation using a hydraulic press or centrifuge. Then, extracting and recovering the filtrate from the sludge and combining it with the first extraction supernatant;
(S4) 상기 단계 (S3)에서 수득된 상등액의 온도를 11~16℃로 유지하면서 호기조의 세라믹 필터 분리막으로부터 산소가 들어있는 기포를 주입시켜 풀빅산을 숙성시키는 단계;(S4) maturing fulvic acid by injecting oxygen-containing bubbles from the ceramic filter membrane of the aerobic tank while maintaining the temperature of the supernatant obtained in step (S3) at 11 to 16°C;
(S5) 상기 단계 (S4)에서 숙성된 숙성액을 세라믹 분리막을 이용하여 미세 잔류 부유물을 부상시켜 제거하는 단계; 및(S5) removing fine residual floating matter from the aged liquid aged in step (S4) using a ceramic separator; and
(S6) 상기 단계 (S5)에서 잔류 부유물을 제거한 숙성액을 0.01~0.5μm의 세라믹 필터를 사용하여 항균 및 멸균여과를 실시하여 투명한 천연의 음용수로서의 풀빅산을 생산하는 단계.(S6) A step of producing fulvic acid as transparent natural drinking water by subjecting the aged liquid from which residual suspended matter has been removed in step (S5) to antibacterial and sterilization filtration using a ceramic filter of 0.01 to 0.5 μm.
본 발명에 의하면, 효소와 세라믹 분리막을 이용한 활성화 발효공정을 통해 부식물질에서 천연물질인 풀빅산을 용이하게 추출할 수 있으며, 제조 공정에 있어서도 가격이 저렴한 간단한 세라믹 분리막을 이용함으로써, 순수한 수용액으로 침전물이 전혀 발생하지 않는, 함수율이 좋으면서 환원 산화력이 강한 천연물질 풀빅산 수용액을 대량으로 생산할 수 있다.According to the present invention, fulvic acid, a natural substance, can be easily extracted from humic substances through an activated fermentation process using enzymes and a ceramic membrane, and by using a simple, inexpensive ceramic membrane in the manufacturing process, the precipitate is converted into a pure aqueous solution. It is possible to produce in large quantities an aqueous solution of fulvic acid, a natural substance that does not occur at all, has a good water content and has strong reducing and oxidizing power.
본 발명의 풀빅산을 생산하는 방법에서 단계 (S1)은 부식토를 물에 첨가하여 pH 6.0~8.0 및 온도 36~44℃를 유지시키면서 혼합 현탁액을 제조하는 것을 특징으로 한다.In the method for producing fulvic acid of the present invention, step (S1) is characterized by adding humus to water to prepare a mixed suspension while maintaining pH 6.0 to 8.0 and temperature 36 to 44 ° C.
상기 풀빅산 추출방법으로, 먼저 현탁액을 담는 수조탱크 바닥면에 기포공급 장치가 있는 세라믹 필터 분리막을 설치한다. 여기에 지하수나 정제된 물(pH 6.0~8.0)을 수조탱크(1톤 용량)에 500~800L 정도 붓는다. 사용되는 추출용 원수는 어떠한 경우에도 염소성분이 제거된 정제수를 사용해야 한다. 염소 성분을 제거하는 방법으로는 활성탄이나 이온교환수지 등의 흡착제를 사용하는 것이 보통이다. 이와 같은 방법으로 염소를 제거한 다음, 그 물을 상온에서 3~5일 정도 정치시킨 후에 다음 공정을 진행한다. In the fulvic acid extraction method, first, a ceramic filter membrane with a bubble supply device is installed on the bottom of the water tank containing the suspension. Here, pour about 500 to 800 L of groundwater or purified water (pH 6.0 to 8.0) into the water tank (1 ton capacity). In all cases, the raw water used for extraction must be purified water from which chlorine has been removed. A common method of removing chlorine components is to use adsorbents such as activated carbon or ion exchange resin. After removing chlorine in this way, the water is allowed to stand at room temperature for 3 to 5 days before proceeding with the next process.
상기와 같이 만들어진 물을 수조에 500~800L 정도 채운 다음, 부식토 150~300kg을 천천히 수조의 물에 투여한다. 실내 작업장의 온도는 작업장 바닥면에서부터 1.5m 위의 공간에서 측정하고, 그 실내 온도가 35~45℃를 유지하도록 한다.After filling about 500 to 800 L of water prepared as above into the tank, slowly add 150 to 300 kg of humus soil to the water in the tank. The temperature of the indoor workplace is measured in a space 1.5m above the workshop floor, and the indoor temperature is maintained at 35-45℃.
본 발명의 풀빅산을 생산하는 방법에서 단계 (S2)는 상기에서 제조된 혼합 현탁액에 NAD, NADP, FAD, CoA, ATP, GTP, TPP 및 비오틴으로 이루어진 군에서 선택된 하나 이상의 효소를 첨가하여 발효시키는 단계로서, 세라믹 필터 0.01~0.5㎛ 분리막을 이용하여 100~200㎛ 크기의 기포를 발생시켜 산소공급을 원활하게 하는 한편, 부유물을 부상시켜 1일 4~5시간씩 3주 동안 간헐적으로 교반한 다음에 13~15일 정도 정치(定置)하면서 미립자 부유물을 완전히 침강시킨다. 세라믹 필터 분리막으로부터 미세한 기포를 발생시켜 상기 현탁액을 교반 부상시킴으로 호기성 산소공급이 원활하도록 하여 발효를 촉진시키는 것을 특징으로 한다.In the method for producing fulvic acid of the present invention, step (S2) is fermented by adding one or more enzymes selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin to the mixed suspension prepared above. As a step, using a 0.01-0.5㎛ ceramic filter membrane to generate bubbles of 100-200㎛ in size to facilitate oxygen supply, float the suspended matter and stir intermittently for 4-5 hours a day for 3 weeks. Let stand for 13 to 15 days to completely settle suspended fine particles. It is characterized in that it generates fine bubbles from the ceramic filter membrane and stirs and levitates the suspension to facilitate aerobic oxygen supply and promote fermentation.
상기 1개 이상의 효소를 첨가한 다음, 수조안에서 효소가 잘 활성화되도록 탱크 내의 수온은 36~44℃, 바람직하게는 38~42℃, 더 바람직하게는 40℃의 온도로 유지시키고, pH는 5.5~7.5로 유지시키는 것을 특징으로 한다. 공정 중 적절한 시기에 수조의 수온이 25~27℃로 도달하도록 작업장 온도를 급격히 낮추면서 신선한 공기를 공급하며 환기하여, 발효공정에 휴식기를 두는 것이 바람직하다. 이후 다시 효소가 활성화되도록 수조탱크 물의 온도를 36~44℃가 되도록 올려 처음의 작업조건을 지속적으로 유지시킨다. After adding the one or more enzymes, the water temperature in the tank is maintained at 36 to 44°C, preferably 38 to 42°C, more preferably 40°C, so that the enzymes are well activated in the water tank, and the pH is 5.5 to 5.5°C. It is characterized by maintaining it at 7.5. It is advisable to allow a rest period in the fermentation process by drastically lowering the temperature of the workplace and supplying and ventilating fresh air so that the water temperature in the water tank reaches 25-27℃ at an appropriate time during the process. Afterwards, the temperature of the water in the water tank is raised to 36~44℃ to activate the enzyme again, and the initial working conditions are continuously maintained.
상기 온도가 36℃ 미만이면 부식토 현탁액에서의 분해효소가 잘 활성화되지 않으며, 상기 온도가 44℃가 넘으면 분해효소가 열에 의해 변성하여 활성이 감소되는 문제점이 있다. If the temperature is less than 36°C, the decomposition enzyme in the humus suspension is not activated well, and if the temperature is above 44°C, there is a problem in that the decomposition enzyme is denatured by heat and its activity is reduced.
효소의 농도는 액체의 경우 통상 1㎖ 중의 효소의 단위수로서 표시되는데, 본 발명과 같이 고체 효소(들)을 사용하는 경우 효소(들)의 투입량은 부식토 1Kg당 1,500~3,000 mg이 적합하며, 이를 초과하지 않는 것이 효율적이다.In the case of liquids, the concentration of the enzyme is usually expressed as the number of enzyme units in 1 ml. When solid enzyme(s) are used as in the present invention, the appropriate dosage of enzyme(s) is 1,500 to 3,000 mg per 1 kg of humus soil. It is efficient not to exceed this.
상기의 부식물질에는 자연적으로 잔재(殘在)하는 다종의 미생물들, 예를 들어 고초균, 광합성균, 사상균, 바실러스균, 조류, 효모 등이 이미 다량으로 혼재(混在)되어 있기 때문에, 혼합물인 현탁액에 별도의 미생물 등을 추가로 투입하는 것이 꼭 필요한 사항은 아니다. 그러나 현탁액을 발효시켜 그의 상등액으로부터 풀빅산을 보다 효율적으로 추출하기 위하여, 특정 효소를 첨가하면 단백질의 일종인 그 효소가 전체적인 발효 반응을 활성화하고 촉진하는 촉매제 역할을 수행한다.Since the above humic substances are already mixed with a large amount of various types of naturally occurring microorganisms, such as Bacillus subtilis, photosynthetic bacteria, filamentous bacteria, Bacillus bacteria, algae, yeast, etc., a suspension as a mixture is used. It is not absolutely necessary to add additional microorganisms, etc. However, in order to more efficiently extract fulvic acid from the supernatant by fermenting the suspension, a specific enzyme is added, and the enzyme, a type of protein, acts as a catalyst to activate and promote the overall fermentation reaction.
상기의 나열한 효소들 중에서 1개 이상을 선택하여 현탁액에 첨가하면 대부분의 효소(들)은, 기질의 농도에 따라서 촉매작용의 속도를 다양하게 변화시킨다. 효소(들)은 일반적으로 15,000~수백만 돌턴(Dolton)의 분자량을 갖는 단백질이며, 효소에 의한 촉매반응은 중간 이하의 온도, 낮은 압력, 중성에 가까운 pH 상태에서 그의 활성도가 높다.When one or more of the enzymes listed above is selected and added to the suspension, most enzyme(s) vary the speed of catalysis depending on the concentration of the substrate. Enzyme(s) are generally proteins with a molecular weight of 15,000 to several million Daltons, and catalytic reactions by enzymes have high activity at low temperatures, low pressure, and near neutral pH.
이때 반응 온도와 pH는 효소의 활성에 큰 영향을 미친다. 온천지대에서 발견되는 내열성 미생물 등의 예외가 있기는 하지만, 상기에서 언급되는 효소의 경우 대개 40~44℃ 정도까지는 온도증가에 따라 활성이 증가하지만 그 이상에서는 열에 의한 변성이 일어나서 대부분 활성을 잃어버린다. 또한 위(Stomach)에서 작용하는 펩신(Pepsin)처럼 최적의 pH가 2 정도의 강산성인 경우도 있으나, 본 발명에서의 효소활성은 대부분의 다른 효소들의 경우와 같이, pH가 중성(5.5~7.5) 부근일 때가 부식물질의 발효에 가장 적합한 것으로 나타난다.At this time, reaction temperature and pH have a great influence on the activity of the enzyme. Although there are exceptions such as heat-resistant microorganisms found in hot spring areas, the activity of the enzymes mentioned above usually increases with increasing temperature up to about 40-44℃, but above that, denaturation due to heat occurs and most of them lose their activity. In addition, there are cases where the optimal pH is strongly acidic around 2, such as pepsin that acts in the stomach, but the enzyme activity in the present invention has a neutral pH (5.5 to 7.5), as in the case of most other enzymes. It appears that the vicinity is most suitable for fermentation of humic substances.
상기의 효소(들)은 단백질, 금속이온, 미네랄, 아미노산 등이 관여하는 모든 생화학 반응에서 촉매 역할을 담당한다. 부식물질에서 효소(들)의 활성도는 36~44℃에서 극대화되므로, 이와 같은 최적온도 범위를 넘어 온도가 상승하면 효소(들)가 열에 의해 변성되므로 활성이 오히려 감소한다.The above enzyme(s) play a catalyst role in all biochemical reactions involving proteins, metal ions, minerals, amino acids, etc. The activity of the enzyme(s) in humic substances is maximized at 36-44℃, so when the temperature rises beyond this optimal temperature range, the enzyme(s) are denatured by heat and the activity decreases.
상기 효소(들)는 기질과 결합하여 효소-기질 복합체(Enzyme-Substrate Complex)를 형성함으로써 반응의 활성화 에너지(Activation Energy)를 낮추는, 촉매의 역할을 담당하고 있다. 어떤 물질들이 모여서 화학반응을 하려면 이 물질들이 서로 결합하거나 충돌할 만큼의 에너지를 가져야 하고, 이런 상태가 되기 위한 최소한의 필요 에너지를 그 물질의 활성화 에너지라고 하는데, 효소는 이와 같은 활성화 에너지를 낮추어 줌으로써, 생물체 내의 화학반응을 촉진시킨다.The enzyme(s) plays the role of a catalyst, lowering the activation energy of the reaction by combining with the substrate to form an enzyme-substrate complex. In order for certain substances to come together and have a chemical reaction, these substances must have enough energy to combine or collide with each other, and the minimum energy required to achieve this state is called the activation energy of the substance. Enzymes lower this activation energy. , promotes chemical reactions within living organisms.
본 발명의 풀빅산을 생산하는 방법에서 단계 (S3)은 상기에서 발효시킨 발효액의 상등액을 1차 분리 추출하고, 바닥면에 가라앉은 침강 및 침전상태의 부식물질 슬러지(Sludge)를 걷어내어 유압기 또는 원심분리기를 이용하여 2차 분리한 다음 그 슬러지에서 여액을 추출 및 회수하여 상기 1차 추출 상등액과 합치는 단계이다.In the method for producing fulvic acid of the present invention, step (S3) is to first separate and extract the supernatant of the fermented broth, and remove the sedimented and precipitated corrosive material sludge that has settled on the bottom, using a hydraulic press or After secondary separation using a centrifuge, the filtrate is extracted and recovered from the sludge and combined with the first extraction supernatant.
상기 공정에서 세라믹 필터 분리막을 수조탱크 바닥면에 설치하여 외부로부터 공기를 유입하여 부상시키는 Solid-Liquid Separation 방법은, 0.01~0.5㎛의 초미세한 세라믹 기공을 통해, 외부로부터 공기를 아래에서 윗방향으로 주입시켜, 그 현탁액 속에서 100~200㎛의 초미세한 산소 기포를 발생시키도록 유도함으로써 현탁액 수중의 부식물질들을 부상시키는 방법이다. 이 과정 중에 적절한 교반이 이루어지면 미생물들이 활성화되어 짧은 기간에 원하는 상등액을 얻을 수 있다. In the above process, the Solid-Liquid Separation method involves installing a ceramic filter membrane on the bottom of the water tank and allowing air to float from the outside, which allows air from the outside to flow from bottom to top through ultra-fine ceramic pores of 0.01 to 0.5 ㎛. This is a method of levitating corrosive substances in the suspension by injecting them and inducing the generation of ultra-fine oxygen bubbles of 100 to 200㎛ in the suspension. If proper agitation is performed during this process, the microorganisms are activated and the desired supernatant can be obtained in a short period of time.
수조탱크에 설치된 세라믹필터 분리막을 통해 기포를 공급하면서, 교반 및 부유물 부상의 과정을 1일 4~5시간씩, 3~5회 정도 시행하기를 총 20~30일간 지속적으로 반복하며 이 상태를 유지시킨다. 이와 같이 교반과 현탁액 부상 공정을 반복적으로 시행하면서 상등액(上澄液)을 관찰하여 보면, 수표면에 짙은 암갈색이 나타나기 시작했다가 이어서 상등액의 표면 위에 미네랄 성분인 회색 막이 형성되면서, 용액의 pH 값이 2.3~2.9로 떨어지게 된다. 이 때가 1차 공정의 완숙단계로서 산화/환원 포텐셜(ORP: Oxidation Reduction Potential) 수치는 500~700mV 범위 내가 된다. While supplying air bubbles through the ceramic filter separator installed in the water tank, the process of stirring and levitating suspended matter is repeated 3 to 5 times for 4 to 5 hours a day, and this state is maintained for a total of 20 to 30 days. I order it. When observing the supernatant while repeatedly performing the stirring and suspension flotation process, a dark brown color begins to appear on the water surface, and then a gray film, which is a mineral component, is formed on the surface of the supernatant, and the pH value of the solution increases. This drops to 2.3~2.9. This is the mature stage of the first process, and the Oxidation Reduction Potential (ORP) value is in the range of 500 to 700 mV.
추출공정 초기에는 현탁액의 pH 값은 5.0~6.0 이었으나 상기와 같이 추출이 진행되어 pH 값이 2.3~2.9 정도로 떨어지면, 수조탱크의 1차 상등액을 펌프로 이송하면서 세라믹 분리막 탱크로부터 옮겨 상등액을 채취한다. At the beginning of the extraction process, the pH value of the suspension was 5.0 to 6.0, but when the extraction progresses as described above and the pH value drops to about 2.3 to 2.9, the primary supernatant from the water tank is transferred to a pump and the supernatant is collected from the ceramic membrane tank.
이어서, 상등액을 채취하고 나면 바닥면에 침전된 슬러지(Sludge)가 남는데, 이를 2차적으로 유압식 착유기나, 통돌이 세탁기 형태의 원심분리기로 착유하여 함유된 수용액을 추출해 낸다. 이와 같이 침강 슬러지에서 2차 추출이 진행된 후에 남은 부식물 슬러지의 수분함량은 26~35% 정도이다.Next, after the supernatant is collected, sludge that settles on the bottom remains. This is secondarily extracted using a hydraulic oil pump or a centrifugal separator in the form of a barrel washing machine to extract the aqueous solution contained therein. In this way, the moisture content of the remaining corrosive sludge after secondary extraction from the settled sludge is approximately 26 to 35%.
이때 발생한 부식물 슬러지를 건조하여 분말로 만든 부식토(MM土라고 칭하며 수분함량은 18~22%)는, 농업에서 모종의 뿌리가 잘 자라도록 돕는 발근제의 첨가제로 사용되고, 축산/가축용으로는 항생제 사료의 첨가/보조제로, 수산업에서는 양식 어류의 천연 항생제 사료용으로 사용할 수 있다.The humus soil (called MM soil, moisture content of 18-22%) made by drying the humus sludge generated at this time is used as an additive to rooting agents in agriculture to help the roots of seedlings grow well, and as an antibiotic for livestock/livestock use. As an additive/supplement to feed, it can be used in the fisheries industry as a natural antibiotic feed for farmed fish.
본 발명의 풀빅산을 생산하는 방법에서 단계 (S4)는 상기 단계 (S3)에서 수득된 상등액의 온도를 11~16℃로 유지하면서 호기조의 세라믹 필터 분리막으로부터 산소가 들어있는 기포를 주입시켜 풀빅산을 숙성시키는 단계이다.In the method for producing fulvic acid of the present invention, step (S4) maintains the temperature of the supernatant obtained in step (S3) at 11 to 16°C and injects oxygen-containing bubbles from the ceramic filter membrane of the aerobic tank to produce fulvic acid. This is the stage of maturing.
상기에서 1차 여과되어 추출된 상등액은 음암(陰暗) 상태로 통풍이 잘되는 실내에서, 온도 11~16℃를 유지하면서 세라믹 필터 분리막을 바닥면에 설치한 별도의 1톤 용량의 수조탱크에 상등액을 붓는다.The supernatant extracted through the primary filtration above is placed in a separate 1-ton capacity water tank with a ceramic filter separator installed on the bottom while maintaining a temperature of 11 to 16°C in a well-ventilated room in the dark. Pour it.
본 발명의 풀빅산을 생산하는 방법에서 단계 (S5)는 상기에서 숙성된 숙성액을 세라믹 분리막을 이용하여 미세 잔류 부유물을 부상시켜 제거하는 단계이다.In the method for producing fulvic acid of the present invention, step (S5) is a step of removing fine residual suspended matter from the aged liquid by floating it using a ceramic separator.
상기 상등액을 수조탱크에 부은 다음 분리막을 작동시켜 상등액에 산소기포를 공급하면서 숙성이 잘 진행되도록 교반하여 미세한 불용성 불순물을 부상시켜 제거한다.The supernatant is poured into a water tank, and then the separation membrane is operated to supply oxygen bubbles to the supernatant and stirred to ensure proper maturation to float and remove fine insoluble impurities.
상기 상등액의 상부표면에 단백질 미네랄 막이 형성이 되기까지 세라믹 필터 분리막으로 초미세한 산소 기포를 발생시키면서 70~90일 동안 숙성공정을 진행하게 되면, 상등액의 표면에 밝은 막이 형성되었다가 소멸된다. When the aging process is carried out for 70 to 90 days while generating ultra-fine oxygen bubbles with a ceramic filter separator until a protein-mineral film is formed on the upper surface of the supernatant, a bright film is formed on the surface of the supernatant and then disappears.
본 발명의 풀빅산을 생산하는 방법에서 단계 (S6)는 상기에서 잔류 부유물을 제거한 숙성액을 0.01~0.5㎛의 세라믹 필터를 사용하여 항균 및 멸균여과를 실시하여 투명한 천연의 음용수로서의 풀빅산을 생산하는 단계이다.In the method for producing fulvic acid of the present invention, in step (S6), the aged liquid from which residual suspended solids have been removed is subjected to antibacterial and sterilization filtration using a ceramic filter of 0.01 to 0.5 ㎛ to produce fulvic acid as transparent natural drinking water. This is the step.
숙성 마지막 단계로서 상기 풀빅산 용액은 창고형 지하공간 또는 폐광산 터널, 또는 사용되지 않는 도로터널 등을 이용하여 장기간 보관목적으로 내부의 온도를 8~15℃로 유지하면서 1~3년 동안 숙성시킨 후, 완숙단계에 도달된 도달한 풀빅산 수용액을 0.01~0.5㎛의 멤브레인 필터로 항균 및 멸균 여과를 실시하여 천연물질 풀빅산을 수득할 수 있다. As the final stage of maturation, the fulvic acid solution is aged for 1 to 3 years while maintaining the internal temperature at 8 to 15°C for long-term storage using a warehouse-type underground space, an abandoned mine tunnel, or an unused road tunnel. , the natural substance fulvic acid can be obtained by subjecting the fulvic acid aqueous solution that has reached the mature stage to antibacterial and sterilization filtration through a 0.01-0.5㎛ membrane filter.
상기 세라믹 필터 분리막을 통해 현탁액에 공기를 주입시키면, 부상하던 초미세 기포가 부식물질 안에 있던 침전/부유 입자(Flocs)들과 충돌·부착하게 되어 Floc들과 기포들과의 결합체 비중을 작게 만듦으로 수면 위로 잘 떠오르게 한다. 또한 교반을 진행하면서 0.01~0.5㎛ 정도의 초미세한 필터의 공경(Pore)을 통해 현탁액으로부터 오염물질을 걸러내는 과정을 통해서 상등액이 형성되면, 일정 기간, 일정 온도에서 숙성시킨 다음 완성된 풀빅산을 효율적으로 추출할 수 있다. When air is injected into the suspension through the ceramic filter separator, the floating ultrafine bubbles collide with and adhere to the settled/suspended particles (Flocs) in the corrosive material, thereby reducing the specific gravity of the combination between Flocs and bubbles. It floats well on the surface of the water. In addition, while stirring, contaminants are filtered out from the suspension through the pores of an ultra-fine filter of about 0.01 to 0.5 ㎛. Once the supernatant is formed, it is aged at a certain temperature for a certain period of time and then the completed fulvic acid is processed. Can be extracted efficiently.
이렇게 추출한 풀빅산을 출수 밸브 두개가 중간 밑의 하부면 위치에 수직 방향으로 부착된 수직형 직사각형태의 수조탱크로 이송한다. 이 수조탱크의 바닥면에 세라믹 필터 분리막을 장착하고 이를 통해 공기를 주입시켜 풀빅산에 부유하는 초미세한 불순물들을 부상시켜 제거하고 난 후, 수조탱크에 장착된 밸브들을 위에서부터 아래로 순차적으로 개방하여 다른 용기에 넣어 저온으로 유지되는 저장고에 보관한다.The fulvic acid extracted in this way is transferred to a vertical rectangular water tank with two outlet valves attached in a vertical direction at the lower part of the tank. A ceramic filter separator is installed on the bottom of the water tank and air is injected through it to float and remove ultrafine impurities floating in the fulvic acid. Then, the valves mounted on the water tank are sequentially opened from top to bottom. Put it in another container and store it in a cold storage.
본 발명의 하나의 구현 예에 따르면, 상기 풀빅산 수용액을 음용수로 사용할 경우에는 저온살균공정을 추가로 실시한다. 이와 같은 저온 장시간 살균(LTLT; Low Temperature Long Time)은, 먼저 수용액의 온도를 63℃에서 30분 유지시킨 다음에 서서히 냉각시키는 공정이다. 주의할 사항으로 저온 살균공정은, 공정시작 전에 용액과 접촉되어 있는 공기를 반드시 밖으로 배출해야 한다는 것이다. 일반적으로 산도(Acidity)는 세균 유기체의 생존의 범위를 결정짓는 주요 잣대인데, 대부분의 독성 세균들은 pH 4.5 이하의 강산의 용액에서는 활동하지 못한다. According to one embodiment of the present invention, when using the fulvic acid aqueous solution as drinking water, a low-temperature sterilization process is additionally performed. This low temperature long time sterilization (LTLT) is a process in which the temperature of the aqueous solution is first maintained at 63°C for 30 minutes and then gradually cooled. One thing to note is that in the low-temperature sterilization process, the air in contact with the solution must be vented out before the process begins. In general, acidity is a major criterion that determines the range of survival of bacterial organisms, and most toxic bacteria are unable to function in strong acid solutions below pH 4.5.
풀빅산 네오맥스는 미각세포에 작용하여 수렴성(떫은 맛)을 느끼게 하는데, 이러한 맛은 탄닌에 의한 것으로 알려져 있다. 떫은 맛을 제공하는 탄닌 성분은 플라보노이드류, 카테킨류 등이 대표적인데, 이 성분들은 인간의 모세혈관을 튼튼하게 만들어주고 고혈압과 동맥경화, 뇌졸증 등을 예방하는 효과를 보인다. 이들 탄닌성분 중 카테킨은 항산화 효과가 비타민C나 비타민E에 비해 50배 이상 높은 것으로 알려져 있는데, 이들 항산화 물질들은 체내의 활성산소를 제거하는 기능을 갖는다. 따라서 비타민, 플라보노이드류, 미네랄, 아미노산 등이 많이 들어 있는 풀빅산을 꾸준히 음용하면, 항산화에 의한 노화지연 등 신체건강 및 질병의 예방에 유익하고 효과적이다.Fulvic acid Neomax acts on taste cells to produce an astringent (astringent) taste, and this taste is known to be caused by tannin. Representative tannin components that provide an astringent taste include flavonoids and catechins. These components strengthen human capillaries and are effective in preventing high blood pressure, arteriosclerosis, and stroke. Among these tannin ingredients, catechin is known to have an antioxidant effect that is more than 50 times higher than that of vitamin C or vitamin E. These antioxidant substances have the function of removing free radicals in the body. Therefore, if you consistently drink fulvic acid, which contains a lot of vitamins, flavonoids, minerals, and amino acids, it is beneficial and effective for physical health and disease prevention, including delaying aging through antioxidants.
본 발명에서 제조된 풀빅산은 원료와 그의 성상에 따라서 암갈색 또는 갈색을 가지는 수용액이며, pH 값은 25℃에서 2.2~2.8, 비중은 1.00~1.03이었다. 또한, 수용액에서는 대장균과 일반세균, 그리고 중금속이 검출되지 않으며, 그 수용액은 감각적, 감상적으로 그 맛을 표현할 때 신맛이 매우 강하고 떫은 맛이 있는 반면 일부 단맛도 가진다. 용액 속의 고형분의 총 함량은 0.85~1.25%, 그 중 순수한 풀빅산의 함유량은 수용액 전체 중량의 0.30~0.55%였다.The fulvic acid produced in the present invention is a dark brown or brown aqueous solution depending on the raw material and its properties, the pH value was 2.2 to 2.8 at 25°C, and the specific gravity was 1.00 to 1.03. In addition, E. coli, general bacteria, and heavy metals are not detected in the aqueous solution, and the aqueous solution has a very strong and astringent taste when expressed sensuously and appreciatively, but also has some sweetness. The total solid content in the solution is 0.85~1.25%, of which The content of pure fulvic acid was 0.30-0.55% of the total weight of the aqueous solution.
본 발명의 하나의 구현예에 따르면, 본 발명에서 추출된 풀빅산 수용액에 대한 관능시험 결과, 밝고 엷은 황동색의 수용액으로서 침전물은 거의 발생하지 않으며, 장기적으로 보관하여도 어떠한 변화가 없이 안정된 상태를 유지하고 있다. According to one embodiment of the present invention, as a result of a sensory test on the aqueous solution of fulvic acid extracted in the present invention, it is a bright and pale brass-colored aqueous solution that hardly generates any precipitate, and remains in a stable state without any change even when stored for a long period of time. Maintaining.
또한, 음용하기에 그 맛은 시큼한 맛, 떫은 맛, 미세한 단 맛을 가진 부드럽고 상큼하여 마시기 좋은 천연물질의 풀빅산 수용액이라고 묘사할 수 있다.In addition, the taste can be described as an aqueous solution of fulvic acid, a natural substance that is soft and refreshing and easy to drink, with a sour taste, an astringent taste, and a subtle sweet taste.
본 발명의 하나의 구현예에 따르면, 비교를 위해 네오맥스(NEOMAX, 상품명)라고 명명된 풀빅산 수용액 원액을 0.2~0.3% 인삼 효소 발효액에 첨가하여 발효시킨 결과, 기존에 통상 3주 정도 소요되었던 발효기간이 7일 정도에서 발효가 완료가 되는 것을 확인하였다. 또한 맥주발효 공정에서의 경우는 발효 기간이 기존 공정보다 45일 이상이 단축됨을 보였다. According to one embodiment of the present invention, for comparison, a stock solution of fulvic acid aqueous solution named NEOMAX (brand name) was added to 0.2-0.3% ginseng enzyme fermentation broth and fermented, resulting in fermentation, which normally took about 3 weeks. It was confirmed that fermentation was completed in about 7 days. Additionally, in the case of the beer fermentation process, the fermentation period was shown to be shorter by more than 45 days compared to the existing process.
본 발명의 하나의 구현예에 따르면, 항생제 내성문제에 대한 대안 중 하나로서 천연물질로만 이루어진 풀빅산 수용액을 가축사료 첨가제로 사용할 목적 하에 음용수로 동물들에게 18~21일 동안 투여하여 보았다. 그 결과 닭이나 반려동물의 털이 윤기가 나고 행동이 온순해지고, 특별히 분변에서 발생하는 악취가 매우 효과적으로 경감되었음을 관찰할 수 있었다. According to one embodiment of the present invention, as an alternative to the antibiotic resistance problem, an aqueous solution of fulvic acid consisting only of natural substances was administered to animals as drinking water for 18 to 21 days for the purpose of using it as a livestock feed additive. As a result, it was observed that the fur of chickens and pets became shiny, their behavior became docile, and the foul odor generated from feces was reduced very effectively.
본 발명의 하나의 구현예에 따르면, 입식된 산란계 닭들에게 초기부터 750:1~500:1로 희석된 풀빅산 수용액을 음용수로 투여하기 시작하였고, 산란이 시작되기 직전부터는 500:1~300:1의 희석비로 풀빅산 음용수를 만들어 먹였다. 이후 1개월 경과 후에 계사에 진입하여 사육 중인 닭 4천마리의 동태(動態)를 주의 깊게 살펴본 결과, 낯선 사람들의 침입에도 불구하고 닭들은 온순하게 반응하였을 뿐 아니라 오히려 사람 앞으로 다가와서 조용히 침묵한 상태로 상당 시간동안 침입자를 바라보고 있는 것으로 보아, 스트레스 없이 편안한 상태로 사육되고 있는 것으로 파악되었다. According to one embodiment of the present invention, an aqueous solution of fulvic acid diluted at 750:1 to 500:1 was administered to housed laying hens as drinking water from the beginning, and immediately before laying eggs began, 500:1 to 300: Fulvic acid drinking water was prepared and fed at a dilution ratio of 1. After one month, we carefully observed the movements of the 4,000 chickens being raised in the cage, and found that despite the intrusion of strangers, the chickens not only responded docilely, but even approached people and remained silent for quite some time. Judging by the fact that it was looking at the intruder for a long time, it was found that it was being raised in a comfortable condition without stress.
본 발명의 하나의 구현예에 따르면, 계란을 수거하기 위한 활동이 진행되어도 닭들은 동요 없이 얌전히 반응하였으며, 계사 안에서 작업자가 장시간 계란 수거활동을 하는 동안에 분뇨 등의 거북한 냄새를 크게 느끼지 못했다고 보고하였다. 산란된 계란들을 관찰하여 보면, 난각이 두껍고 비릿한 냄새가 나지 않았다. 충남대학교 농업기술센터에 계란의 성분분석을 의뢰한 결과 영양성분으로서, 비타민C 8.78mg/kg, 탄닌 6.22mg/100g, 비타민D3 9,295.35 IU/kg, 폴리페놀 16.86mg/100g, 플라보노이드 1.75mg/100g, 황 1.931.11mg/kg과 같은 수치를 확인할 수 있었다. According to one embodiment of the present invention, even when the activity to collect eggs was carried out, the chickens responded calmly without being agitated, and it was reported that the workers did not notice any unpleasant odors such as excrement while collecting eggs for a long time in the cage. . When observing the laid eggs, the shells were thick and there was no fishy smell. As a result of requesting the Chungnam National University Agricultural Technology Center to analyze the composition of eggs, the nutrients were vitamin C 8.78mg/kg, tannin 6.22mg/100g, vitamin D3 9,295.35 IU/kg, polyphenol 16.86mg/100g, flavonoid 1.75mg/100g. , a value such as 1.931.11mg/kg of sulfur was confirmed.
본 발명의 하나의 구현예에 따르면, 네오맥스 (풀빅산 수용액)를 750:1~500:1의 비율로 희석한 다음, 인삼 1년근 묘삼을 1개월 동안 수경 재배하는 과정에 영양제로 공급하여 주었다. 재배 시작 30일 경과 후, 1년근 인삼의 줄기대의 상태는 짙은 자색으로 발달되었다. (일반적으로 인삼의 줄기대는 초기 성장기에 옅은 녹색을 띤다) 일반적으로 5년근 이상 된 열매에서는 성분검사 결과로 인삼의 주성분인 Re가 30%~35% 정도 나타난다고 알려져 있으나, 본 발명의 경우 1년근 묘삼을 1개월 동안 수경재배한 다음 수삼상태로 한국식품 과학연구원에 성분분석 의뢰한 결과, Re 성분이 50.3%, 즉 주성분으로 존재함을 확인할 수 있었다.According to one embodiment of the present invention, Neomax (fulvic acid aqueous solution) was diluted at a ratio of 750:1 to 500:1, and then supplied as a nutrient to one-year-old ginseng seedlings during hydroponic cultivation for one month. . 30 days after the start of cultivation, the stems of 1-year-old ginseng developed into a dark purple color. (Generally, the stem of ginseng has a light green color during the early growth period.) It is generally known that 30% to 35% of Re, the main component of ginseng, is found in fruits older than 5 years old as a result of component tests, but in the case of the present invention, 1-year-old roots are used. As a result of cultivating ginseng seedlings hydroponically for one month and then requesting a composition analysis in fresh ginseng form from the Korea Research Institute of Food Science, it was confirmed that Re was present at 50.3%, that is, as the main ingredient.
본 발명의 하나의 구현예에 따르면, 풀빅산 수용액인 네오맥스를 사람이 음용하게 되면, 체내에 들어가 위를 거쳐 장에 도달하게 된다. 네오맥스에 존재하는 유기산의 작용에 의하여서 장에서 유익균이 증가하고 유해균이 감소함으로, 장내 세균총(細菌叢)이 건전하고 건강한 상태가 된다. 그 결과 변 등의 냄새가 약해지고(방취 효과) 나아가서는 사람에 따라 혈액에서 나는 냄새 성분이 줄어들기 때문에 체취·구취가 경감되는 효과가 나타난다. 장내 세균총이 건전해지면 그 결과로서 장의 기능도 연쇄적으로 활발해져서 섭취된 음식으로부터 영양 흡수효율이 향상되고, 변비개선, 숙취경감 등의 효과가 나타난다는 음용 체험자의 공통적인 보고를 확인할 수 있었다.According to one embodiment of the present invention, when a person drinks Neomax, an aqueous fulvic acid solution, it enters the body and reaches the intestines through the stomach. Due to the action of organic acids present in Neomax, beneficial bacteria increase and harmful bacteria decrease in the intestines, making the intestinal flora sound and healthy. As a result, the odor of stool, etc. is weakened (deodorizing effect) and, depending on the person, the odor component from the blood is reduced, thereby reducing body odor and bad breath. We were able to confirm common reports from drinkers that when the intestinal flora becomes healthy, the intestinal function becomes more active in a chain, improving the efficiency of nutrient absorption from ingested food, improving constipation, and reducing hangovers.
이와 같이, 본 발명에 따른 부식토로부터 풀빅산을 추출하는 방법은 NAD, NADP, FAD, CoA, ATP, GTP, TPP 및 비오틴으로 이루어진 군에서 선택된 하나 이상의 효소 및 세라믹 분리막을 사용함으로써 부식토인 부식물질을 활성화시켜 풀빅산의 전체적인 추출시간을 단축시킬 수 있을 뿐만 아니라 효소를 사용하지 않았을 때보다 풀빅산의 추출 수율이 더욱 높아지는 이점이 있다. 또한, 본 발명에 따르면 산화환원력이 강한(불활성의) 상태의 풀빅산을 일체의 화학성분의 첨가없이 수득할 수 있다. 따라서, 본 발명에 따르면 산화환원력이 강한 물질로서 항균 및 살균 작용 외에도 바이러스 불활화 작용, 항산화 작용, 방부 방취 방식작용, 계면활성작용, 중금속 용해작용, 유해화학물질 용해 및 중화작용 등의 효과를 가지는 바, 농업, 수산업, 축산업 분야에서 활성제, 항상제, 보조제로 매우 유용하게 사용될 수 있을 것으로 기대된다. As such, the method of extracting fulvic acid from humus soil according to the present invention removes humic substances, which are humus soil, by using at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP, and biotin and a ceramic separator. Not only can activation shorten the overall extraction time of fulvic acid, but it also has the advantage of increasing the extraction yield of fulvic acid compared to when the enzyme is not used. In addition, according to the present invention, fulvic acid in a strong (inactive) redox state can be obtained without adding any chemical components. Therefore, according to the present invention, it is a material with strong oxidation-reduction power, and has effects such as virus inactivation, antioxidant effect, preservative and deodorizing effect, surfactant activity, heavy metal dissolution effect, and harmful chemical substance dissolution and neutralization effect in addition to antibacterial and sterilizing effect. It is expected to be very useful as an activator, antioxidant, and supplement in the fields of agriculture, fisheries, and livestock farming.
이상으로 본 발명의 특정한 부분을 상세히 기술하였는바, 당업계의 통상의 지식을 가진 자에게 있어서 이러한 구체적인 기술은 단지 바람직한 구현예일 뿐이며, 이에 본 발명의 범위가 제한되는 것이 아닌 점은 명백하다. 따라서, 본 발명의 실질적인 범위는 첨부된 청구항과 그의 등가물에 의하여 정의된다고 할 것이다.As the specific parts of the present invention have been described in detail above, it is clear to those skilled in the art that these specific techniques are merely preferred embodiments and do not limit the scope of the present invention. Accordingly, the substantial scope of the present invention will be defined by the appended claims and their equivalents.

Claims (16)

  1. 하기 단계를 포함하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법:A method for extracting a large amount of natural fulvic acid aqueous solution from humic substances, comprising the following steps:
    (S1) 부식토를 물에 첨가하여 pH 6.0~8.0 및 온도 36~44℃를 유지시키면서 혼합 현탁액을 제조하는 단계; (S1) adding humus to water to prepare a mixed suspension while maintaining pH 6.0-8.0 and temperature 36-44°C;
    (S2) 상기 (S1)에서 제조된 혼합 현탁액에 NAD, NADP, FAD, CoA, ATP, GTP, TPP 및 비오틴으로 이루어진 군에서 선택된 하나 이상의 효소를 첨가하여 발효시키는 단계;(S2) fermentation by adding at least one enzyme selected from the group consisting of NAD, NADP, FAD, CoA, ATP, GTP, TPP and biotin to the mixed suspension prepared in (S1);
    (S3) 상기 단계 (S2)에서 발효시킨 발효액의 상등액을 1차 분리 추출하고, 바닥면에 가라앉은 침강 및 침전상태의 부식물질 슬러지(Sludge)를 걷어내어 유압기 또는 원심분리기를 이용하여 2차 분리한 다음 그 슬러지에서 여액을 추출 및 회수하여 상기 1차 추출 상등액과 합치는 단계;(S3) First separation and extraction of the supernatant of the fermentation broth fermented in step (S2), removal of sedimented and precipitated corrosive material sludge that has settled on the bottom, and secondary separation using a hydraulic press or centrifuge. Then, extracting and recovering the filtrate from the sludge and combining it with the first extraction supernatant;
    (S4) 상기 단계 (S3)에서 수득된 상등액의 온도를 11~16℃로 유지하면서 호기조의 세라믹 필터 분리막으로부터 산소가 들어있는 기포를 주입시켜 풀빅산을 숙성시키는 단계;(S4) maturing fulvic acid by injecting oxygen-containing bubbles from the ceramic filter membrane of the aerobic tank while maintaining the temperature of the supernatant obtained in step (S3) at 11 to 16°C;
    (S5) 상기 단계 (S4)에서 숙성된 숙성액을 세라믹 분리막을 이용하여 미세 잔류 부유물을 부상시켜 제거하는 단계; 및(S5) removing fine residual floating matter from the aged liquid aged in step (S4) using a ceramic separator; and
    (S6) 상기 단계 (S5)에서 잔류 부유물을 제거한 숙성액을 0.01~0.5μm의 세라믹 필터를 사용하여 항균 및 멸균여과를 실시하여 풀빅산을 생산하는 단계.(S6) A step of producing fulvic acid by subjecting the aged liquid from which residual suspended matter was removed in step (S5) to antibacterial and sterilization filtration using a ceramic filter of 0.01 to 0.5 μm.
  2. 제 1 항에 있어서, According to claim 1,
    상기 단계 (S1)에서 물 500~800 L에 대하여 부식토 150~300 kg을 넣는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A method for extracting a large amount of natural fulvic acid aqueous solution from humic substances, characterized in that 150 to 300 kg of humus soil is added to 500 to 800 L of water in the step (S1).
  3. 제 1 항에 있어서, According to claim 1,
    상기 단계 (S1)에서 물은 지하수 또는 정제수인 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.In step (S1), the water is groundwater or purified water. A method for extracting a large amount of natural fulvic acid aqueous solution from a humic substance.
  4. 제 3 항에 있어서, According to claim 3,
    상기 지하수 또는 정제수는 염소 성분이 제거된 것임을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A method of extracting a large amount of natural fulvic acid aqueous solution from a corrosive material, wherein the groundwater or purified water has the chlorine component removed.
  5. 제 4 항에 있어서, According to claim 4,
    상기 염소 성분 제거는 활성탄 또는 이온교환수지 흡착제를 사용하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A method of extracting a large amount of natural fulvic acid aqueous solution from a corrosive material, characterized in that the chlorine component is removed using activated carbon or an ion exchange resin adsorbent.
  6. 제 1 항에 있어서, According to claim 1,
    상기 단계 (S2)에서 효소는 부식토 1Kg당 1,500~3,000 mg의 양으로 첨가하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.In the step (S2), the enzyme is added in an amount of 1,500 to 3,000 mg per 1 kg of humus soil. A method of extracting a large amount of natural fulvic acid aqueous solution from humus material.
  7. 제 1 항에 있어서, According to claim 1,
    상기 단계 (S2)에서 세라믹 필터 0.01~0.5㎛ 분리막을 이용하여 100~200㎛ 크기의 기포를 발생시켜 산소공급을 원활하게 하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A method of extracting a large amount of natural fulvic acid aqueous solution from a corrosive material, characterized in that in the step (S2), a ceramic filter membrane of 0.01 to 0.5 ㎛ is used to generate bubbles of 100 to 200 ㎛ in size to facilitate oxygen supply.
  8. 제 1 항에 있어서, According to claim 1,
    상기 단계 (S2)에서 수온 36~44℃ 및 pH 5.5~7.5로 유지시키는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A method of extracting a large amount of natural fulvic acid aqueous solution from a humic substance, characterized in that the water temperature is maintained at 36-44°C and pH 5.5-7.5 in step (S2).
  9. 제 1 항에 있어서, According to claim 1,
    상기 단계 (S3)에서 상등액 분리는 0.01~0.5㎛의 초미세한 세라믹 기공을 통해 외부로부터 공기를 아래에서 윗방향으로 주입시킴으로써 현탁액 속에서 100~200㎛의 초미세한 산소 기포를 발생시키도록 유도시켜 현탁액 수중의 부식물질들을 부상시킴으로써 상등액을 분리시키는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.In the step (S3), the supernatant is separated by injecting air from the outside from bottom to top through ultra-fine ceramic pores of 0.01-0.5 ㎛, thereby inducing the generation of ultra-fine oxygen bubbles of 100-200 ㎛ in the suspension. A method of extracting a large amount of natural fulvic acid aqueous solution from corrosive substances, characterized in that the supernatant is separated by floating the corrosive substances in water.
  10. 제 1 항에 있어서,According to claim 1,
    상기 단계 (S3)에서 2차 추출이 진행된 후에 남은 부식물 슬러지를 건조하여 수분함량 18~22%의 부식토 분말을 제조하는 단계를 추가로 포함하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A large amount of natural fulvic acid aqueous solution is produced from the humus material, characterized in that it further comprises the step of drying the remaining humus sludge after the secondary extraction in step (S3) to produce humus powder with a moisture content of 18 to 22%. How to extract it.
  11. 제 10 항에 있어서, According to claim 10,
    상기 부식토 분말은 농업에서 모종의 뿌리가 잘 자라도록 돕는 발근제, 축산/가축용으로는 항생제 사료의 첨가/보조제 또는 수산업에서 양식 어류의 천연 항생제 사료용으로 사용하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.The humus powder is used as a rooting agent to help the roots of seedlings grow well in agriculture, as an additive/supplement to antibiotic feed for livestock/livestock, or as a natural antibiotic feed for farmed fish in the fisheries industry. Method for extracting large quantities of aqueous acid solution.
  12. 제 1 항에 있어서,According to claim 1,
    상기 단계 (S4)에서 산소 기포를 발생시키면서 70~90일 동안 숙성공정을 진행하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A method of extracting a large amount of natural fulvic acid aqueous solution from a humic substance, characterized in that the aging process is carried out for 70 to 90 days while generating oxygen bubbles in the step (S4).
  13. 제 1 항에 있어서, According to claim 1,
    상기 단계 (S6)에서 숙성액을 교반시키면서 항균 및 멸균여과를 수행하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A method for extracting a large amount of natural fulvic acid aqueous solution from a humic substance, characterized in that antibacterial and sterilizing filtration are performed while stirring the aged solution in the step (S6).
  14. 제 1 항에 있어서, According to claim 1,
    상기 단계 (S6)에서 수득된 풀빅산을 저온살균공정을 추가로 실시하는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.A method for extracting a large amount of natural fulvic acid aqueous solution from a humic substance, characterized in that the fulvic acid obtained in step (S6) is further subjected to a low-temperature sterilization process.
  15. 제 14 항에 있어서, According to claim 14,
    상기 저온살균은 수용액의 온도를 63℃에서 30분 유지시킨 다음 서서히 냉각시키는 것을 특징으로 하는 부식물질로부터 천연 풀빅산 수용액을 대량으로 추출하는 방법.The pasteurization is a method of extracting a large amount of natural fulvic acid aqueous solution from a corrosive material, characterized in that the temperature of the aqueous solution is maintained at 63° C. for 30 minutes and then slowly cooled.
  16. 제 1 항 내지 제 15 항 중 어느 하나에 다른 방법에 의해 제조된 천연 풀빅산 수용액.A natural fulvic acid aqueous solution prepared by a method according to any one of claims 1 to 15.
PCT/KR2022/018813 2022-03-25 2022-11-25 Method for mass production of fulvic acid from humus soil WO2023182610A1 (en)

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KR20160025746A (en) * 2014-08-28 2016-03-09 주식회사 에포코리아 Preparation method of fulvic acid for beverage
JP6095110B2 (en) * 2013-02-21 2017-03-15 孝義 豊田 Humic acid-derived fulvic acid aqueous solution and method for producing the same
JP2018127413A (en) * 2017-02-08 2018-08-16 株式会社ケーツーコミュニケーションズ Method for extracting fulvic acid and humic acid and method for fractionating humus material
KR102154243B1 (en) * 2019-08-09 2020-09-09 고해훈 Extracting method of high purity fulvic acid
KR20210128119A (en) * 2020-04-16 2021-10-26 주식회사 원상피앤씨 Environment friendly extraction method for humic substance

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6095110B2 (en) * 2013-02-21 2017-03-15 孝義 豊田 Humic acid-derived fulvic acid aqueous solution and method for producing the same
KR20160025746A (en) * 2014-08-28 2016-03-09 주식회사 에포코리아 Preparation method of fulvic acid for beverage
JP2018127413A (en) * 2017-02-08 2018-08-16 株式会社ケーツーコミュニケーションズ Method for extracting fulvic acid and humic acid and method for fractionating humus material
KR102154243B1 (en) * 2019-08-09 2020-09-09 고해훈 Extracting method of high purity fulvic acid
KR20210128119A (en) * 2020-04-16 2021-10-26 주식회사 원상피앤씨 Environment friendly extraction method for humic substance

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