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WO2025023114A1 - Acide humique liquide et procédé de production d'acide humique liquide - Google Patents

Acide humique liquide et procédé de production d'acide humique liquide Download PDF

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Publication number
WO2025023114A1
WO2025023114A1 PCT/JP2024/025614 JP2024025614W WO2025023114A1 WO 2025023114 A1 WO2025023114 A1 WO 2025023114A1 JP 2024025614 W JP2024025614 W JP 2024025614W WO 2025023114 A1 WO2025023114 A1 WO 2025023114A1
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WIPO (PCT)
Prior art keywords
humic acid
liquid
acid
liquid humic
total organic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/JP2024/025614
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English (en)
Japanese (ja)
Inventor
峻 大川
史也 星賀
藤樹 飯野
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Denka Co Ltd
Original Assignee
Denka Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Denka Co Ltd filed Critical Denka Co Ltd
Priority to JP2024574618A priority Critical patent/JP7664499B1/ja
Priority to JP2025009291A priority patent/JP2025065168A/ja
Publication of WO2025023114A1 publication Critical patent/WO2025023114A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F11/00—Other organic fertilisers
    • C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • 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; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G5/00—Fertilisers characterised by their form
    • C05G5/20—Liquid fertilisers

Definitions

  • the present invention relates to liquid humic acid and a method for producing liquid humic acid.
  • this humic acid extract is produced by extracting it from a crude humic acid product obtained by oxidizing young coal such as brown coal and lignite with nitric acid (Patent Document 1).
  • liquid humic acid involves a process of reacting lignite with nitric acid, but since the production is carried out using nitric acid, nitrate radicals may remain in the liquid humic acid produced. If nitrate radicals are present in liquid humic acid, there is a concern that the nitrate radicals may be generated as nitric acid gas during long-term storage. Therefore, it was necessary to take complicated storage measures, such as storing the liquid humic acid in a cool, dark place with good ventilation, away from direct sunlight. Therefore, there was a demand for liquid humic acid that could be stored safely.
  • the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a liquid humic acid that can be stably stored for a long period of time. Furthermore, an object of the present invention is to provide a method for producing liquid humic acid with reduced environmental impact.
  • the present inventors discovered that by keeping the concentration of nitrate ions at or below a predetermined concentration, it is possible to suppress the generation of nitric acid gas due to long-term storage, and that by keeping the ratio of the total organic carbon concentrations in the precipitate and soluble parts within a predetermined range, it is possible to further improve crop growth, and thus completed the present invention.
  • the present inventors discovered that by including a reaction process in which young coal and hydrogen peroxide are oxidized in the presence of a metal catalyst, liquid humic acid can be produced and the generation of NOx gas can be suppressed, thereby completing the present invention. That is, the present invention is as follows.
  • the value of B/A x 100 is preferably 20 to 800.
  • the preferred value of B/A x 100 also varies depending on the condition of the soil in which the liquid humic acid is used or the type of crop. When the soil pH is high or the crop is a leafy vegetable or root vegetable, the preferred value is 15 to 100, more preferably 20 to 80. When the soil pH is low or the crop is a fruit or flower, the preferred value is 80 to 1000, more preferably 100 to 800.
  • the total organic carbon concentration of the precipitate and the total organic carbon concentration of the soluble portion can be measured by the method described in the Examples below.
  • the total organic carbon concentration of the precipitate is substantially equal to the total organic carbon concentration of humic acid
  • the organic matter contained in the soluble is mainly composed of fulvic acid
  • the total organic carbon concentration of the soluble is substantially equal to the total organic carbon concentration of fulvic acid.
  • humic acid can be classified into humic acid, which is an insoluble fraction, alkali-soluble and acid-insoluble humic acid (also called humic acid), and acid-soluble fulvic acid. Therefore, the precipitate in liquid humic acid may be humic acid, and the soluble part may be fulvic acid.
  • the sum of the total organic carbon concentration of humic acid and the total organic carbon concentration of fulvic acid in the liquid humic acid is more preferably 5,000 to 130,000 mg/L, and even more preferably 5,000 to 120,000 mg/L.
  • the sum of the total organic carbon concentration of humic acid and the total organic carbon concentration of fulvic acid in the liquid humic acid is substantially equal to the total organic carbon concentration of the liquid humic acid.
  • the concentration of tungsten in the liquid humic acid according to this embodiment is preferably 5 ⁇ g/g or more and 500 ⁇ g/g or less, more preferably 8 ⁇ g/g or more and 400 ⁇ g/g or less, and even more preferably 10 ⁇ g/g or more and 200 ⁇ g/g or less.
  • the concentration of tungsten in liquid humic acid can be adjusted by adjusting the concentration of tungsten acid, heterotungstic acid, and their salts, which are metal catalysts used in producing liquid humic acid.
  • the concentration of tungsten can be measured by ICP emission spectrometry.
  • the pH of the liquid humic acid according to this embodiment is preferably 5 to 10.
  • the pH of the liquid humic acid is 5 to 10
  • the precipitation of humic acid and fulvic acid in the liquid humic acid can be suppressed.
  • the pH of the liquid humic acid is 5 to 10
  • the liquid humic acid can be handled more safely, and the solubility of the liquid humic acid with fertilizer components can be further improved.
  • the pH of the liquid humic acid according to this embodiment is more preferably 6.5 to 8. More preferably, it is 6.5 to 7.5.
  • the pH of the liquid humic acid can be measured by the method described in the Examples below.
  • Young coal is coal with a lower carbon content than bituminous coal, and is defined as having a carbon content of 83% by mass or less.
  • Examples of young coal include peat, lignite, brown coal, and subbituminous coal. Of these, it is preferable to use lignite, as it produces a high yield of humic acid. It is also possible to use a mixture of two or more of the above coals.
  • the amount of metal catalyst used is preferably 3 parts by mass or less, and more preferably 1.5 parts by mass or less, per 100 parts by mass of young coal.
  • the amount of metal catalyst used is preferably 0.001 parts by mass or more, and more preferably 0.002 parts by mass or more, per 100 parts by mass of young coal.
  • the temperature for producing liquid humic acid is preferably from room temperature (20°C) to 90°C, more preferably from 35°C to 90°C, even more preferably from 45°C to 85°C, and particularly preferably from 75°C to 85°C.
  • the reaction time is preferably from 30 minutes to 6 hours, more preferably from 1 to 5 hours.
  • the amount of alkali to be used can be determined in advance by conducting tests in which different amounts of alkali are used with respect to the crude humic acid product, and determining the desired pH of the liquid humic acid and the amount of alkali to be used.
  • the alkali to be added to adjust the pH during extraction can be selected according to the intended use, such as potassium hydroxide, which can be used as a fertilizer component.
  • the extraction is performed using a hot water bath or the like, and the liquid is held at a temperature of 40 to 90°C for 0.5 to 24 hours to extract a humic acid extract. If the liquid temperature and holding time are within the above ranges, the extract will not freeze and the quality of the extract can be ensured. From this perspective, the liquid temperature is preferably 45 to 90°C, and more preferably 50 to 80°C. The holding time is preferably 0.5 to 12 hours, and more preferably 1 to 6 hours. After the humic acid extract is extracted, it is preferably cooled to 40°C or less. The unreacted residue is separated from the humic acid extract by, for example, centrifugation or a filter press.
  • pH Measurement The pH was measured by the glass electrode method while stirring the suspension (humic acid extract) with a magnetic stirrer.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Fertilizers (AREA)

Abstract

Un but de la présente invention est de fournir de l'acide humique liquide qui peut être stocké de manière stable sur une longue période. L'acide humique liquide a une concentration de radicaux d'acide nitrique de 2 000 μg/g ou moins et, par ajout d'acide chlorhydrique à l'acide humique liquide pour ajuster le pH à 1, est séparé en une partie de sédimentation et une partie soluble. Lorsque la concentration totale en carbone organique de la partie de sédimentation est exprimée par A mg/L et la concentration totale en carbone organique de la partie soluble est exprimée par B mg/L, alors la valeur de B/A × 100 est de 15 à 1000.
PCT/JP2024/025614 2023-07-25 2024-07-17 Acide humique liquide et procédé de production d'acide humique liquide Pending WO2025023114A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2024574618A JP7664499B1 (ja) 2023-07-25 2024-07-17 液状腐植酸、及び液状腐植酸の製造方法
JP2025009291A JP2025065168A (ja) 2023-07-25 2025-01-22 液状腐植酸、及び液状腐植酸の製造方法

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2023-120479 2023-07-25
JP2023-120480 2023-07-25
JP2023120480 2023-07-25
JP2023120479 2023-07-25

Publications (1)

Publication Number Publication Date
WO2025023114A1 true WO2025023114A1 (fr) 2025-01-30

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2024/025614 Pending WO2025023114A1 (fr) 2023-07-25 2024-07-17 Acide humique liquide et procédé de production d'acide humique liquide

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JP (2) JP7664499B1 (fr)
WO (1) WO2025023114A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5415778A (en) * 1993-03-03 1995-05-16 Hydrogeo North America L.L.C. Method and related product for purification of waste water
JP2010509311A (ja) * 2006-11-03 2010-03-25 ビジャム バイオサイエンシス プライベート リミテッド 亜炭の分解による機能的有効有機分子の製造
JP2018095555A (ja) * 2016-12-08 2018-06-21 デンカ株式会社 腐植酸抽出液及びその製造方法
JP2018127413A (ja) * 2017-02-08 2018-08-16 株式会社ケーツーコミュニケーションズ フルボ酸およびフミン酸の抽出方法、ならびに腐植物質の分画方法
WO2023139886A1 (fr) * 2022-01-21 2023-07-27 デンカ株式会社 Acide humique liquide et procédé de production d'acide humique liquide

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5415778A (en) * 1993-03-03 1995-05-16 Hydrogeo North America L.L.C. Method and related product for purification of waste water
JP2010509311A (ja) * 2006-11-03 2010-03-25 ビジャム バイオサイエンシス プライベート リミテッド 亜炭の分解による機能的有効有機分子の製造
JP2018095555A (ja) * 2016-12-08 2018-06-21 デンカ株式会社 腐植酸抽出液及びその製造方法
JP2018127413A (ja) * 2017-02-08 2018-08-16 株式会社ケーツーコミュニケーションズ フルボ酸およびフミン酸の抽出方法、ならびに腐植物質の分画方法
WO2023139886A1 (fr) * 2022-01-21 2023-07-27 デンカ株式会社 Acide humique liquide et procédé de production d'acide humique liquide

Also Published As

Publication number Publication date
JPWO2025023114A1 (fr) 2025-01-30
JP7664499B1 (ja) 2025-04-17
JP2025065168A (ja) 2025-04-17

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