CN110129562A - A kind of method for saponification of rare earth organic extractant - Google Patents
A kind of method for saponification of rare earth organic extractant Download PDFInfo
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- CN110129562A CN110129562A CN201910592160.2A CN201910592160A CN110129562A CN 110129562 A CN110129562 A CN 110129562A CN 201910592160 A CN201910592160 A CN 201910592160A CN 110129562 A CN110129562 A CN 110129562A
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- rare earth
- saponification
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- organic extractant
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
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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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
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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
- 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 kind of method for saponification of rare earth organic extractant, are related to rare earth organic extractant saponification field, are to solve clarification limewash and carry out the problem of saponification lacks operability.Specific step is as follows: step 1 by the present invention, raw ore dissolution；Step 2 adjusts enrichment thing liquid；Step 3, preparation extraction agent solution；Step 4, saponification.The sodium ion for being difficult to remove is not introduced into process flow of the invention, ammonium hydroxide only plays the effect for adjusting pH value, is not the source for being saponified lye, ammonia-nitrogen content is few in waste water, the purity is high of product；Conventional clarification limewash is replaced to be saponified using 92% or more active calcium hydroxide pulvis in the present invention, water phase volume reduces about half, reduces the discharge amount of ammonia nitrogen waste water, and it is lower to be saponified cost compared to soda and ammonia alkali for calcium hydroxide pulvis；Calcium chloride is recyclable in waste water of the invention, and environmental pollution is small, and has economic value.
Description
Technical field
The present invention relates to rare earth organic extractants to be saponified field, the method for saponification of specifically a kind of rare earth organic extractant.
Background technique
Rare-earth original ore extraction and separation technology is by the molten rear resulting mixed chlorinated rare earth solution of raw ore acid, is extraction with P507
Agent, kerosene are dispersing agent, the extracting rare-earth after ammonium hydroxide is saponified, according to separation different between each rare earth element, by tandem
After extraction and separation, each rare earth element is gradually separated, obtains the technology of single high-purity rare-earth chloride enriched substance solution.
In old production technology, ammonium hydroxide as saponification raw material, have be saponified it is high-efficient, do not introduce the advantages such as new impurity, but
Cost of material is high, and ammonia nitrogen waste water pollution on the environment is serious, therefore ammonium hydroxide saponification process is eliminated substantially.
Domestic existing rare earth extraction object organic phase saponification mostly uses soda to replace ammonium hydroxide, it is advantageous that saponification waste-water pair
Environmental pollution is small, is saponified stabilised efficiency, and defect is that new impurity sodium ion, the rare-earth oxidation of this production technology output can be introduced
For object generally up to 2N grades, small part is having extreme high purity that the optomagnetic of (5N grades) is required to wait fields rare earth oxide up to 3N grades
Application be restricted.
Calcium hydroxide saponification is one of the emphasis direction of rare-earth sodium saponification technological transformation in recent years.In water due to calcium hydroxide
Solubility it is smaller, the basicity of clear limewash is only 0.02mol/L or so, directly with clarification limewash saponification need it is larger
Water phase volume, to saponification equipment requirement it is excessively high.Usually the saponification number of organic phase is 0.5mol/L in production, that is, is saponified 1 volume
Organic phase needs 0.1 volume of ammonium hydroxide of 5mol/L, and clarifies limewash and then need 25 volumes.Water phase volume mistake after the completion of saponification
Greatly, it will lead to larger with the organic phase loss for abandoning water discharge.Therefore, it is saponified using clarification limewash and is also lacked in actual production
Weary operability.
Summary of the invention
The purpose of the present invention is to provide a kind of method for saponification of rare earth organic extractant, to solve in above-mentioned background technique
The problem of proposition.
To achieve the above object, the invention provides the following technical scheme:
A kind of method for saponification of rare earth organic extractant, the specific steps are as follows:
Raw ore dissolution: step 1 rare-earth original ore calcination is crushed, rare-earth original ore powder is obtained, by rare-earth original ore powder and quality
The mixed in hydrochloric acid of score 32-39%, in a kettle heating stirring are further continued for being added the hydrochloric acid of mass fraction 32-39% to solid
It no longer reduces, is separated by solid-liquid separation after being cooled to room temperature, obtain mixed rare earth chlorides solution；
Step 2 adjusts enrichment thing liquid: ammonium hydroxide being added into mixed rare earth chlorides solution, adjusts pH to neutrality, pure water is added
Into solution, rare earth ion concentration is 1.4mol/L, obtains rare earth ion enrichment thing liquid；
Preparation extraction agent solution: step 3 solvent and dispersing agent is mixed according to mass ratio 1:1.3-1.8 stirring at normal temperature, are made
Extract agent solution；
Saponification: rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water and saponification is added by step 4
Pond, is stirred and stratification, upper organic phase are target product, and upper organic phase enters separating and extracting program and becomes
Rare earth oxide or the raw material of chloride preparation, lower layer's water phase enter calcium chloride reclaimer.
As a further solution of the present invention: the mixed in hydrochloric acid of rare-earth original ore powder and mass fraction 32-39% in step 1
When rare earth ion and chloride ion molar ratio be 1:2-4.
As a further solution of the present invention: heating temperature is 52-59 DEG C, mixing time 2-3h in step 1, solid-liquid
Isolated mode is filters pressing.
As a further solution of the present invention: the molar ratio of rare earth ion and the ammonium ion in ammonium hydroxide is 1 in step 2:
0.1-0.6。
As a further solution of the present invention: solvent is P507 in step 3, and dispersing agent is kerosene.
As a further solution of the present invention: rare earth ion enrichment thing liquid, extraction agent solution, calcium hydroxide powder in step 4
The mass ratio of agent and pure water is 1:1:0.03:9.5-10.4.
As a further solution of the present invention: whipping temp is room temperature, mixing time 4-6h in step 4.
Compared with prior art, the beneficial effects of the present invention are:
The sodium ion for being difficult to remove is not introduced into process flow of the invention, it is not soap that ammonium hydroxide, which only plays the effect for adjusting pH value,
The source of choline liquid, ammonia-nitrogen content is few in waste water, the purity is high of product；
In the present invention using 92% or more purity, partial size 800-1000 mesh calcium hydroxide pulvis replace conventional clarification limewash into
Row saponification, water phase volume reduce about half, reduce the discharge amount of ammonia nitrogen waste water, calcium hydroxide pulvis is compared to soda and ammonia
Alkali, saponification cost are lower；
Calcium chloride is recyclable in waste water of the invention, and environmental pollution is small, and has economic value, before wide application
Scape is recycled according to pilot experiment as a result, the calcium constituent rate of recovery can reach 60% ~ 75%.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
A kind of method for saponification of rare earth organic extractant, the specific steps are as follows:
Raw ore dissolution: step 1 rare-earth original ore calcination is crushed, rare-earth original ore powder is obtained, by rare-earth original ore powder and quality
Mole of rare earth ion and chloride ion when the mixed in hydrochloric acid of the mixed in hydrochloric acid of score 32%, rare-earth original ore powder and mass fraction 32%
Than being heated to 52 DEG C in a kettle and stirring 2.4h for 1:2, it is further continued for that the hydrochloric acid of mass fraction 32% is added to solid not
It reduces, is separated by solid-liquid separation by the way of filters pressing after being cooled to room temperature again, obtain mixed rare earth chlorides solution；
Step 2 adjusts enrichment thing liquid: ammonium hydroxide being added into mixed rare earth chlorides solution, adjusts pH to neutrality, pure water is added
Into solution, rare earth ion concentration is 1.4mol/L, obtains rare earth ion enrichment thing liquid；
Preparation extraction agent solution: step 3 solvent and dispersing agent is mixed according to mass ratio 1:1.3 stirring at normal temperature, extraction is made
Agent solution；
Saponification: rare earth ion is enriched with thing liquid, extraction agent solution, activity and added for 92% calcium hydroxide pulvis and pure water by step 4
Enter saponification pond, the mass ratio that rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water is 1:1:
0.03:9.5, is stirred and stratification, upper organic phase are target product, and upper organic phase enters separating and extracting program
The raw material of rare earth oxide or chloride preparation is become, lower layer's water phase enters calcium chloride reclaimer.
Embodiment 2
A kind of method for saponification of rare earth organic extractant, the specific steps are as follows:
Raw ore dissolution: step 1 rare-earth original ore calcination is crushed, rare-earth original ore powder is obtained, by rare-earth original ore powder and quality
Mole of rare earth ion and chloride ion when the mixed in hydrochloric acid of the mixed in hydrochloric acid of score 38%, rare-earth original ore powder and mass fraction 38%
Than for 1:3.2, heating stirring, the hydrochloric acid for being further continued for being added mass fraction 38% are no longer reduced to solid, are cooled in a kettle
It is separated by solid-liquid separation after room temperature, obtains mixed rare earth chlorides solution；
Step 2 adjusts enrichment thing liquid: ammonium hydroxide being added into mixed rare earth chlorides solution, adjusts pH to neutrality, rare earth ion
Molar ratio with the ammonium ion in ammonium hydroxide is 1:0.1, and it is 1.4mol/L that pure water rare earth ion concentration into solution, which is added, is obtained
Rare earth ion is enriched with thing liquid；
Preparation extraction agent solution: step 3 P507 and kerosene is mixed according to mass ratio 1:1.6 stirring at normal temperature, extractant is made
Solution；
Saponification: rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water and saponification is added by step 4
Pond, stirring at normal temperature 5.2h and stratification, upper organic phase are target product, and upper organic phase enters separating and extracting journey
Sequence becomes the raw material of rare earth oxide or chloride preparation, and lower layer's water phase enters calcium chloride reclaimer.
Embodiment 3
A kind of method for saponification of rare earth organic extractant, the specific steps are as follows:
Raw ore dissolution: step 1 rare-earth original ore calcination is crushed, rare-earth original ore powder is obtained, by rare-earth original ore powder and quality
Mole of rare earth ion and chloride ion when the mixed in hydrochloric acid of the mixed in hydrochloric acid of score 35%, rare-earth original ore powder and mass fraction 35%
Than being heated to 55 DEG C in a kettle and stirring 3h for 1:4, it is further continued for that the hydrochloric acid of mass fraction 35% is added to solid no longer
It reduces, is separated by solid-liquid separation by the way of filters pressing after being cooled to room temperature, obtains mixed rare earth chlorides solution；
Step 2 adjusts enrichment thing liquid: ammonium hydroxide, the ammonium root in rare earth ion and ammonium hydroxide being added into mixed rare earth chlorides solution
The molar ratio of ion is 1:0.45, adjusts pH to neutrality, it is 1.4mol/L that pure water rare earth ion concentration into solution, which is added, is obtained
Rare earth ion is enriched with thing liquid；
Preparation extraction agent solution: step 3 P507 and kerosene is mixed according to mass ratio 1:1.5 stirring at normal temperature, extractant is made
Solution；
Saponification: rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water and saponification is added by step 4
Pond, the mass ratio that rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water is 1:1:0.03:10, and room temperature stirs
6h and stratification are mixed, upper organic phase is target product, and upper organic phase enters separating and extracting program and becomes dilute
Native oxide or the raw material of chloride preparation, lower layer's water phase enter calcium chloride reclaimer.
Embodiment 4
A kind of method for saponification of rare earth organic extractant, the specific steps are as follows:
Raw ore dissolution: step 1 rare-earth original ore calcination is crushed, rare-earth original ore powder is obtained, by rare-earth original ore powder and quality
Mole of rare earth ion and chloride ion when the mixed in hydrochloric acid of the mixed in hydrochloric acid of score 39%, rare-earth original ore powder and mass fraction 39%
Than for 1:3.3, heating stirring, the hydrochloric acid for being further continued for being added mass fraction 39% are no longer reduced to solid, are cooled in a kettle
It is separated by solid-liquid separation after room temperature, obtains mixed rare earth chlorides solution；
Step 2 adjusts enrichment thing liquid: ammonium hydroxide, the ammonium root in rare earth ion and ammonium hydroxide being added into mixed rare earth chlorides solution
The molar ratio of ion is 1:0.6, adjusts pH to neutrality, it is 1.4mol/L that pure water rare earth ion concentration into solution, which is added, is obtained
Rare earth ion is enriched with thing liquid；
Preparation extraction agent solution: step 3 solvent and dispersing agent is mixed according to mass ratio 1:1.3-1.8 stirring at normal temperature, are made
Extract agent solution；
Saponification: rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water and saponification is added by step 4
Pond, the mass ratio that rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water is 1:1:0.03:10.4, room temperature
Stir 4.8h and stratification, upper organic phase is target product, and upper organic phase enters separating and extracting program
For raw material prepared by rare earth oxide or chloride, lower layer's water phase enters calcium chloride reclaimer.
The working principle of the invention is: raw ore first quantitatively puts into hydrochloric acid when dissolving, and directly throws relative to conventional excess acid
Production cost can be reduced by entering；Again plus hydrochloric acid is to solid that no longer to reduce be to dissolve the complete other impurities of unreacted in raw ore.
It adjusts according to the grade of raw ore difference when being enriched with thing liquid, the amount floating range that ammonium hydroxide is added is very big.
Upper organic phase enters separating and extracting program after saponification, the specific process parameter of program according to target product (lanthanum,
Cerium, praseodymium, neodymium, samarium, europium, gadolinium etc.) difference and product purity require have larger difference.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (7)
1. a kind of method for saponification of rare earth organic extractant, which is characterized in that specific step is as follows:
Raw ore dissolution: step 1 rare-earth original ore calcination is crushed, rare-earth original ore powder is obtained, by rare-earth original ore powder and quality
The mixed in hydrochloric acid of score 32-39%, heating stirring, the hydrochloric acid for being further continued for being added mass fraction 32-39% is no longer reduced to solid, cold
But to being separated by solid-liquid separation after room temperature, mixed rare earth chlorides solution is obtained；
Step 2 adjusts enrichment thing liquid: ammonium hydroxide being added into mixed rare earth chlorides solution, adjusts pH to neutrality, pure water is added
Into solution, rare earth ion concentration is 1.4mol/L, obtains rare earth ion enrichment thing liquid；
Preparation extraction agent solution: step 3 solvent and dispersing agent is mixed according to mass ratio 1:1.3-1.8 stirring at normal temperature, are made
Extract agent solution；
Saponification: rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water and saponification is added by step 4
Pond, stirring and stratification.
2. a kind of method for saponification of rare earth organic extractant according to claim 1, which is characterized in that in the step 1
The molar ratio of rare earth ion and chloride ion is 1:2-4 when the mixed in hydrochloric acid of rare-earth original ore powder and mass fraction 32-39%.
3. a kind of method for saponification of rare earth organic extractant according to claim 1 or 2, which is characterized in that the step
Heating temperature is 52-59 DEG C, mixing time 2-3h in one, and the mode of separation of solid and liquid is filters pressing.
4. a kind of method for saponification of rare earth organic extractant according to claim 1, which is characterized in that in the step 2
The molar ratio of ammonium ion in rare earth ion and ammonium hydroxide is 1:0.1-0.6.
5. a kind of method for saponification of rare earth organic extractant according to claim 1, which is characterized in that in the step 3
Solvent is P507, and dispersing agent is kerosene.
6. a kind of method for saponification of rare earth organic extractant according to claim 1, which is characterized in that in the step 4
The mass ratio that rare earth ion is enriched with thing liquid, extraction agent solution, calcium hydroxide pulvis and pure water is 1:1:0.03:9.5-10.4.
7. a kind of method for saponification of rare earth organic extractant according to claim 6, which is characterized in that in the step 4
Whipping temp is room temperature, mixing time 4-6h.
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| CN201910592160.2A CN110129562A (en) | 2019-07-03 | 2019-07-03 | A kind of method for saponification of rare earth organic extractant |
| PCT/CN2020/096112 WO2021000721A1 (en) | 2019-07-03 | 2020-06-15 | Method for saponifying rare-earth organic extractant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021000721A1 (en) * | 2019-07-03 | 2021-01-07 | 德庆兴邦稀土新材料有限公司 | Method for saponifying rare-earth organic extractant |
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| CN1125261A (en) * | 1995-11-08 | 1996-06-26 | 北京大学 | Organic phase continuous saponification technique |
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| CN110129562A (en) * | 2019-07-03 | 2019-08-16 | 德庆兴邦稀土新材料有限公司 | A kind of method for saponification of rare earth organic extractant |
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2019
- 2019-07-03 CN CN201910592160.2A patent/CN110129562A/en active Pending
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| CN101319275A (en) * | 2007-06-04 | 2008-12-10 | 北京有色金属研究总院 | Process for solvent extraction separation purification of rare earth element |
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