CN108330301A - Bastnaesite smelts the processing method of three-phase emulsion in separation - Google Patents
Bastnaesite smelts the processing method of three-phase emulsion in separation Download PDFInfo
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- CN108330301A CN108330301A CN201711441920.7A CN201711441920A CN108330301A CN 108330301 A CN108330301 A CN 108330301A CN 201711441920 A CN201711441920 A CN 201711441920A CN 108330301 A CN108330301 A CN 108330301A
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- phase
- separation
- phase emulsion
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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
-
- 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
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline 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
- 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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
-
- 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 processing methods of fluorine-containing three-phase emulsion in fluorine carbon cerium mischmetal concentrate wet separation, are related to bastnaesite and smelt separation field.It includes collecting three-phase emulsion, and leaching agent is added thereto, the first filtrate and the first filter residue is obtained by filtration；First filter residue high-temperature alkali washes to obtain water lotion and washing slag after turning；Water lotion discharges after defluorinating agent precipitates fluorine removal；Washing slag filters to obtain the second filtrate and the second filter residue after acid solution dissolves；First filtrate is separately recovered upper organic phase and closes lower layer's rare earth water phase through stratification.This method, which smelts after the three-phase emulsion formed in separation is demulsified bastnaesite, to be separated by solid-liquid separation, and then respectively obtains organic phase, water phase and rare-earth phase from solid-liquid binary states respectively；Organic phase recycles, and is discharged after water phase fluorine removal, rare-earth phase Collection utilization makes resource obtain comprehensive reutilization, reduces the production cost of enterprise, increases benefit；After three-phase emulsion is by processing, discharged wastewater met the national standard is good for the environment.
Description
Technical field
The present invention relates to fluorine carbon cerium mischmetal concentrate wet separation field, especially a kind of bastnaesite is smelted fluorine-containing in separation
Three-phase emulsion processing method.
Background technology
Bastnaesite is the main mineral of global Rare-earth Industry, and representative mine mainly has U.S. awns court of a feudal ruler Paasche dilute
Native mine, sichuan yak level ground mine and packet header Bayan Obo mischmetal mine and Shandong Weishan Lake Rare Earth Mine.Baotou rare earth mine
For mixed type Rare Earth Mine, wherein bastnaesite：Monazite general proportions are 3:1, Sichuan bastnaesite and Shandong Weishan Lake mine category
In single bastnaesite, the Rare Earth Mine REO of both types is in 50% or so (in terms of rare earth oxide), and fluorine is 6% or so.
Sichuan fluorine carbon cerium mischmetal ore mining is with " oxidizing roasting-salt Ore Leaching-high-temperature alkali converts-washes press filtration-hydrochloric acid second
Leaching-purification of leaching liquor removal of impurities-extraction and separation-precipitation-calcining " technique.Single bastnaesite enters extraction after treatment
Liquid in contain the foreign ions such as fluorine ion.
It generates three-phase emulsion in Rare Earths Countercurrent Extraction Process to be inevitable, the main reason is that rare earth is into slot feed liquid
The factors such as the complexity that cleans are related.The main reason for such three-phase emulsion formation is to contain a certain amount of F in feed liquid-、Ba2 +、SO4 2-Equal impurity, these impurity are progressively enriched with as extraction and separation are run, and stabilization is just formed when gathering a certain amount of
Water-In-Oil shape condensate, as three-phase emulsion.There are the extractions point between water phase and organic phase, influencing rare earth for three-phase emulsion
From causing the blocking of pipeline when serious and cause to shut down.
After Sichuan bastnaesite is chemically treated, the fluorine-containing equal impurity of feed liquid are difficult to eliminate, and the generation of three-phase emulsion is outstanding
It is serious.To the three-phase emulsion processing that is generated in extraction process, there are many researchs both at home and abroad, for example three-phase emulsion is pre-
Anti-, three-phase emulsion post-processing etc..But to bastnaesite extraction separation process cause three-phase emulsion processing I
At present Yet-have be not seen in report.It is to shelve side, or bury, or burn to such three-phase emulsion majority producer, pole is not
Sharp environmental protection.Thus it is considered that very necessary to such three-phase emulsion treatment research.
Invention content
The goal of the invention of the present invention is：In view of the above problems, a kind of bastnaesite is provided to smelt three in separation
The processing method of phase emulsion, this method smelt solid-liquid point after the three-phase emulsion formed in separation is demulsified to bastnaesite
From organic phase, water phase and rare-earth phase are then respectively obtained from solid-liquid binary states respectively；And recycle organic phase, water phase is removed
It is discharged after fluorine, on the one hand rare-earth phase Collection utilization makes resource obtain comprehensive reutilization, reduce the production cost of enterprise, increases
Benefit is added；On the other hand, after three-phase emulsion is by processing, discharged wastewater met the national standard is good for the environment.
The technical solution adopted by the present invention is as follows：
Bastnaesite smelts the processing method of three-phase emulsion in separation comprising following steps：
（1）Three-phase emulsion is collected, leaching agent is added thereto, the first filtrate and the first filter residue is obtained by filtration；
（2）First filter residue is washed after alkali turns, and obtains water lotion and washing slag；Water lotion discharges after defluorinating agent precipitates fluorine removal；
Washing slag filters to obtain the second filtrate and the second filter residue after acid solution dissolves；
（3）First filtrate is clarified and is layered through standing, and upper layer is organic phase, and lower layer is rare earth water phase.
By adopting the above-described technical solution, leaching agent makes three-phase emulsion be demulsified, initial isolation is solid-liquid two-phase, filtering
Obtain the first filtrate and the first filter residue；Contain organic phase, water phase and rare-earth phase in first filtrate and the first filter residue.First filter residue
Turn by alkali and wash, realize second and be separated by solid-liquid separation, filtrate is waste water, is discharged after FLUORIDE REMOVAL IN WASTEWATER, and pollution environment, filter residue are avoided
In contain rare earth, rare earth is dissolved in acid solution and realizes separation.Water phase and organic phase in first filtrate is after stratification, organic phase
It recycles, rare earth is dissolved in water phase.On the one hand, organic phase recycles, and isolated earth solution, realizes resource
Comprehensive reutilization reduces the production cost of enterprise, increases benefit；On the other hand, discharged wastewater met the national standard is conducive to ring
It protects.
A kind of bastnaesite of the present invention smelts the processing method of three-phase emulsion in separation, step（1）In, it is described to help leaching
Agent is the sodium hydroxide solution of 4-6mol/L.
The present invention a kind of bastnaesite smelt separation in three-phase emulsion processing method, sodium hydroxide solution with it is described
The ratio between volume of three-phase emulsion is 0.5-2:1.
By adopting the above-described technical solution, sodium hydroxide changes the property of water-oil interface, emulsion droplet is made to rupture, preliminary shape
At solid-liquid two-phase.
A kind of bastnaesite of the present invention smelts the processing method of three-phase emulsion in separation, step（2）In, alkali is subcontracted
It includes：Lye is added into first filter residue, is heated 2-4 hours under the conditions of 90-110 DEG C, alkali is obtained by filtration and turns liquid and alkali turn
Slag；It is rare earth hydrate that the alkali, which turns slag,.
A kind of bastnaesite of the present invention smelts the processing method of three-phase emulsion in separation, and the lye is a concentration of 3-
The volume of the sodium hydroxide solution of 5mol/L, the lye and the first filter residue is 1:1-3.
By adopting the above-described technical solution, alkali turns to convert rare earth to the rare earth hydrate precipitation that hydrochloric acid can dissolve,
With rare-earth separating phase and organic phase and water phase.
A kind of bastnaesite of the present invention smelts the processing method of three-phase emulsion in separation, and washing is rinsed with tap water
The alkali turns slag, obtains washing slag and water lotion.
By adopting the above-described technical solution, tap water washes away the impurity that alkali turns slag surface, ensure that alkali turns the purity of slag.
A kind of bastnaesite of the present invention smelts the processing method of three-phase emulsion in separation, merges the water lotion and institute
It states alkali and turns liquid, stratification, upper organic phase recycles, and lower layer is that defluorinating agent is added in water phase, is discharged after precipitating fluorine removal.
By adopting the above-described technical solution, realizing the separation of organic phase and water phase again, organic phase recycles, water phase
It is discharged after fluorine removal, avoids pollution environment.
A kind of bastnaesite of the present invention smelts the processing method of three-phase emulsion in separation, and the defluorinating agent tries for calcic
Agent.
By adopting the above-described technical solution, containing in calcon calcium ion and fluorine ion combine form calcium fluoride precipitate,
To Removal of F- ion.
A kind of bastnaesite of the present invention smelts the processing method of three-phase emulsion in separation, is slowly added into washing slag
Mass fraction is the dissolving of 31-37% hydrochloric acid solutions, and concentration of hydrochloric acid control is filtered less than or equal to 1mol/L in liquid when terminal
To the second filtrate and the second filter residue；Second filtrate is earth solution.
It is dissolved in hydrochloric acid by adopting the above-described technical solution, alkali turns the rare-earth phase in slag, removes slightly solubility impurity.
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1. the fluorine-containing three-phase emulsion during pair bastnaesite wet separation carries out demulsification processing, it is avoided directly to shelve, cover
It buries or burns and pollute environment.
2. being separated by solid-liquid separation after demulsification, organic phase and rare-earth phase are then recycled from solid-liquid two-phase respectively, realizes the comprehensive of resource
It closes and recycles, reduce the production cost of enterprise, increase benefit.
3. abolishing the waste water obtained after processing to discharge after fluorine removal is handled, it is good for the environment.
Description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein：
Fig. 1 is that the bastnaesite of the present invention smelts the process flow chart of the processing method of three-phase emulsion in separation.
Specific implementation mode
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
This specification（Including any accessory claim, abstract）Disclosed in any feature, unless specifically stated,
It is replaced by other equivalent or with similar purpose alternative features.That is, unless specifically stated, each feature is a series of
An example in equivalent or similar characteristics.
Embodiment 1
The present embodiment provides the processing methods that a kind of bastnaesite smelts three-phase emulsion in separation, and this method is to bastnaesite smelting
The three-phase emulsion formed in refining separation is separated by solid-liquid separation after being demulsified, and is then respectively obtained from solid-liquid binary states respectively organic
Phase, water phase and rare-earth phase；And recycle organic phase, it is discharged after water phase fluorine removal, on the one hand rare-earth phase Collection utilization makes resource
Comprehensive reutilization is obtained, the production cost of enterprise is reduced, increases benefit；On the other hand, three-phase emulsion passes through processing
Afterwards, discharged wastewater met the national standard is good for the environment.This method specifically comprises the following steps：
Step 1：The three-phase emulsion in bastnaesite smelting separation is collected, according to 4mol/L sodium hydroxide solutions and three-phase breast
The volume ratio of compound is 2:1 4mol/L sodium hydroxide solutions are added into three-phase emulsion, are stirred to react 2 hours, are obtained by filtration
First filtrate and the first filter residue.
Step 2：First filtrate stands to complete layering, and upper organic phase and lower layer's rare earth water phase is separately recovered.
Step 3：The first filter residue is taken, is 1 according to the sodium hydroxide solution of 3mol/L and the volume ratio of the first filter residue:1 to its
It is middle that the sodium hydroxide solution of a concentration of 3mol/L is added, and heated 2 hours under the conditions of 110 DEG C, alkali is obtained by filtration and turns liquid and alkali
Turn slag.It takes alkali to turn slag, is rinsed with tap water, obtain water lotion and washing slag, water lotion is turned liquid with alkali to be merged, quiet
After setting layering, upper organic phase recycles, and lower water is discharged after being added to defluorinating agent precipitation fluorine removal.
Step 4：Mass fraction is slowly added to washing slag to dissolve for 31% hydrochloric acid solution, the concentration of hydrochloric acid of liquid when terminal
The second filtrate and the second filter residue is obtained by filtration less than or equal to 1mol/L in control；Second filtrate is earth solution, and the second filter residue is
Excellent molten slag.
Embodiment 2
The present embodiment provides the processing methods that a kind of bastnaesite smelts three-phase emulsion in separation, and this method is to bastnaesite smelting
The three-phase emulsion formed in refining separation is separated by solid-liquid separation after being demulsified, and is then respectively obtained from solid-liquid binary states respectively organic
Phase, water phase and rare-earth phase；And recycle organic phase, it is discharged after water phase fluorine removal, on the one hand rare-earth phase Collection utilization makes resource
Comprehensive reutilization is obtained, the production cost of enterprise is reduced, increases benefit；On the other hand, three-phase emulsion passes through processing
Afterwards, discharged wastewater met the national standard is good for the environment.This method specifically comprises the following steps：
Step 1：The three-phase emulsion in bastnaesite smelting separation is collected, according to 5mol/L sodium hydroxide solutions and three-phase breast
The volume ratio of compound is 1:1 5mol/L sodium hydroxide solutions are added into three-phase emulsion and 1h are stirred to react, using press filtration
The first filtrate and the first filter residue is obtained by filtration in mode.
Step 2：First filtrate stands to complete layering, and upper organic phase and lower layer's rare earth water phase is separately recovered.
Step 2：The first filter residue is taken, is 1 according to the sodium hydroxide solution of 4mol/L and the volume ratio of the first filter residue:2 to its
It is middle that the sodium hydroxide solution of a concentration of 4mol/L is added, and 3h is heated under the conditions of 100 DEG C, alkali is obtained by filtration and turns liquid and alkali turn
Slag.It takes alkali to turn slag, is rinsed with tap water, obtain water lotion and washing slag, water lotion is turned liquid with alkali to be merged, and is stood
After layering, upper organic phase recycles, and lower water is discharged after being added to defluorinating agent precipitation fluorine removal.
Step 4：Mass fraction is slowly added to washing slag to dissolve for 34% hydrochloric acid solution, the concentration of hydrochloric acid of liquid when terminal
The second filtrate and the second filter residue is obtained by filtration less than or equal to 1mol/L in control；Second filtrate is earth solution, and the second filter residue is
Excellent molten slag.
Embodiment 3
The present embodiment provides the processing methods that a kind of bastnaesite smelts three-phase emulsion in separation, and this method is to bastnaesite smelting
The three-phase emulsion formed in refining separation is separated by solid-liquid separation after being demulsified, and is then respectively obtained from solid-liquid binary states respectively organic
Phase, water phase and rare-earth phase；And recycle organic phase, it is discharged after water phase fluorine removal, on the one hand rare-earth phase Collection utilization makes resource
Comprehensive reutilization is obtained, the production cost of enterprise is reduced, increases benefit；On the other hand, three-phase emulsion passes through processing
Afterwards, discharged wastewater met the national standard is good for the environment.This method specifically comprises the following steps：
Step 1：The three-phase emulsion in bastnaesite smelting separation is collected, according to 6mol/L sodium hydroxide solutions and three-phase breast
The volume ratio of compound is 0.5:1 6mol/L sodium hydroxide solutions are added into three-phase emulsion, 3h are stirred to react, using press filtration
The first filtrate and the first filter residue is obtained by filtration in mode.
Step 2：First filtrate stands to complete layering, and upper organic phase and lower layer's rare earth water phase is separately recovered.
Step 2：The first filter residue is taken, is 1 according to the sodium hydroxide solution of 5mol/L and the volume ratio of the first filter residue:3 to its
It is middle that the sodium hydroxide solution of a concentration of 5mol/L is added, and 4h is heated under the conditions of 90 DEG C, it is obtained by filtration that alkali turns liquid and alkali turns slag.
It takes alkali to turn slag, is rinsed with tap water, obtain water lotion and washing slag, water lotion is turned liquid with alkali to be merged, and is stood and is divided
After layer, upper organic phase recycles, and lower water is discharged after being added to defluorinating agent precipitation fluorine removal.
Step 4：Mass fraction is slowly added to washing slag to dissolve for 34% hydrochloric acid solution, the concentration of hydrochloric acid of liquid when terminal
The second filtrate and the second filter residue is obtained by filtration less than or equal to 1mol/L in control；Second filtrate is earth solution, and the second filter residue is
Excellent molten slag.
Claims (9)
1. bastnaesite smelts the processing method of three-phase emulsion in separation, which is characterized in that it includes the following steps：
(1) three-phase emulsion is collected, leaching agent is added thereto, the first filtrate and the first filter residue is obtained by filtration；
(2) first filter residues are washed after alkali turns, and obtain water lotion and washing slag；Water lotion discharges after defluorinating agent precipitates fluorine removal；
Washing slag filters to obtain the second filtrate and the second filter residue after acid solution dissolves；
(3) first filtrates are clarified and are layered through standing, and it is rare earth water phase that upper organic phase, which is separately recovered, and closes lower layer.
2. bastnaesite according to claim 1 smelts the processing method of three-phase emulsion in separation, which is characterized in that step
Suddenly（1）In, the leaching agent is the sodium hydroxide solution of 4-6mol/L.
3. bastnaesite according to claim 2 smelts the processing method of three-phase emulsion in separation, which is characterized in that hydrogen
The ratio between sodium hydroxide solution and the volume of the three-phase emulsion are 0.5-2:1.
4. bastnaesite according to claim 1 smelts the processing method of three-phase emulsion in separation, which is characterized in that step
Suddenly（2）In, alkali, which is subcontracted, to be included：Lye is added into first filter residue, heats 2-4 hours, filters under the conditions of 90-110 DEG C
Turn liquid to alkali and alkali turns slag；It is rare earth hydrate that the alkali, which turns slag,.
5. bastnaesite according to claim 4 smelts the processing method of three-phase emulsion in separation, which is characterized in that institute
Lye is stated as the sodium hydroxide solution of a concentration of 3-5mol/L, the volume of the lye and the first filter residue is 1:1-3.
6. bastnaesite according to claim 5 smelts the processing method of three-phase emulsion in separation, which is characterized in that water
It washes and turns slag with the tap water flushing alkali, obtain washing slag and water lotion.
7. bastnaesite according to claim 6 smelts the processing method of three-phase emulsion in separation, which is characterized in that close
And the water lotion turns liquid, stratification with the alkali, upper organic phase recycles, and lower layer is that defluorinating agent is added in water phase, is sunk
It is discharged after the fluorine removal of shallow lake.
8. bastnaesite according to claim 7 smelts the processing method of three-phase emulsion in separation, which is characterized in that institute
It is containing calcon to state defluorinating agent.
9. bastnaesite according to claim 6 smelts the processing method of three-phase emulsion in separation, which is characterized in that
Mass fraction is slowly added in washing slag to dissolve for 31-37% hydrochloric acid solutions, when terminal in liquid concentration of hydrochloric acid control less than etc.
In 1mol/L, the second filtrate and the second filter residue is obtained by filtration；Second filtrate is earth solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647744A (en) * | 2020-07-01 | 2020-09-11 | 四川省冕宁县方兴稀土有限公司 | Method for recovering organic and rare earth from bastnaesite extraction three phases |
| CN113584329A (en) * | 2021-07-29 | 2021-11-02 | 赣州稀土友力科技开发有限公司 | Recovery method for extracting three-phase substances from neodymium iron boron waste |
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| CN1218113A (en) * | 1998-09-28 | 1999-06-02 | 周静 | Method for treating and recovering emulsion phase in extracting separation of raw rare earth materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647744A (en) * | 2020-07-01 | 2020-09-11 | 四川省冕宁县方兴稀土有限公司 | Method for recovering organic and rare earth from bastnaesite extraction three phases |
| CN111647744B (en) * | 2020-07-01 | 2021-09-21 | 四川省冕宁县方兴稀土有限公司 | Method for recovering organic and rare earth from bastnaesite extraction three phases |
| CN113584329A (en) * | 2021-07-29 | 2021-11-02 | 赣州稀土友力科技开发有限公司 | Recovery method for extracting three-phase substances from neodymium iron boron waste |
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Application publication date: 20180727 |