# US 11,111,187 B2 · Production method for fulvic acid solution, and fulvic acid solution > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,111,187 B2 - Document ID: US11111187B2 - Status: Granted - Kind: B2 - Application number: 16/092,597 - Filed: 2017-11-01 - Published: 2021-02-25 - Granted: 2021-09-07 - Earliest claimed: 2017-08-31 - Assignees: G-8 International Trading Co., Ltd - Applicants: G-8 International Trading Co., Ltd. - Inventors: Saburo Matsui - Web page: https://patentgrep.com/patent/US11111187B2 ## CPC - C05F 11/06: Apparatus for the manufacture - C07D 493/04: Ortho-condensed systems - B01J 3/02: Feed or outlet devices therefor - B01J 3/03: Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor - B01J 3/04: Pressure vessels, e.g. autoclaves - C05F 11/00: Other organic fertilisers - C05F 11/02: from peat, brown coal, and similar vegetable deposits - C05G 5/23: Solutions - C07C 51/00: Preparation of carboxylic acids or their salts, halides or anhydrides (of acids by hydrolysis of oils, fats or waxes C11C) - C07C 51/42: Separation; Purification; Stabilisation; Use of additives - C02F 11/10: by pyrolysis - Y02W 30/78: Recycling of wood or furniture waste - C05F: ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE - C07D: HETEROCYCLIC COMPOUNDS (macromolecular compounds C08) - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - C05G: MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS (organic fertilisers containing added bacterial cultures, mycelia, or the like C05F11/08; organic fertilisers containing plant vitamins or hormones C05F11/10); FERTILISERS CHARACTERISED BY THEIR FORM - C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS - C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes) - Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT ## Abstract The fulvic acid solution production method of the present invention comprises: an apparatus preparation step of preparing a processing apparatus which comprises: a hermetic container internally having a closeable processing space; a steam jetting device operable to jet high-temperature and high-pressure steam into the hermetic container; a supply section having an opening-closing mechanism and operable to supply a raw material into the hermetic container; and a discharge section having an opening-closing mechanism and operable to discharge, to the outside, a processed liquid produced through processing of the raw material by the steam; a raw material input step of inputting a raw material containing chips of wood as a primary raw material, from the supply section into the processing space of the hermetic container of the processing apparatus; a stream introduction step of introducing steam having a temperature of 120 to 250° C. and a pressure of 12 to 35 atm into the processing space in which the raw material is input; a processing step of subjecting the raw material to a subcritical water reaction processing, under stirring, while introducing the steam; a mixed solution obtaining step of cooling the processed raw material after the processing step to obtain a mixed solution containing fulvic acid and humic acid; and a fulvic acid solution taking-out step of separating humic acid and fulvic acid from the obtained mixed solution to take out a fulvic acid solution. ## Claims ### Claim 1 A fulvic acid solution production method comprising: an apparatus preparation step of preparing a processing apparatus which comprises: a hermetic container internally having a closeable processing space; a steam jetting device operable to jet high-temperature and high-pressure steam into the hermetic container; a supply section having an opening-closing mechanism and operable to supply a raw material into the hermetic container; a stirring device for stirring the raw material supplied into the hermetic container; and a discharge section having an opening-closing mechanism and operable to discharge, to the outside, a processed liquid produced through processing of the raw material by the steam; a raw material input step of inputting a raw material containing chips of wood as a primary raw material, from the supply section into the processing space of the hermetic container of the processing apparatus; a processing step of subjecting the raw material to a subcritical water reaction processing, under stirring, while introducing steam having a temperature of 120 to 250° C. and a pressure of 12 to 35 atm into the processing space in which the raw material is input, to obtain a mixed solution containing fulvic acid, humic acid, and suspended matter of chips of wood and/or fragments thereof; and a fulvic acid solution taking-out step of separating fulvic acid from the obtained mixed solution to take out a fulvic acid solution. ### Claim 2 (depends on 1) The fulvic acid solution production method as recited in claim 1, wherein the wood is a felled timber or wood scrap. ### Claim 3 (depends on 2) The fulvic acid solution production method as recited in claim 2, wherein the felled timber is obtained from a broad-leaved tree or a needle-leaved tree. ### Claim 4 (depends on 3) The fulvic acid solution production method as recited in claim 3, wherein the broad-leaved tree is at least one selected from the group consisting of white birch (Betula platyphylla), willow (Salicaceae), chestnut tree (Castanea crenata), oak (Quercus), and beech (Fagus crenata). ### Claim 5 (depends on 3) The fulvic acid solution production method as recited in claim 3, wherein the needle-leaved tree is at least one selected from the group consisting of pine (Pinus), Japanese cedar (Cryptomeria japonica), Japanese cypress (Chamaecyparis obtusa), and Hiba (Thujopsis dolabrata). ### Claim 6 (depends on 2) The fulvic acid solution production method as recited in claim 2, wherein the wood scrap is solid wood or plywood. ### Claim 7 (depends on 1) The fulvic acid solution production method as recited in claim 1 wherein the processing step is performed for 1 to 8 hours. ### Claim 8 (depends on 3) The fulvic acid solution production method as recited in claim 3, wherein the primary raw material is a broad-leaved tree, and wherein the pressure of steam to be introduced in the processing step is in the range of 12 to 25 atm. ### Claim 9 (depends on 3) The fulvic acid solution production method as recited in claim 3, wherein the primary raw material is a needle-leaved tree, and wherein the pressure of steam to be introduced in the processing step is in the range of 20 to 35 atm. ### Claim 10 A fulvic acid solution production method comprising: an apparatus preparation step of preparing a processing apparatus which comprises: a hermetic container internally having a closeable processing space; a steam jetting device operable to jet high-temperature and high-pressure steam into the hermetic container; a supply section having an opening-closing mechanism and operable to supply a raw material into the hermetic container; a stirring device for stirring the raw material supplied into the hermetic container; and a discharge section having an opening-closing mechanism and operable to discharge, to the outside, a processed liquid produced through processing of the raw material by the steam; a raw material input step of inputting a plant raw material comprised of a gramineous plant as a primary raw material, from the supply section into the processing space of the hermetic container of the processing apparatus; a processing step of subjecting the raw material to a subcritical water reaction processing, under stirring, while introducing steam having a temperature of 100 to 200° C. and a pressure of 5 to 25 atm into the processing space in which the raw material is input, to obtain a mixed solution containing fulvic acid and humic acid; and a fulvic acid solution taking-out step of separating fulvic acid from the obtained mixed solution to take out a fulvic acid solution. ### Claim 11 (depends on 10) The fulvic acid solution production method as recited in claim 10, wherein the plant raw material is felled or mowed plant, or a plant scrap. ### Claim 12 (depends on 11) The fulvic acid solution production method as recited in claim 11, wherein the felled or mowed plant is at least one selected from the group consisting of rice (Oryza sativa), wheat (Triticum aestivum), barley (Hordeum vulgare), oat (Avena fatua), rye (Secale cereale), proso millet (Panicum miliaceum), foxtail millet (Setaria italica), Japanese millet (Echinochloa esculenta), corn (Zea mays), finger millet (Eleusine coracana), sorghum (Sorghum bicolor), bamboo (Bambusoideae), manchurian wild rice (Zizania latifolia), sugar cane (Saccharum officinarum), adlay (Coix lacryma-jobi var. ma-yuen), reed (Phragmites australis), Japanese silver grass (Miscanthus sinensis), arrow bamboo (Pseudosasa japonica), giant reed (Arundo donax), pampas grass (Cortaderia selloana), and lawn grass. ### Claim 13 (depends on 11) The fulvic acid solution production method as recited in claim 11, wherein the felled or mowed plant is rice straw or wheat straw. ### Claim 14 (depends on 12) The fulvic acid solution production method as recited in claim 12, wherein the felled or mowed plant is bamboo. ### Claim 15 (depends on 14) The fulvic acid solution production method as recited in claim 14, wherein the bamboo is formed in a chip shape. ### Claim 16 (depends on 10) The fulvic acid solution production method as recited in claim 10, wherein the raw material is a post-use plant scrap. ### Claim 17 (depends on 16) The fulvic acid solution production method as recited in claim 16, wherein the plant scrap is an aging tatami mat. ### Claim 18 (depends on 10) The fulvic acid solution production method as recited in claim 10, wherein the processing step is performed for 3 to 30 minutes. ### Claim 19 (depends on 1) The fulvic acid solution production method as recited in claim 1, wherein the raw material is introduced into the processing space in an amount of 90% by volume or less of the processing space. ### Claim 20 (depends on 1) The fulvic acid solution production method as recited in claim 1, wherein the raw material is introduced into the processing space in an amount of 50 to 80% by volume of the processing space. ### Claim 21 (depends on 1) The fulvic acid solution production method as recited in claim 1, wherein the stirring in the processing step is performed by a stirring member rotatably disposed in the processing space. ### Claim 22 (depends on 1) The fulvic acid solution production method as recited in claim 1, wherein the raw material input step includes adding an alkaline solution as an additive.