CN106148691A - A kind of alkaline process processes monazite and the technique of extracting and separating rear earth - Google Patents

A kind of alkaline process processes monazite and the technique of extracting and separating rear earth Download PDF

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CN106148691A
CN106148691A CN201510188991.5A CN201510188991A CN106148691A CN 106148691 A CN106148691 A CN 106148691A CN 201510188991 A CN201510188991 A CN 201510188991A CN 106148691 A CN106148691 A CN 106148691A
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monazite
rare earth
earth
extracting
technique
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CN106148691B (en
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李效平
王凯
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YONGZHOU XIANGJIANG RIVER RARE EARTH Co Ltd
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YONGZHOU XIANGJIANG RIVER RARE EARTH Co Ltd
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Abstract

The invention provides a kind of alkaline process and process monazite and the technique of extracting and separating rear earth; concrete scheme is to carry out alkaline process under non-oxidizable protective atmosphere to process monazite; obtain containing trivalent rare earth hydroxide; directly carry out reaction obtain the organic facies of supported rare earth with acidic extractant; trivalent cerium hydroxide has characteristic that is readily soluble and that save acid consumption relative to ceric hydroxide; rare earth is preferentially dissolved, it is achieved separate, with impurity such as indissoluble thorium dioxides, the condition of creating for follow-up faintly acid extractant;Trivalent rare earth hydroxide directly uses acidic extractant to dissolve, and uses the too high problem of acid and alkali consumption that organic liquid caustic soda or ammonia saponification mode rare-earth separating bring, and operation simplifies.

Description

A kind of alkaline process processes monazite and the technique of extracting and separating rear earth
Technical field
The present invention relates to a kind of alkaline process and process the technique that monazite and rare earth extraction separate, specifically one Plant under non-oxidizable protective atmosphere, carry out alkaline process process monazite, obtain trivalent rare earth hydroxide, directly Carry out reaction with acidic extractant and obtain the organic facies of supported rare earth, belong to Rare Earth Mine and smelt production field
Background technology
Monazite is a kind of industry Ree-phospeate Minerals, it is easy to sort, monazite minerals in the concentrate obtained Content is up to more than 95%.Industrial general employing Caustic soda decomposition method processes monazite concentrate.[" rare earth ", The first edition first volume, metallurgical industry publishing house 1978, P221-237.)] Industrial, traditional handicraft is to use caustic lye of soda and concentrate proportionally to prepare entrance decomposer, and decomposer uses Steam jacket heating makes reaction carry out at relatively high temperatures.Continuous print charging and discharging, it is ensured that under decomposition temperature Reaction, is converted by alkali and reaches the purpose that rare earth separates with phosphorus, obtain the mixing of rare earth hydrate and tertiary sodium phosphate Serosity, obtains rare earth hydrate subsequently into filtration, washing procedure, the more preferential dissolution process of hydrochloric acid produces mixed Close rare earth chloride, then use acidic extractant to carry out extract and separate, it is thus achieved that single rare earth.
During traditional handicraft caustic digestion, the rare earth formation rare-earth hydroxide of except cerium:
REPO4+3OH-=RE (OH)3+PO4 3-
Cerium is oxidized by oxygen in this process, the ceric hydroxide that generation is poorly soluble:
The thorium formation thorium dioxide of association:
Th3(PO4)4+12OH-=3Th (OH)4+4PO4 3-
Traditional rare earth extraction separate mode typically uses saponification P507 extract and separate at rare-earth chlorination objects system Rare earth element (rare earth chemistry collection of thesis, institute's nineteen eighty-two, Science Press should be changed in Changchun), the method extracts Rare-earth separating is effective, and application is wide.Extraction process use rare earth chloride as feed liquid, it is necessary to use ammonia or The saponification such as sodium hydroxide are organic, carried out through extraction section, washing section and back extraction section by fractional extraction mode Rare Earth Separation, this process produces a large amount of ammonia nitrogens or high-salt wastewater, environment causes bigger pollution.
The invention provides a kind of under non-oxidizable protective atmosphere, airtight heating carries out alkaline process and processes monazite Technique, rare earth forms trivalent rare earth hydroxide during caustic digestion, then uses acid organic extractant Directly dissolve, obtain the organic facies of supported rare earth.
Wherein alkali conversion reaction is as follows
REPO4+3OH-=RE (OH)3+PO4 3-
CePO4+3OH-=Ce (OH)3+PO4 3-
Th3(PO4)4+12OH-=3Th (OH)4+4PO4 3-
And trivalent rare earth hydroxide reacts as follows in the dissolving of acidic extractant:
RE(OH)3+ 3HA=REA3+H+
HA acidic extractant
Summary of the invention
The invention provides a kind of under non-oxidizable protective atmosphere, airtight heating carries out alkaline process and processes monazite Technique, rare earth forms trivalent rare earth hydroxide during caustic digestion, the technical scheme is that
Liquid caustic soda and monazite mixture are heated during processing monazite in hermetic container by described alkaline process Reacting, protect under non-oxidizing atmosphere, the rare earth in monazite forms three in caustic digestion process Valency rare-earth hydroxide and sodium radio-phosphate,P-32 solution, after filtration washing separates, trivalent rare earth hydroxide uses acid Property extractant dissolves, and obtains the organic facies extract and separate for rare earth of supported rare earth.
It is as follows that alkaline process processes monazite reaction
REPO4+3OH-=RE (OH)3+PO4 3-
CePO4+3OH-=Ce (OH)3+PO4 3-
Th3(PO4)4+12OH-=3Th (OH)4+4PO4 3-
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Monazite is the monazite concentrate of 30%REO-65%REO.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Liquid caustic soda is at least one in sodium hydroxide, potassium hydroxide, and alkali concn is 20%-75%, liquid caustic soda and monazite Liquid-solid ratio be 1.5:1-10:1, reaction temperature is 80 DEG C-350 DEG C.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Non-oxidizing gas includes but not limited at least one in nitrogen, argon, helium, hydrogen.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Hermetic container uses but is not limited to enclosed reactor.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Heating process can use at least one in steam heating, oil bath heating, Far-infrared Heating, eddy current electrical heating Mode of heating, preferential employing Far-infrared Heating or eddy current Electric heating.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described In trivalent rare earth hydroxide, cerium is with+trivalent state rare-earth hydroxide form existence, wherein Ce3+/ Σ Ce is 80%-100%.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Acidic extractant includes but not limited at least one in P204, P507, aphthenic acids, C272.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Acidic extractant solution temperature is 20-50 DEG C, and described organic concentrations is 0.2-1.8mol/L, according to organic negative Carrying rare earth content is that 0.02-0.2mol/L carries out the reaction that feeds intake.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Acidic extractant carries out in course of dissolution, is stored up as excellent molten slag by a small amount of insoluble matter obtained, is used for reclaiming Thorium therein, uranium.
Described a kind of alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that described Acidic extractant carries out in course of dissolution, in the case of prioritizing selection rare-earth yield is less than 99%, by obtain A small amount of insoluble matter carry out hydrochloric acid preferentially dissolve, after filtration washing, filtrate middle rare earth carries out extract and separate, excellent molten Slag muck is deposited, and is used for reclaiming thorium therein, uranium.
Described trivalent rare earth hydroxide can directly use hydrochloric acid that it is carried out excellent molten formation rare earth chloride, real Existing rare earth separates with thorium.
Described process program is equally applicable to alkaline process and processes other terres rares ore deposits such as xenotime, bastnaesite.
Beneficial effects of the present invention is as follows:
(1) have employed non-oxidizable protective atmosphere to process, it is to avoid monazite middle rare earth partition accounts for 50% Left and right Ce elements is converted into tetravalence cerium hydroxide, reduces alkaline consumption during caustic digestion.
(2) trivalent cerium hydroxide is relative to ceric hydroxide (Ce (OH)4) have readily soluble With the characteristic of saving acid consumption, directly dissolve for follow-up faintly acid extractant and preferentially dissolve rare earth, it is achieved with difficulty The separation of the impurity such as molten thorium dioxide creates condition.
(3) preferentially dissolve obtain rare earth chloride with traditional hydrochloric acid, then use organic liquid caustic soda or ammonia saponification Mode rare-earth separating technics comparing, trivalent rare earth hydroxide directly uses acidic extractant to dissolve, extracts Take separation, there is operation and simplify, the advantage saving acid and alkali consumption.
(4) preferentially dissolve compare with traditional alkaline process decomposition hydrochloric acid, trivalent cerium hydroxide acidic extractant In preferential course of dissolution, poisonous chlorine will not be generated because of quadrivalent cerium and the redox reaction of chlorine root in system Gas, it is achieved that safely cleaning produces.
(5) have employed non-oxidizable protective atmosphere, airtight heat treated, whole system be in extraneous every Suppressed to greatest extent from state, radioactive pollution and harm problem.
Detailed description of the invention
Embodiment 1
By the liquid caustic soda of monazite (ThO2 content 3.9%) that REO content is 51.2% with 40% with liquid-solid ratio it is 3:1 is placed in the reactor of nitrogen protection atmosphere, uses Far-infrared Heating to 140 DEG C of decomposition reactions, reaction slurry Material is through filtration washing, and monazite resolution ratio is 97.9%, wherein with+trivalent state cerium hydroxide in rare earth hydrate Cerium ratio Ce3+/Σ Ce that form exists is 89%, and in filtrate, recycle of alkali liquor recycles, and ton ore deposit consumes hydrogen Sodium oxide 0.57 ton.
At 20 DEG C, the P204 of rare earth hydrate alkali cake 0.2mol/L is dissolved, dissolve above-mentioned filter cake During on-the-spot without chlorine generation, obtain the organic facies that supported rare earth concentration is 0.02mol/L, the extraction of rare earth The rate of getting reaches 99.1%, the extraction yield 0.035% of thorium, it is achieved thorium and Rare Earth Separation.
Load organic separate with insoluble matter after, the organic extract and separate as single rare earth of supported rare earth dilute Earth material directly separates, and a small amount of insoluble matter is stored up as excellent molten slag, thorium therein to be recycled, uranium.
Embodiment 2
By monazite (ThO2 content 3.1%) that REO content is 31.1% with 65% liquid caustic soda with liquid-solid ratio It is placed in the reactor of argon atmosphere for 1.5:1, after employing eddy current electrical heating to 80 DEG C of decomposition reactions, Reaction paste is through filtration washing, and monazite resolution ratio is 96.5%, wherein with+trivalent state hydrogen in rare earth hydrate Cerium ratio Ce3+/Σ Ce that cerium oxide form exists is 95%, and in filtrate, recycle of alkali liquor recycles, ton ore deposit Consume sodium hydroxide 0.42 ton.
At 50 DEG C, the C272 of rare earth hydrate alkali cake 0.5mol/L is dissolved, dissolve above-mentioned During filter cake, scene produces without chlorine, obtains the organic facies that supported rare earth concentration is 0.05mol/L, rare earth Extraction yield reach 99.0%, the extraction yield of thorium be less than 0.01%, it is achieved thorium and Rare Earth Separation.
Load organic separate with insoluble matter after, supported rare earth organic facies is as the extract and separate of single rare earth Rare earth material directly separates, a small amount of insoluble matter carry out hydrochloric acid preferentially dissolve, after filtration washing, dilute in filtrate Soil carries out extract and separate, and excellent molten slag is stored up, thorium therein to be recycled, uranium.
Embodiment 3
By the liquid caustic soda of monazite (ThO2 content 4.3%) that REO content is 64.9% with 20% with liquid-solid ratio it is 10:1 is placed in the tubular reactor of helium protective atmosphere, uses after being steam heated to 345 DEG C of decomposition reactions, Reaction paste is through filtration washing, and monazite resolution ratio is 98.5%, wherein with+trivalent state hydrogen in rare earth hydrate Cerium ratio Ce3+/Σ Ce that cerium oxide form exists is 85%, and in filtrate, recycle of alkali liquor recycles, ton ore deposit Consume sodium hydroxide 0.71 ton.
At 30 DEG C, the aphthenic acids of rare earth hydrate alkali cake 0.9mol/L is dissolved, dissolve above-mentioned filter cake During on-the-spot without chlorine generation, obtain the organic facies that supported rare earth concentration is 0.09mol/L, the extraction of rare earth The rate of getting reaches 92.5%, the extraction yield 0.014% of thorium, it is achieved thorium and Rare Earth Separation.
Load organic separate with insoluble matter after, supported rare earth organic facies is as the extract and separate of single rare earth Rare earth material directly separates, a small amount of insoluble matter carry out hydrochloric acid preferentially dissolve, after filtration washing, dilute in filtrate Soil carries out extract and separate, and excellent molten slag is stored up, thorium therein to be recycled, uranium.
Embodiment 4
By the liquid caustic soda of monazite (ThO2 content 3.9%) that REO content is 51.3% with 50% with liquid-solid ratio it is 3:1 is placed in the tubular reactor of nitrogen protection atmosphere, after using oil bath to be heated to 170 DEG C of decomposition reactions, instead Answering slurry through filtration washing, monazite resolution ratio is 98.7%, wherein with+trivalent state hydrogen-oxygen in rare earth hydrate The cerium ratio Ce3+/Σ Ce changing the existence of cerium form is 100%, and in filtrate, recycle of alkali liquor recycles, and ton ore deposit disappears Consumption sodium hydroxide 0.55 ton.
At 30 DEG C, the P204 of rare earth hydrate alkali cake 1.5mol/L is dissolved, dissolve above-mentioned filter cake During on-the-spot without chlorine generation, obtain the organic facies that supported rare earth concentration is 0.17mol/L, the extraction of rare earth The rate of getting reaches 99.5%, the extraction yield 0.011% of thorium, it is achieved thorium and Rare Earth Separation.
Load organic separate with insoluble matter after, supported rare earth organic facies is as the extract and separate of single rare earth Rare earth material directly separates, and a small amount of insoluble matter is directly stored up as excellent molten slag, thorium therein to be recycled, uranium.

Claims (12)

1. an alkaline process processes monazite and the technique of extracting and separating rear earth, it is characterised in that at described alkaline process During reason monazite, liquid caustic soda and monazite mixture are heated in hermetic container and react, non-oxide Property atmosphere under protect, the rare earth in monazite forms trivalent rare earth hydroxide and phosphorus in caustic digestion process Acid sodium solution, after filtration washing separates, trivalent rare earth hydroxide uses acidic extractant to dissolve, Obtain the organic facies extract and separate for rare earth of supported rare earth.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, and it is special Levying and be, described monazite is the monazite concentrate of 30%REO-65%REO.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, and it is special Levying and be, described liquid caustic soda is at least one in sodium hydroxide, potassium hydroxide, and alkali concn is 20%-75%, Liquid caustic soda is 1.5:1-10:1 with the liquid-solid ratio of monazite, and reaction temperature is 80 DEG C-350 DEG C.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, and it is special Levying and be, described non-oxidizing gas includes but not limited in nitrogen, argon, helium, hydrogen at least A kind of.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, and it is special Levying and be, described hermetic container uses but is not limited to enclosed reactor.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, and it is special Levying and be, described heating process can use steam heating, oil bath heating, Far-infrared Heating, eddy current electricity to add At least one mode of heating hankered, preferential employing Far-infrared Heating or eddy current Electric heating.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, and it is special Levying and be, in described trivalent rare earth hydroxide, cerium is with+trivalent state rare-earth hydroxide form existence, its Middle Ce3+/ Σ Ce is 80%-100%.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, and it is special Levying and be, described acidic extractant includes but not limited in P204, P507, aphthenic acids, C272 extremely Few one.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, and it is special Levying and be, described acidic extractant solution temperature is 20-50 DEG C, and described organic concentrations is 0.2-1.8mol/L, is that 0.02-0.2mol/L carries out the reaction that feeds intake according to organic load rare earth content.
A kind of alkaline process the most according to claim 1 processes monazite and the technique of extracting and separating rear earth, It is characterized in that, described acidic extractant carries out in course of dissolution, using a small amount of insoluble matter of obtaining as excellent Molten slag is stored up, and is used for reclaiming thorium therein, uranium.
11. a kind of alkaline process according to claim 1 process monazite and the technique of extracting and separating rear earth, It is characterized in that, described acidic extractant carries out in course of dissolution, and prioritizing selection rare-earth yield is less than 99% In the case of, a small amount of insoluble matter obtained is carried out hydrochloric acid preferentially dissolve, after filtration washing, filtrate middle rare earth Carrying out extract and separate, excellent molten slag is stored up, and is used for reclaiming thorium therein, uranium.
12. a kind of alkaline process according to claim 1 process monazite and the technique of extracting and separating rear earth, It is characterized in that, described trivalent rare earth hydroxide can directly use hydrochloric acid that it is carried out excellent molten formation chlorination Rare earth, it is achieved rare earth separates with thorium.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112126802A (en) * 2020-08-14 2020-12-25 南昌大学 Rare earth alkaline precipitation, conversion, decomposition and separation method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1142542A (en) * 1995-07-04 1997-02-12 山东微山华能稀土总公司 Process and apparatus for preparing chlorinated rare-earth from fine rare-earth minerals by alkali water heating process
CN102212674A (en) * 2011-05-12 2011-10-12 包头稀土研究院 Process for comprehensively recovering liquid alkali roasting resource of mixed rare earth concentrate
CN103014333A (en) * 2012-11-27 2013-04-03 益阳鸿源稀土有限责任公司 Separation and recovery method of uranium, thorium and rare earth in monazite slag
CN103103349A (en) * 2013-02-05 2013-05-15 内蒙古科技大学 Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1142542A (en) * 1995-07-04 1997-02-12 山东微山华能稀土总公司 Process and apparatus for preparing chlorinated rare-earth from fine rare-earth minerals by alkali water heating process
CN102212674A (en) * 2011-05-12 2011-10-12 包头稀土研究院 Process for comprehensively recovering liquid alkali roasting resource of mixed rare earth concentrate
CN103014333A (en) * 2012-11-27 2013-04-03 益阳鸿源稀土有限责任公司 Separation and recovery method of uranium, thorium and rare earth in monazite slag
CN103103349A (en) * 2013-02-05 2013-05-15 内蒙古科技大学 Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112126802A (en) * 2020-08-14 2020-12-25 南昌大学 Rare earth alkaline precipitation, conversion, decomposition and separation method

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