CN105695739B - Method for improving recovery rate of associated rare earth in phosphorite - Google Patents

Method for improving recovery rate of associated rare earth in phosphorite Download PDF

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Publication number
CN105695739B
CN105695739B CN201610096676.4A CN201610096676A CN105695739B CN 105695739 B CN105695739 B CN 105695739B CN 201610096676 A CN201610096676 A CN 201610096676A CN 105695739 B CN105695739 B CN 105695739B
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phosphoric acid
rare earth
acid
mixed
solution
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CN105695739A (en
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冯林永
蒋训雄
范艳青
汪胜东
张登高
刘巍
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Beijing General Research Institute of Mining and Metallurgy
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Beijing General Research Institute of Mining and Metallurgy
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00—Obtaining rare earth metals
    • 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

Abstract

The invention discloses a method for improving recovery rate of associated rare earth in phosphorite. Leaching the phosphorite containing the rare earth by using phosphoric acid as a main component and a mixed acid solution containing a proper amount of sulfuric acid and fluoride, and then carrying out solid-liquid separation to obtain leaching slag and a solution containing the rare earth; the solution containing rare earth is added into a phosphoric acid regeneration stirring tank together with a proper amount of sulfuric acid after the rare earth is recovered by extraction or ion exchange to react to obtain mixed slurry containing phosphoric acid and gypsum, a part of the mixed slurry is returned into the regeneration stirring tank as return slurry, and the rest is subjected to solid-liquid separation to obtain phosphoric acid solution and gypsum residue; and opening a part of the phosphoric acid solution, adjusting components, returning the components as mixed acid for recycling, and producing phosphoric acid from the rest part. The method utilizes sulfuric acid and F in mixed acid‑The erosion function of the rare earth leaching agent dissolves a small amount of insoluble independent rare earth minerals or rare earth substances wrapped by silicate in the phosphorite, and the leaching rate of the rare earth can be effectively improved.

Description

A kind of method of association rare earth yield in raising phosphorus ore
Technical field
A kind of method of association rare earth yield in raising phosphorus ore, belongs to the synthetical recovery field of association rare earth, especially relates to A kind of and method that the phosphorus ore middle rare earth rate of recovery is improved by using fluorine-containing mixture of sulfuric phosphoric acid.
Background technology
Rare earth element also has part and apatite and phosphorite symbiosis in addition to preservation is in Rare Earth Mine.Due to rare earth Ionic radius is very close with calcium ion, and rare earth is generally present in phosphorus ore in a manner of isomorph, and rare earth element content with The increase of phosphorus ore grade and increase.Russia, the Chinese, U.S. are the countries of three main association rare earth phosphate rocks in the world, wherein E Luoxibin apatite, Kola phosphorus ore middle rare earth average grade are respectively 0.5%~5% and 0.5%~0.67%, especially tool It is representative.World phosphate gross reserves is about 100,000,000,000 tons, is 0.05% estimation by rare earth average content, gross reserves is up to 50,000,000 Ton, association rare earth element reserves are huge in phosphorus ore.
Recovery association rare earth is the master of association rare earth element in current comprehensive utilization phosphorus ore during Wet-process Phosphoric Acid Production Want approach.Russia is disclosed using in 20-25% sulfuric acid leaching ardealite in patent RU2225892C1 disclosed in 2002 Rare earth.French Patent (FRP) (US4636369) Rhone-Poulenc Chimie de Base disclose to be drawn in phosphoric acid by wet process ore pulp Enter aluminium ion, iron ion, silicon ion or its hybrid ionic, to increase the solubility of rare earth in the solution, rare earth highest enrichment For 56%.Chinese patent 200710178377.6 discloses that organic or inorganic surfaces are added in sulfuric acid decomposition phosphorite process is active Agent changes ardealite crystal formation, and enrichment of the rare earth in phosphoric acid is up to 80%.Polish researcher is also reported using dilute sulfuric acid Ardealite is leached, obtains the enriched substances of 10-18% containing rare earth through being concentrated by evaporation, then prepare through hydrofluoric acid precipitation or NPPA solvent extractions Purity of Rare Earth is more than 40% enriched substance.
Phosphoric acid method is a kind of new separation phosphorus ore middle rare earth side for developing in recent years according to traditional sulfuric acid process feature Method.It is to leach association rare earth phosphate rock using phosphoric acid to realize most of phosphorus calcium and Rare Earth Separation.Chinese patent 201010217142.5 disclose a kind of method that phosphoric acid leaches rare earth, and association rare earth phosphate rock is leached with phosphoric acid at 100 DEG C, dilute Native leaching rate reaches as high as 93.2%.Chinese patent 201110143415.0 discloses a kind of side of the rare-earth separating from phosphorus ore Method, leached at 15~50 DEG C of lower temperature with phosphoric acid, the dissolving of the element such as most of phosphorus, calcium, iron, aluminium enters solution, about 95% Rare earth element stay in leached mud and obtain rare-earth enrichment slag.
In using phosphoric acid method dissolving phosphorus ore during association rare earth, leaching condition is harsher and because part rare earth is glued Native mineral parcel exists in the form of the Independent Mineral for being insoluble in phosphoric acid and influences the rate of recovery of rare earth.
The content of the invention
The purpose of the present invention is the deficiency existing for prior art, especially for phosphoric acid method dissolution association rare earth element When severe reaction conditions and existing part rare earth the problem of can not being dissolved, there is provided one kind improves association rare earth in phosphorus ore and returned The method of yield.
The purpose of the present invention is achieved by the following technical solution.
A kind of method of association rare earth yield in raising phosphorus ore, it is characterised in that comprise the following steps：
(1) rare earth phosphate rock will be contained reaction a period of time in tank diameter is added together with appropriate mixed acid, separation of solid and liquid, obtained Containing re dip solution and leached mud, the mixed acid is mixed acid based on phosphoric acid, containing moderate amount of sulfuric acid and fluoride, mixed acid In phosphoric acid quality concentration (with P2O5Meter) for 10%~55%, sulfuric acid concentration is (with SO4 2-Meter) it is 1~15g/L, fluoride concentration (with F-Meter) it is 3~30g/L, described fluoride is hydrofluoric acid (HF) and fluosilicic acid (H2SiF6) one or both of it is mixed Compound.
(2) extraction, ion exchange adsorption, the precipitation method, crystallisation are passed through containing re dip solution by what step (1) obtained One or both of method recovering rare earth, solution after recovering rare earth in phosphoric acid regenerating stirring tank with moderate amount of sulfuric acid reaction one The section time, obtain the ore pulp of phosphoric acid and gypsum.
(3) phosphoric acid and the ore pulp of gypsum obtained step (2) carries out separation of solid and liquid, obtains phosphoric acid solution and gypsum Slag.
(4) return to step (1) is followed as mixed acid after a part of adjusting component of phosphoric acid solution open circuit obtained step (3) Ring uses, and the phosphoric acid solution of remainder is used to produce phosphoric acid.
The method of association rare earth yield in a kind of raising phosphorus ore of the present invention, what step (1) was added contains rare earth phosphate rock With the solid-liquid quality and volume ratio 1 of mixed acid:2~1:10kg/L, reaction temperature are 30 DEG C~100 DEG C, preferably 40 DEG C~90 DEG C； Reaction time is 1~10 hour, preferably 2~4 hours.
The method of association rare earth yield in a kind of raising phosphorus ore of the present invention, the sulfuric acid described in step (2) are dense for quality The industrial sulphuric acid of degree >=90%, the mol ratio of calcium ion is 0.8 in the solution after the sulfuric acid and recovering rare earth that are added:1~ 1.3:1, hybrid reaction temperature 60 C~100 DEG C, 1~4h of reaction time.
The method of association rare earth yield, the phosphoric acid and gypsum that step (2) obtains in a kind of raising phosphorus ore of the present invention Ore pulp be divided into two parts, a part as returning in the phosphoric acid regenerating stirring tank that slurry is returned to described in step (2), press by remainder Step (3) carries out separation of solid and liquid, obtains phosphoric acid solution and gypsum tailings.It is step to return the part phosphoric acid of slurry and the ore pulp of gypsum (2) 0.5~20 times of the liquor capacity after the rare-earth separating.
The present invention a kind of raising phosphorus ore in association rare earth yield method, the adjusting component described in step (4), be by The phosphoric acid solution of open circuit and water, wash heat water, sulfuric acid, active SiO2In one or more kinds of mixtures be mixed to get mixing Acid, control mixed acid in phosphoric acid quality concentration (with P2O5Meter) 20%~35%, sulfuric acid concentration is (with SO4 2-Meter) for 1~15g/L, Fluoride concentration is (with F-Meter) it is 3~30g/L.
The method of association rare earth yield in a kind of raising phosphorus ore of the present invention, the mixed acid described in step (1) is by step (4) obtain, or prepare to obtain with fluoride, sulfuric acid and water by light phosphoric acid or industrial phosphoric acid.
The method of association rare earth yield, is used based on phosphoric acid, containing appropriate sulphur in a kind of raising phosphorus ore of the present invention The mixed acid of acid and fluoride containing rare earth phosphate rock to leaching, by F in nitration mixture-Corrosion function, can will be a small amount of in phosphorus ore Rare earth thing phase dissolution of independent the rare-earth mineral phase or preservation of indissoluble in silicate, can effectively improve association rare earth in phosphorus ore Leaching rate, matched in combination with paste-making method is returned with Wet Processes of Phosphoric Acid, there is the characteristics of technique is simple, separation of solid and liquid is easy.
Brief description of the drawings
Accompanying drawing is the principle process chart of the inventive method.
Embodiment
Further explanation is made to the present invention below in conjunction with accompanying drawing.
A kind of method of association rare earth yield in raising phosphorus ore, it is 10wt%-55wt% that will contain rare earth phosphate rock with concentration P2O5、F-3~30g/L, SO4 2-1~15g/L mixed acid solution is in solid-to-liquid ratio 1:2-10 is mixed, by mixture at 30 DEG C -100 Stirring reaction 1-10 hours under the conditions of DEG C, then carry out separation of solid and liquid and obtain leached mud and the solution containing rare earth.Containing earth solution By one or both of extraction, ion exchange adsorption, the precipitation method, crystallisation method rare-earth separating, after rare-earth separating Solution mix in phosphoric acid regenerating stirring tank with mass concentration more than 90% sulfuric acid, sulphuric acid is by calcium mole in solution 0.8~1.3 times of several additions, in 60 DEG C~100 DEG C 1~4h of reaction time, phosphoric acid regeneration ore pulp is divided into two parts, wherein one Part conduct is returned slurry and returned in regenerating stirring tank, and it is to be added in regenerating stirring tank liquid after rare-earth separating to accumulate to return slurry amount 0.5~20 times, remainder phosphoric acid regeneration solid-liquid separation on ore pulp obtains phosphoric acid solution and gypsum tailings, a part of phosphoric acid solution of opening a way It is incorporated suitable quantity of water, wash heat water, sulfuric acid, active SiO2In one or more kinds of materials, obtain P2O510%~55%, F-3~ 30g/L、SO4 2-1~15g/L nitration mixture returns to leach as acid reflux contains rare earth phosphate rock, and remaining phosphoric acid solution is used for phosphoric acid by wet process Production.
The method of the present invention is further described with following nonlimiting examples, to help to understand the present invention's Content and its advantage, and determined not as limiting the scope of the present invention, protection scope of the present invention by claims.
Embodiment 1
Take 10g Phosphoric concentration bearing rare-earths and contain P2O535wt%, F-5g/L、SO4 2-5g/L phosphoric acid solution by solid-liquid quality with Volume ratio 1:10 mixing, stirring reaction 2 hours at 90 DEG C are filtrated to get filtrate and leached mud, and leached mud is weighed after drying, divided Analysis, it is 95.1% to calculate rare earth leaching rate.
Embodiment 2
Take 10g Phosphoric concentration bearing rare-earths and contain P2O535wt%, F-25g/L、SO4 2-10g/L phosphoric acid solution presses solid-liquid quality With volume ratio 1:10 mixing, stirring reaction 2 hours at 90 DEG C, filtrate and leached mud are filtrated to get, weighed after leached mud drying, Analysis, it is 98.5% to calculate rare earth leaching rate.
Embodiment 3
Take 10g Phosphoric concentration bearing rare-earths and contain P2O535wt%, F-25g/L、SO4 2-10g/L phosphoric acid solution presses solid-liquid quality With volume ratio 1:6 mixing, stirring reaction 2 hours at 90 DEG C, filtrate and leached mud are filtrated to get, weighed after leached mud drying, Analysis, it is 97.3% to calculate rare earth leaching rate.
Embodiment 4
Take 10g Phosphoric concentration bearing rare-earths and contain P2O520wt%, F-25g/L、SO4 2-10g/L phosphoric acid solution presses solid-liquid quality With volume ratio 1:10 mixing, stirring reaction 2 hours at 90 DEG C, filtrate and leached mud are filtrated to get, weighed after leached mud drying, Analysis, it is 94.6% to calculate rare earth leaching rate.
Embodiment 5
Will in above-described embodiment 1 containing earth solution by extraction rare-earth separating, the solution after rare-earth separating is pressed in solution 0.8 times of calcium molal quantity adds 98% sulfuric acid in 60 DEG C of reaction time 4h, phosphoric acid regeneration ore pulp is divided into two parts, wherein one Part conduct is returned slurry and returned in regenerating stirring tank, and it is be added in regenerating stirring tank liquid product after rare-earth separating 10 to return slurry amount Times, remainder phosphoric acid regeneration solid-liquid separation on ore pulp obtains phosphoric acid solution, open a way a part of phosphoric acid solution supplying suitable quantity of water, activity SiO2, obtain P2O535wt%, F-5g/L、SO4 2-5g/L phosphoric acid, the part phosphoric acid is returned into leaching and contains rare earth phosphate rock, by solid Liquid quality and volume ratio 1:10 at 90 DEG C stirring reaction 2 hours, slag meter rare earth leaching rate be 96.3%.
Embodiment 6
Will in above-described embodiment 2 containing earth solution by extraction rare-earth separating, the solution after rare-earth separating is pressed in solution 0.8 times of calcium molal quantity adds 98% sulfuric acid in 60 DEG C of reaction time 4h, phosphoric acid regeneration ore pulp is divided into two parts, wherein one Part conduct is returned slurry and returned in regenerating stirring tank, and it is be added in regenerating stirring tank liquid product after rare-earth separating 10 to return slurry amount Times, remainder phosphoric acid regeneration solid-liquid separation on ore pulp obtains phosphoric acid solution, open a way a part of phosphoric acid solution supplying suitable quantity of water, activity SiO2, obtain P2O535wt%, F-25g/L、SO4 2-10g/L phosphoric acid, the part phosphoric acid is returned into leaching and contains rare earth phosphate rock, is pressed Solid-liquid quality and volume ratio 1:10 at 90 DEG C stirring reaction 2 hours, slag meter rare earth leaching rate be 99%.

Claims (8)

  1. A kind of 1. method for improving association rare earth yield in phosphorus ore, it is characterised in that comprise the following steps：
    (1) rare earth phosphate rock will be contained reaction a period of time, separation of solid and liquid in tank diameter is added together with appropriate mixed acid, obtained containing dilute Native leachate and leached mud, the mixed acid are mixed acid based on phosphoric acid, containing moderate amount of sulfuric acid and fluoride, in mixed acid Phosphoric acid quality concentration is with P2O510%~55%, sulfuric acid concentration is calculated as with SO4 2-1~15g/L, fluoride concentration are calculated as with F-It is calculated as 3~30g/L, described fluoride are the mixture of one or both of hydrofluoric acid and fluosilicic acid；
    (2) pass through what step (1) obtained containing re dip solution in extraction, ion exchange adsorption, the precipitation method, crystallisation One or two kinds of method recovering rare earths, when the solution after recovering rare earth reacts one section in phosphoric acid regenerating stirring tank with moderate amount of sulfuric acid Between, obtain the ore pulp of phosphoric acid and gypsum；
    (3) phosphoric acid and the solid-liquid separation on ore pulp of gypsum obtained step (2), obtains phosphoric acid solution and gypsum tailings；
    (4) return to step (1) makes as mixed acid circulation after a part of adjusting component of phosphoric acid solution open circuit obtained step (3) With remaining phosphoric acid solution is used to produce phosphoric acid.
  2. 2. according to the method for claim 1, it is characterised in that step (1) added containing rare earth phosphate rock and mixed acid Solid-liquid quality and volume ratio 1:2~1:10kg/L, reaction temperature are 30 DEG C~100 DEG C, and the reaction time is 1~10 hour.
  3. 3. according to the method for claim 2, it is characterised in that step (1) reaction temperature is 40 DEG C~90 DEG C, the reaction time For 2~4 hours.
  4. 4. according to the method for claim 1, it is characterised in that the sulfuric acid described in step (2) is mass concentration >=90% Industrial sulphuric acid, the mol ratio of calcium ion is 0.8 in the solution after the sulfuric acid and recovering rare earth that are added:1~1.3:1, mixing is anti- Answer temperature 60 C~100 DEG C, 1~4h of reaction time.
  5. 5. according to the method for claim 1, it is characterised in that the phosphoric acid and the ore pulp of gypsum for obtaining step (2) point Into two parts, for a part as returning in the phosphoric acid regenerating stirring tank that slurry is returned to described in step (2), remainder presses step (3) Separation of solid and liquid, obtain phosphoric acid solution and gypsum tailings.
  6. 6. according to the method for claim 5, it is characterised in that it is step to return the part phosphoric acid of slurry and the ore pulp of gypsum (2) 0.5~20 times of the liquor capacity after the rare-earth separating.
  7. 7. according to the method for claim 1, it is characterised in that the adjusting component described in step (4), be by the phosphoric acid of open circuit Solution and water, wash heat water, sulfuric acid, active SiO2In one or more kinds of mixtures be mixed to get mixed acid, control is mixed Phosphoric acid quality concentration is with P in conjunction acid2O520%~35%, sulfuric acid concentration is calculated as with SO4 2-Be calculated as 1~15g/L, fluoride concentration with F-It is calculated as 3~30g/L.
  8. 8. according to the method for claim 1, it is characterised in that what the mixed acid described in step (1) was obtained by step (4), Or prepare to obtain with fluoride, sulfuric acid and water by light phosphoric acid or industrial phosphoric acid.
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CN106391293A (en) * 2016-08-30 2017-02-15 北京矿冶研究总院 Method for separating and enriching rare earth in phosphorite through mineral separation
CN112080654B (en) * 2020-09-25 2022-08-16 贵州省地质矿产中心实验室(贵州省矿产品黄金宝石制品质量检验站) Method for recovering acid and silicon from phosphorus rare earth chemical concentrate leachate
CN113355538A (en) * 2021-04-14 2021-09-07 中稀(常州)稀土新材料有限公司 Terbium oxide extraction process for treating ion ore by combining hydrochloric acid and organic extractant

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CN102312089B (en) * 2010-07-01 2013-06-05 北京矿冶研究总院 Method for recovering rare earth from rare earth-containing phosphorite
CN104862502A (en) * 2014-02-20 2015-08-26 中国科学院过程工程研究所 Cleaning smelting technology of bastnaesite and monazite mixed rare earth ore concentrate

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