CN204298445U - The abstraction impurity removal system of mishmetal feed liquid - Google Patents
The abstraction impurity removal system of mishmetal feed liquid Download PDFInfo
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- CN204298445U CN204298445U CN201420629369.4U CN201420629369U CN204298445U CN 204298445 U CN204298445 U CN 204298445U CN 201420629369 U CN201420629369 U CN 201420629369U CN 204298445 U CN204298445 U CN 204298445U
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- Prior art keywords
- feed liquid
- mishmetal
- impurity removal
- abstraction impurity
- removal system
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- 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
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Abstract
An abstraction impurity removal system for mishmetal feed liquid, is characterized in that, comprise feed liquid compounding system before removal of impurities, it comprises the acid dissolve device with whipping appts, and it is provided with technical hydrochloric acid upstream end and mishmetal raw material upstream end; Organic phase dispenser; Extracting system, it comprises the agitation vat be connected with feed liquid compounding system before described removal of impurities and organic phase dispenser, and described agitation vat connects solid feeding machine, aqueous phase filtration unit and load organic phases concentrator.The utility model can remove iron, aluminium impurity in mixed chlorinated rare earth feed liquid.
Description
Technical field
The utility model relates to the abstraction impurity removal system of mishmetal feed liquid, and it utilizes the solvent-extracted method degree of depth to remove impurity elements of ferrum, the aluminium of mishmetal feed liquid.
Background technology
In Rare Earth Separation industry, for mishmetal raw material, now adopt traditional technology dissolved ions type mishmetal raw material (oxide compound or carbonate) of dissolving with hydrochloric acid, hydrolysis removal of impurities, the heavy molten recovering rare earth of hydrolysis residue.
This technological operation is numerous and diverse, energy consumption is high, filtration difficulty, straight yield of rare earth are low.
Especially, the removal of impurity aluminum is incomplete, together enters extraction system in company with rare earth feed liquid, directly affects the quality of various product separation on the one hand, causes extraction process easily to produce emulsion on the other hand, thus affects device processes ability.
In product solution, the control method of aluminium content often needs to remove with oxalate precipitation method.In addition, due to the existence of impurity element aluminium, the following process of rare-earth products is also very unfavorable.
Up to now, in Rare Earth Separation enterprise, fail to solve this difficult problem always.
Utility model content
The purpose of this utility model is to provide a kind of abstraction impurity removal system of mishmetal feed liquid, can remove iron, aluminium impurity in mixed chlorinated rare earth feed liquid.
For this reason, the utility model provides a kind of abstraction impurity removal system of mishmetal feed liquid, it is characterized in that, comprises
Feed liquid compounding system before removal of impurities, it comprises the acid dissolve device with whipping appts, and it is provided with technical hydrochloric acid upstream end and mishmetal raw material upstream end;
Organic phase dispenser;
Extracting system, it comprises the agitation vat be connected with feed liquid compounding system before described removal of impurities and organic phase dispenser, and described agitation vat connects solid feeding machine, aqueous phase filtration unit and load organic phases concentrator.
Preferably, back extraction system is also comprised.
Preferably, described back extraction system is connected with described load organic phases concentrator.
Preferably, described back extraction system comprises extraction tank, settler, filtration unit, calcination retrieving arrangement.
Preferably, described extraction tank is connected with organic phase dispenser.
Preferably, described calcination retrieving arrangement is connected with mishmetal raw material upstream end.
Preferably, before described removal of impurities, feed liquid compounding system also comprises filtering system and store holder.
Preferably, described store holder is connected with the agitation vat of extracting system.
Preferably, described store holder is provided with and exchanges hydrochloric acid upstream end.
Preferably, described store holder is with pump circulation device or whipping appts.
According to the abstraction impurity removal system of mishmetal feed liquid of the present utility model, iron, aluminium impurity can be removed in mixed chlorinated rare earth feed liquid.
Accompanying drawing explanation
Fig. 1 is the schema of the abstraction impurity removal method according to mishmetal feed liquid of the present utility model.
Fig. 2 is the abstraction impurity removal system architecture schematic diagram according to mishmetal feed liquid of the present utility model.
Embodiment
As shown in Figure 1-2, the abstraction impurity removal system of the mishmetal feed liquid of the utility model employing comprises acid dissolve device 1, technical hydrochloric acid upstream end 2, mishmetal raw material upstream end 3, filtration unit 4, liquid storing barrel 5, exchanges hydrochloric acid upstream end 6, agitation vat 7, organic phase dispenser 8, solid feeding machine 9, filtration unit 10, load organic phases concentrator 11,6N hydrochloric acid upstream end 12, extraction tank 13, settler 14, filtering system 15, calcination retrieving arrangement 16.
1, dissolving with hydrochloric acid and filtration
In one embodiment, conventional molten miner's skill can be adopted, do not need to do any transformation.Mishmetal carbonate or oxide compound and technical hydrochloric acid are added acid dissolve device 1 respectively by mishmetal raw material upstream end 3 and technical hydrochloric acid upstream end 2 dissolve, dissolve and arrive acidity 0.2N completely, device 4 filtered while hot removes mechanical foreign material after filtration.The rare earth filtered is transferred to liquid storing barrel 5 and is waited to prepare burden.Preferably can be incubated more than 40 DEG C.
2, rare earth feed liquid preparation
Requirement: acidity 0.15-0.25N.
Exchange hydrochloric acid is added in liquid storing barrel 5 (or agitation vat 7), with acid-soluble good rare earth feed liquid mixed configuration, according to the effective volume V of liquid storing barrel by exchanging hydrochloric acid upstream end 6
material, calculate the volume V adding and exchange hydrochloric acid
hand over.Feed pump circulates or stirs, and sample examination rare earth concentration, impurity iron, aluminium content, then, the feed liquid that this barrel prepares deposits more than 48 hours.
Add the volume exchanging hydrochloric acid to calculate as follows: V
hand over=V
material* 0.20/N
hand over
3, rare earth feed liquid extraction deironing, aluminium
(1) organic phase preparation
Carry out in organic phase dispenser 8, acidic extractant A concentration 0.5-0.7M, or 20% acidic extractant A, 20% auxiliary reagent B, 60% sulfonated kerosene.
(2) calculating of saponifying agent bicarbonate of ammonia consumption
A. H excessive in and in feed liquid
+the bicarbonate of ammonia consumed:
Material liquid volume (liter) * 0.20*0.079 (kg)
B. the H produced in and when extracting iron ion
+the bicarbonate of ammonia consumed:
Content (grams per liter) ÷ 55.85*3*0.079 (kg) of iron in material liquid volume (liter) * feed liquid
C. the H produced in and when extracting aluminum ion
+the bicarbonate of ammonia consumed:
Content (grams per liter) ÷ 27*3*0.079 (kg) of aluminium in material liquid volume (liter) * feed liquid
The bicarbonate of ammonia amount that above three kinds of summations consumed will consume when being rare earth feed liquid extraction deironing, aluminium, selects excessive 30-40% during actually operating.
(3) rare earth feed liquid extraction deironing, aluminium
Proper handling determines straight yield of rare earth and impurity-eliminating effect.Complete in agitation vat 7, require to stir, and have certain stirring intensity.
Abstraction impurity removal is compared (organic phase/feed liquid): 1-3/1, determines (iron, aluminium content are higher, compare larger), temperature of reaction 25 DEG C (more preferably greater than 25 DEG C) according to iron, aluminium content in mishmetal raw material.
According to the effective volume of agitation vat add in agitation vat prepare and deposit the rare earth feed liquid of more than 48 hours and non-saponification organic phase, start stirring, in 480 minutes, evenly add the bicarbonate of ammonia of calculated amount with solid feeding machine 9.
After adding, continue stirring 60 minutes, clarify 8 hours, aqueous phase after filtration device 10 obtains qualified rare earth feed liquid after filtering, load organic phases enters load organic phases concentrator 11, then pass into extraction tank 13, add 6N hydrochloric acid by 6N hydrochloric acid upstream end 12 and carry out continuous back extraction, blank organic phase returns in organic phase configurator 8 and recycles, strip aqueous is concentrated and is led to settler 14, after adding oxalic acid precipitation, after being filtered by filtering system 15, through calcination retrieving arrangement 16 recovering rare earth.
Except the rare earth feed liquid after complete iron, aluminium is limpid, in rose-red color, pH4.5-5, directly can enter P507 extraction system and carry out extracting and separating.
According to the chemical equation of bicarbonate of ammonia and acid-respons, often consume the bicarbonate of ammonia of 79 grams by the water of generation 18 grams.Therefore, consume double centner bicarbonate of ammonia by generation 3 premium on currency, after calculating rare earth feed liquid purification and impurity removal, when straight yield of rare earth or volume, this factor should be considered.
The utility model can reach the target of deep iron removal, aluminium, simple to operate, and impurity-eliminating effect is stablized, and whole flow process base closed circulation, substantially produce without three-phase, rare earth free of losses, rare earth total recovery is close to 100%.
More specifically, prepare about feed liquid:
1) in process for preparation, add exchanged acid is that the positively charged ion such as iron, aluminium is eliminated, so add exchanged acid can not bring the impurity elements such as iron aluminium into because exchanged acid has carried out ion exchange treatment on the basis of technical hydrochloric acid;
2) feed liquid requirement acidity 0.15-0.2N deposit 48 hours, main purpose: one is the Fe allowed in mishmetal feed liquid
2+ion is all oxidized to Fe
3+ion, so that iron can enter organic phase in abstraction impurity removal process; Two is, at the bottom of allowing the suspended substance in rare earth feed liquid sink to completely barrel, make rare earth feed liquid limpid, avoid the generation of emulsion in abstraction impurity removal process.
The object that raffinate filters is, extraction deironing, " three-phase " that may be formed in aluminium process can not be entered in qualified rare earth feed liquid, in order to avoid have an impact to follow-up extraction and separation technology.
The object of load organic phases continuous back extraction in extraction tank that abstraction impurity removal is formed: one is allow blank machine phase not iron content, aluminium and rare earth, is beneficial to recycle; Two is to reduce production cost, because the strip liquor spent acid of the multistage back extraction of extraction tank is lower than the back extraction of single-stage agitation vat, acid consumption is lower, and meanwhile, because spent acid is lower, the ammoniacal liquor consumed during oxalic acid precipitation recovering rare earth is also less.
Strip aqueous concentrates the object of oxalic acid precipitation recovering rare earth: one is the rare earth yield guaranteeing whole impurity removed system; Two be oxalic acid precipitation high ferro, aluminium impurity strip liquor time, rare earth and oxalic acid form oxalic rare earth precipitates thing, and the foreign ion such as iron, aluminium then forms water-soluble complex compound with oxalic acid, realize being separated of the foreign ions such as iron aluminium and rare earth.General effect is: the foreign ions such as iron aluminium are with discharge of wastewater (iron aluminium has outlet), and rare earth ion returns body series.
The abstraction impurity removal method implementing mishmetal feed liquid of the present utility model comprises the steps:
Feed liquid preparation before removal of impurities: acidity control, at 0.15-0.25N, stirs, and at least displays 48 hours;
Organic phase is prepared: acidic extractant A concentration is 0.5-0.7M; Or, 20% extraction agent A, 20% auxiliary reagent B, 60% sulfonated kerosene;
Rare earth feed liquid extraction deironing, aluminium: operating process completes in agitation vat, stirs, and has certain stirring intensity; Abstraction impurity removal is compared (organic phase/feed liquid): 1-3/1, determines (iron, aluminium content are higher, compare larger), temperature of reaction 25 DEG C (more preferably greater than 25 DEG C) according to iron, aluminium content in mishmetal raw material; Add the solid soap agent bicarbonate of ammonia determined by calculated value while stirring; In 8 hours, the bicarbonate of ammonia of calculated amount is evenly added with solid feeding machine; Add rear continuation stirring 60 minutes, clarify 8 hours; Aqueous phase metre filter after removal of impurities.
Preferably, at dissolving with hydrochloric acid and filtration step, mishmetal carbonate or oxide salt acid dissolve are arrived acidity 0.2N completely, filtered while hot is except mechanical foreign material; The earth solution filtered is transferred to liquid storing barrel and is treated batching (preferably insulation is more than 40 DEG C).
Preferably, in rare earth feed liquid preparation steps, the acid-soluble good rare earth feed liquid of acidity 0.15-0.25N is added exchange hydrochloric acid, according to the effective volume V of liquid storing barrel
material, calculate the volume V adding and exchange hydrochloric acid
hand over; Feed pump circulates or stirs, sample examination rare earth concentration, impurity iron, aluminium content, and then, the feed liquid that this barrel prepares deposits more than 48 hours; Add the volume V exchanging hydrochloric acid
hand over=V
material* 0.20/N
hand over.
Preferably, be following three sums by the saponifying agent bicarbonate of ammonia consumption of consumption when rare earth feed liquid extraction deironing, aluminium: in and H excessive in feed liquid
+the bicarbonate of ammonia consumed: material liquid volume (liter) * 0.20*0.079 (kg); The H produced during neutralization extraction iron ion
+the bicarbonate of ammonia consumed: content (grams per liter) ÷ 55.85*3*0.079 (kg) of iron in material liquid volume (liter) * feed liquid; The H produced during neutralization extraction aluminum ion
+the bicarbonate of ammonia consumed: content (grams per liter) ÷ 27*3*0.079 (kg) of aluminium in material liquid volume (liter) * feed liquid, then select excessive 30-40%.
Preferably, in rare earth feed liquid extraction deironing, aluminium step, according to the effective volume of agitation vat add in agitation vat prepare and deposit the rare earth feed liquid of more than 48 hours and non-saponification organic phase, start stirring, in 480 minutes, evenly add the bicarbonate of ammonia of calculated amount with solid feeding machine.
Preferably, after adding, continue stirring 60 minutes, clarify 8 hours, aqueous phase obtains qualified rare earth feed liquid after filtering; The continuous back extraction of the concentrated extraction tank of organic phase, blank organic phase recycles, and strip aqueous concentrates oxalic acid precipitation recovering rare earth.
Preferably, except the rare earth feed liquid after complete iron, aluminium is limpid, in rose-red color, pH4.5-5, directly can enter P507 extraction system and carry out extracting and separating.
According to the utility model, by rare earths material at normal temperatures hydrochloric acid decompose to acidity 0.2N, cross and filter mechanical impurity, then implement the abstraction impurity removal of mishmetal feed liquid.After removal of impurities, in rare earth feed liquid, iron, aluminium content are all less than 300mg/l; Straight yield of rare earth is more than or equal to 97%, and all the other rare earths are together with iron, aluminium, and this part rare earth can reclaim by oxalic acid precipitation.
According to the utility model removal of impurities, mixed rare earth chlorides solution can reach following index:
1. straight yield of rare earth: >=97%.(before straight yield of rare earth=qualified feed liquid rare earth metal amount/acid-soluble rear removal of impurities rare earth metal amount × 100%);
2. foreign matter content (feed liquid rare earth concentration: 1.3M) in qualified rare earth feed liquid: Fe < 20mg/l, Al < 300mg/l;
3. the reagent used in dedoping step does not have any impact to follow-up extraction process and quality product.
Claims (10)
1. an abstraction impurity removal system for mishmetal feed liquid, is characterized in that, comprising:
Feed liquid compounding system before removal of impurities, it comprises the acid dissolve device with whipping appts, and it is provided with technical hydrochloric acid upstream end and mishmetal raw material upstream end;
Organic phase dispenser;
Extracting system, it comprises the agitation vat be connected with feed liquid compounding system before described removal of impurities and organic phase dispenser, and described agitation vat connects solid feeding machine, aqueous phase filtration unit and load organic phases concentrator.
2. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 1, is characterized in that, also comprise back extraction system.
3. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 2, it is characterized in that, described back extraction system is connected with described load organic phases concentrator.
4. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 2, it is characterized in that, described back extraction system comprises extraction tank, settler, filtration unit, calcination retrieving arrangement.
5. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 4, it is characterized in that, described extraction tank is connected with organic phase dispenser.
6. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 4, it is characterized in that, described calcination retrieving arrangement is connected with mishmetal raw material upstream end.
7. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 1, it is characterized in that, before described removal of impurities, feed liquid compounding system also comprises filtering system and store holder.
8. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 7, it is characterized in that, described store holder is connected with the agitation vat of extracting system.
9. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 7, is characterized in that, described store holder is provided with and exchanges hydrochloric acid upstream end.
10. the abstraction impurity removal system of mishmetal feed liquid as claimed in claim 7, it is characterized in that, described store holder is with pump circulation device or whipping appts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420629369.4U CN204298445U (en) | 2014-10-28 | 2014-10-28 | The abstraction impurity removal system of mishmetal feed liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420629369.4U CN204298445U (en) | 2014-10-28 | 2014-10-28 | The abstraction impurity removal system of mishmetal feed liquid |
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| Publication Number | Publication Date |
|---|---|
| CN204298445U true CN204298445U (en) | 2015-04-29 |
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|---|---|---|---|
| CN201420629369.4U Withdrawn - After Issue CN204298445U (en) | 2014-10-28 | 2014-10-28 | The abstraction impurity removal system of mishmetal feed liquid |
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| Country | Link |
|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372186A (en) * | 2014-10-28 | 2015-02-25 | 江西稀有金属钨业控股集团有限公司 | Extraction and impurity removal method and system for mixed rare earth liquor |
| CN110306055A (en) * | 2018-07-26 | 2019-10-08 | 安徽金三隆再生资源有限公司 | A kind of neodymium iron boron waste material removal of impurities extraction equipment |
-
2014
- 2014-10-28 CN CN201420629369.4U patent/CN204298445U/en not_active Withdrawn - After Issue
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372186A (en) * | 2014-10-28 | 2015-02-25 | 江西稀有金属钨业控股集团有限公司 | Extraction and impurity removal method and system for mixed rare earth liquor |
| CN110306055A (en) * | 2018-07-26 | 2019-10-08 | 安徽金三隆再生资源有限公司 | A kind of neodymium iron boron waste material removal of impurities extraction equipment |
| CN110306055B (en) * | 2018-07-26 | 2021-03-23 | 安徽金三隆再生资源有限公司 | Neodymium iron boron waste material edulcoration extraction device |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20150429 Effective date of abandoning: 20160824 |
|
| C25 | Abandonment of patent right or utility model to avoid double patenting |