WO2025013525A1 - リン酸塩の製造方法 - Google Patents

リン酸塩の製造方法 Download PDF

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Publication number
WO2025013525A1
WO2025013525A1 PCT/JP2024/021829 JP2024021829W WO2025013525A1 WO 2025013525 A1 WO2025013525 A1 WO 2025013525A1 JP 2024021829 W JP2024021829 W JP 2024021829W WO 2025013525 A1 WO2025013525 A1 WO 2025013525A1
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Prior art keywords
phosphate
acid
phosphorus
producing
phosphoric acid
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PCT/JP2024/021829
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English (en)
French (fr)
Japanese (ja)
Inventor
泰武 矢埜
久宏 松永
克則 ▲高▼橋
茂 杉山
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JFE Steel Corp
University of Tokushima NUC
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JFE Steel Corp
University of Tokushima NUC
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Priority to JP2024562268A priority Critical patent/JP7795004B2/ja
Priority to KR1020257041202A priority patent/KR20260008131A/ko
Priority to EP24839421.5A priority patent/EP4711330A1/en
Publication of WO2025013525A1 publication Critical patent/WO2025013525A1/ja
Anticipated expiration legal-status Critical
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/37—Phosphates of heavy metals
    • C01B25/375—Phosphates of heavy metals of iron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a method for producing phosphates.
  • phosphorus While phosphorus is used in a wide range of fields, including agriculture, food, medicine, and industry, it is a resource that is unevenly distributed around the world, and is only produced in a limited number of countries, including China, the United States, and Morocco.
  • the phosphorus resources circulating in Japan are phosphorus products such as yellow phosphorus and crude phosphoric acid, and the raw material for these, phosphate rock, and the entire supply is imported.
  • the phosphorus concentration of molten iron tapped from a blast furnace is about 0.1% by mass, and the phosphorus concentration in steelmaking slag produced by subjecting this molten iron to conventional general treatments (dephosphorization treatment, decarburization refining) is as low as about 5% by mass at most, calculated as P2O5 .
  • dephosphorization treatment, decarburization refining is as low as about 5% by mass at most, calculated as P2O5 .
  • Patent Document 1 discloses a method for recovering phosphorus in the form of calcium phosphate (i.e., producing calcium phosphate) from dephosphorization slag, a type of steelmaking slag.
  • Calcium phosphate produced by the method described in Patent Document 1 may contain large amounts of impurities such as silicon.
  • phosphorus (phosphate) cannot be recovered in a form other than calcium phosphate.
  • the present invention has been made in consideration of the above points, and aims to provide a method for producing phosphate that can obtain the desired phosphate with few impurities.
  • a method for producing a target phosphate comprising: a precipitation step of adding an alkali to a phosphorus-containing liquid to obtain a precipitate; and a dissolution step of dissolving the precipitate with an acid to obtain a phosphoric acid liquid, wherein in the precipitation step, the composition of the precipitate is changed by changing the timing of adding the alkali depending on the type of the phosphate.
  • the desired phosphate can be obtained with few impurities.
  • 1 is a flowchart showing the flow of a method for producing a phosphate according to the present embodiment.
  • 1 is a graph showing the relationship between the timing of adding an alkali to a phosphorus-containing liquid and the precipitation rate of each element.
  • 1 is a graph showing the content (unit: mmol/100 mL) of each element in a phosphoric acid solution for each concentration (0.5 M and 13.5 M) of acid used.
  • 1 is an X-ray diffraction pattern of the residue (III) obtained when an acid (nitric acid) having a concentration of 13.5 M was used.
  • FIG. 1 is a flow chart showing the flow of the method for producing a phosphate according to the present embodiment.
  • the method for producing a phosphate according to the present embodiment is a method for recovering phosphorus from a starting material in the form of a target phosphate (calcium phosphate, iron phosphate, etc.), and includes an acid leaching step (S0), a precipitation step (S1), a dissolution step (S2), and a cation exchange step (S3), in this order.
  • the acid leaching step (S0) and the cation exchange step (S3) are optional steps and may be omitted.
  • the method for producing a phosphate according to this embodiment may include an addition step (S4) after the dissolving step (S2) or the cation exchange step (S3).
  • ⁇ Acid leaching step (S0)> the components contained in the starting material are leached in acid to obtain a phosphorus-containing liquid. Specifically, for example, the starting material is added to the acid, stirred, and then filtered. This produces a residue (I) and a leachate (A). The leachate (A) is the phosphorus-containing liquid.
  • the acid used in the acid leaching step (S0) may be at least one selected from the group consisting of nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, and organic acids (e.g., citric acid), of which nitric acid or hydrochloric acid is preferred, and nitric acid is more preferred.
  • the concentration of the acid is not particularly limited, but is preferably 0.1 to 1.5M, and more preferably 0.3 to 0.8M.
  • the starting material examples include steelmaking slag such as dephosphorization slag and decarburization slag.
  • the starting material is a phosphorus - containing compound, and preferably contains at least CaO, P2O5 , Al2O3 , and FetO .
  • the pH of the acid used in the acid leaching step (S0) is preferably 4.0 or less, more preferably 1.0 or less, and even more preferably 0.5 or less.
  • the pH of the acid is within this range, if the ratio of the starting material to the acid is high, the amount of silicon eluted increases accordingly, and the resulting phosphorus-containing liquid may gel. For this reason, it is preferable to determine the ratio of the starting material to the acid by carefully examining the conditions of each step described below.
  • pH is measured in accordance with JIS Z8802:2011 "pH measurement method" (hereinafter the same).
  • the temperature when measuring pH is 25°C unless otherwise specified.
  • ⁇ Precipitation Step (S1)> an alkali is added to the phosphorus-containing liquid to obtain a precipitate. Specifically, for example, an alkali is added to the phosphorus-containing liquid, and then the liquid is filtered. As a result, a precipitate (II) and a filtrate (B) are obtained. The precipitate (II) is the precipitate.
  • the phosphorus-containing liquid for example, the leachate (A) obtained in the acid leaching step (S0) is used, but one obtained in another step may also be used.
  • the phosphorus-containing liquid preferably contains at least the elements calcium (Ca), phosphorus (P), aluminum (Al) and iron (Fe).
  • the phosphorus-containing liquid may further contain elements such as silicon (Si), magnesium (Mg) and manganese (Mn).
  • Examples of the alkali used in the precipitation step (S1) include sodium hydroxide, potassium hydroxide, calcium hydroxide, and aqueous ammonia (NH 4 OH). Of these, aqueous ammonia is preferred because it does not contain unnecessary cations.
  • the concentration of the aqueous ammonia is not particularly limited, but is preferably from 20 to 40% by mass, and more preferably from 25 to 35% by mass.
  • impurities are elements other than the elements that constitute the target phosphate.
  • the "impurities” are elements (Fe, Si, Al, etc.) other than calcium (Ca), phosphorus (P) and oxygen (O).
  • FIG. 2 is a graph showing the relationship between the timing of adding an alkali to the phosphorus-containing liquid and the precipitation rate of each element.
  • the timing of adding an alkali to the phosphorus-containing liquid specifically means, for example, the time from when the phosphorus-containing liquid is obtained in the acid leaching step (S0) to when the alkali is added to the phosphorus-containing liquid.
  • the vertical axis in FIG. 2 indicates, for each element, the ratio of the content in the precipitate obtained by adding the alkali (precipitation ratio) to the content in the phosphorus-containing liquid before adding the alkali.
  • the precipitation ratio of element M is 100%, it means that all of element M in the phosphorus-containing liquid has been transferred to the precipitate, whereas when the precipitation ratio is 0%, it means that none of element M in the phosphorus-containing liquid has been transferred to the precipitate.
  • the timing of adding an alkali to the phosphorus-containing liquid is changed depending on the type of the target phosphate, thereby changing the composition of the resulting precipitate. Specifically, for example, the time from obtaining the phosphorus-containing solution in the acid leaching step (S0) to adding the alkali thereto is changed.
  • the timing of adding the alkali is delayed in order to allow the precipitate to contain a sufficient amount of Fe, which is a necessary element.
  • the time from obtaining the phosphorus-containing liquid to adding the alkali is preferably 4 hours or more.
  • the precipitate since the precipitate also contains a large amount of Si as an impurity, it is preferable to remove Si in the dissolving step (S2) described below.
  • the timing of adding the alkali is made earlier in order to reduce the impurities of Si and Fe from the precipitate.
  • the time from obtaining the phosphorus-containing liquid to adding the alkali is preferably 1 hour or less.
  • the precipitate contains only a small amount of the necessary Ca, it is preferable to add an additional raw material (calcium nitrate) corresponding to the target phosphate (calcium phosphate) in the addition step (S4) described below.
  • Si may be removed in the dissolving step (S2) described below.
  • ⁇ Dissolving step (S2)> the precipitate (II) obtained in the precipitation step (S1) is dissolved using an acid. This results in a phosphoric acid solution. Specifically, for example, the precipitate is added to an acid, stirred, and then filtered. This results in a residue (III) and a filtrate (C). The filtrate (C) is the phosphoric acid solution.
  • the acid used in the dissolution step (S2) may be at least one selected from the group consisting of nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, and organic acids (e.g., citric acid), with nitric acid or hydrochloric acid being preferred, and nitric acid being more preferred.
  • Fig. 3 is a graph showing the content (unit: mmol/100 mL) of each element in the phosphoric acid solution for each concentration of acid used (0.5 M and 13.5 M).
  • Fig. 4 shows the X-ray diffraction pattern of the residue (III) obtained when an acid (nitric acid) having a concentration of 13.5 M was used. From Fig. 4, it can be seen that the residue (III) contains silica (SiO 2 ), and Si was separated as silica.
  • the concentration of the acid used in the dissolving step (S2) is preferably 10.0 M or more, more preferably 11.5 M or more, and even more preferably 13.0 M or more. This makes it possible to reduce the Si content in the resulting phosphoric acid solution.
  • the target phosphate is iron phosphate, calcium phosphate, or the like, since Si is an impurity, it is very beneficial to reduce the Si content in the resulting phosphoric acid solution.
  • ⁇ Cation exchange step (S3)> It is preferred to provide a cation exchange step (S3) after the dissolution step (S2).
  • the phosphoric acid solution obtained in the dissolving step (S2) is treated with a cation exchange resin (cation exchange treatment), which removes cations from the phosphoric acid solution and increases the purity of the phosphate salt finally obtained.
  • the treatment using a cation exchange resin may be, for example, the same treatment as that described in paragraphs [0022] to [0024] of Patent Document 1.
  • ⁇ Addition step (S4)> It is preferable to provide an addition step (S4) after the dissolution step (S2) or the cation exchange step (S3).
  • an addition step (S4) an additional raw material according to the type of target phosphate is added to the phosphoric acid solution obtained in the dissolving step (S2) (or the phosphoric acid solution treated in the cation exchange step (S3)). In this way, the target phosphate is obtained.
  • the target phosphate is calcium phosphate
  • calcium nitrate is added as an additional raw material to the phosphoric acid solution in the adding step (S4).
  • An alkali is then added to the phosphoric acid solution to which calcium nitrate has been added, thereby obtaining a precipitate of calcium phosphate.
  • the alkali to be added is preferably one of those described as the alkali used in the precipitation forming step (S1) above.
  • the content of impurities such as Si and Fe in the finally obtained phosphate (calcium phosphate) can be reduced.
  • the target phosphate is iron phosphate
  • iron nitrate is added as an additional raw material to the phosphoric acid solution, thereby obtaining a precipitate of iron phosphate.
  • the content of the impurity Si in the finally obtained phosphate (iron phosphate) can be reduced.
  • the desired phosphate can be obtained with few impurities.
  • the desired phosphate was obtained.
  • the timing of adding the alkali in the precipitation step (S1) and the concentration of the acid (nitric acid) in the dissolution step (S2) were changed.
  • Ammonia water concentration: 28% by mass was used as the alkali.
  • slag 1 steelmaking slag having the composition shown in Table 1 below were leached in nitric acid (concentration: 0.5 M) to obtain a phosphorus-containing liquid.
  • Example 1 The desired phosphate was calcium phosphate.
  • the timing of addition of the alkali (the time from obtaining the phosphorus-containing liquid to adding the alkali thereto) was set to 1 hour or less to obtain a precipitate.
  • the precipitate was dissolved using nitric acid having a concentration of 13.5 M to obtain a phosphoric acid solution.
  • the phosphoric acid solution was passed through a cation exchange resin to obtain a phosphoric acid solution having the composition shown in Table 2 below.
  • the adding step (S4) calcium nitrate was added as an additional raw material to the phosphoric acid solution to obtain single-phase calcium phosphate.
  • Example 2 In the precipitation step (S1), the timing of adding the alkali was changed to 4 h. Otherwise, a phosphoric acid solution having the composition shown in Table 2 below was obtained in the same manner as in Example 1. Thereafter, in the adding step (S4), calcium nitrate was added as an additional raw material to the phosphoric acid solution to obtain single-phase calcium phosphate. As shown in Table 2 below, the phosphoric acid solution in Example 2 had a higher content of Fe as an impurity than that in Example 1. As a result, the calcium phosphate obtained from the phosphoric acid solution had a higher content of Fe as an impurity.
  • Example 3 The desired phosphate was iron phosphate.
  • the timing of addition of the alkali (the time from obtaining the phosphorus-containing liquid to adding the alkali thereto) was set to 4 hours, and a precipitate was obtained.
  • the precipitate was dissolved using nitric acid having a concentration of 13.5 M to obtain a phosphoric acid solution.
  • the phosphoric acid solution was passed through a cation exchange resin to obtain a phosphoric acid solution having the composition shown in Table 3 below.
  • iron nitrate was added to the phosphoric acid solution as an additional raw material to obtain iron phosphate.
  • Example 4 In the dissolution step (S2), nitric acid having a concentration of 8.5 M was used. Otherwise, the procedure was the same as in Example 3 to obtain a phosphoric acid solution having the composition shown in Table 3 below. Thereafter, in the adding step (S4), iron nitrate was added to the phosphoric acid solution as an additional raw material to obtain iron phosphate. As shown in Table 3 below, the phosphoric acid solution in Example 4 had a higher content of Si, which was an impurity, than that in Example 3. As a result, the iron phosphate obtained from the phosphoric acid solution had a higher content of Si, which was an impurity.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)
PCT/JP2024/021829 2023-07-12 2024-06-17 リン酸塩の製造方法 Pending WO2025013525A1 (ja)

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JP2024562268A JP7795004B2 (ja) 2023-07-12 2024-06-17 リン酸塩の製造方法
KR1020257041202A KR20260008131A (ko) 2023-07-12 2024-06-17 인산염의 제조 방법
EP24839421.5A EP4711330A1 (en) 2023-07-12 2024-06-17 Phosphoric acid salt production method

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014133196A (ja) * 2013-01-09 2014-07-24 Kobelco Eco-Solutions Co Ltd 下水汚泥焼却灰又は製鋼スラグからのリン酸回収方法
JP2017505280A (ja) * 2013-12-02 2017-02-16 エコフォス・エス・アー 農業及び食品産業向けのリン酸塩源
JP2020018951A (ja) * 2018-07-30 2020-02-06 日本製鉄株式会社 鉄鋼スラグからリン酸塩を回収する方法
JP2020192483A (ja) * 2019-05-24 2020-12-03 国立大学法人 新潟大学 処理方法
JP2022150640A (ja) 2021-03-26 2022-10-07 株式会社北匠 リン化合物の製造方法
CN116395695A (zh) * 2023-05-10 2023-07-07 昆明理工大学 一种利用赤泥制备磷酸盐的方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014133196A (ja) * 2013-01-09 2014-07-24 Kobelco Eco-Solutions Co Ltd 下水汚泥焼却灰又は製鋼スラグからのリン酸回収方法
JP2017505280A (ja) * 2013-12-02 2017-02-16 エコフォス・エス・アー 農業及び食品産業向けのリン酸塩源
JP2020018951A (ja) * 2018-07-30 2020-02-06 日本製鉄株式会社 鉄鋼スラグからリン酸塩を回収する方法
JP2020192483A (ja) * 2019-05-24 2020-12-03 国立大学法人 新潟大学 処理方法
JP2022150640A (ja) 2021-03-26 2022-10-07 株式会社北匠 リン化合物の製造方法
CN116395695A (zh) * 2023-05-10 2023-07-07 昆明理工大学 一种利用赤泥制备磷酸盐的方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SUGIYAMA SHIGERU, HSIAO LI-HAO, TOKUNAGA TAIZO, HASHIMOTO TAKUMI, HABARA MASAKI, SHIMODA NAOHIRO, LIU JHY-CHERN, ABE SEIICHI, YAMA: "PHOSPHORUS RECOVERY FROM SEWAGE-SLUDGE MOLTEN SLAG USING A COMBINATION OF ACID-DISSOLUTION, ALKALI-PRECIPITATION, AND ION-EXCHANGE", PHOSPHORUS RESEARCH BULLETIN, TOKYO, JP, vol. 38, no. 0, 1 January 2022 (2022-01-01), JP , pages 60 - 66, XP093261036, ISSN: 0918-4783, DOI: 10.3363/prb.38.60 *

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TW202508963A (zh) 2025-03-01
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EP4711330A1 (en) 2026-03-18
JP7795004B2 (ja) 2026-01-06

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