CN109264763A - The devices and methods therefor of continuous production crystal carbonated rare earth - Google Patents

The devices and methods therefor of continuous production crystal carbonated rare earth Download PDF

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Publication number
CN109264763A
CN109264763A CN201811342451.8A CN201811342451A CN109264763A CN 109264763 A CN109264763 A CN 109264763A CN 201811342451 A CN201811342451 A CN 201811342451A CN 109264763 A CN109264763 A CN 109264763A
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China
Prior art keywords
supernatant
precipitation tank
regulating valve
electromagnetic flowmeter
rare earth
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Pending
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CN201811342451.8A
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Chinese (zh)
Inventor
赵治华
桑晓云
刘瑞金
张文斌
柳凌云
张正中
娄利平
张永华
高媛
高天佐
王晓华
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China North Rare Earth (group) Hi Tech Ltd By Share Ltd
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China North Rare Earth (group) Hi Tech Ltd By Share Ltd
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Priority to CN201811342451.8A priority Critical patent/CN109264763A/en
Publication of CN109264763A publication Critical patent/CN109264763A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/247Carbonates
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention discloses a kind of devices of continuous production crystal carbonated rare earth, comprising: flow control system, crystal seed return-flow system, settling system, dense system, supernatant storage tank.The invention also discloses a kind of methods of continuous production crystal carbonated rare earth.The present invention can be continuously available the crystal carbonated rare earth that quality is stable, is easy to filter and wash.

Description

The devices and methods therefor of continuous production crystal carbonated rare earth
Technical field
The invention belongs to a kind of rare-earth wet methods to smelt production field, and in particular to a kind of continuous production crystal carbonated rare earth Devices and methods therefor.
Background technique
Chemical precipitation method is a kind of partial crystallization phenomenon, and the growth rate of crystallization is decided by precipitate in the surface and solution of the nuclei of crystallization Simple precipitation reaction and crystal seed circular response can be used in the difference of agent concentration and its saturated concentration, chemical precipitation reactive mode.Crystal seed Precipitation reaction is to add good precipitation seed into precipitation system in initial reaction stage, and to be formed, crystal grain is big, precipitating is fast, moisture content The good precipitated product of low outlet effect.
Rare-earth trade production carbonated rare earth precipitating be exactly using chemical precipitation method, with earth solution and ammonium bicarbonate solution or Sodium carbonate liquor etc. containing carbonate soluble salt solutions reaction, obtain carbonated rare earth precipitating, and by filtering, realize rare earth with The separation of other non-rare earth impurities.It is easy to the carbonated rare earth filtered in order to obtain, it is anti-that present rare-earth trade is all made of seeded precipitation It answers, but the unstable quality of carbonated rare earth, and carbonated rare earth is not easy filtering, impurity content height.
Summary of the invention
Technical problem solved by the invention is to provide a kind of devices and methods therefor of continuous production crystal carbonated rare earth, energy Enough it is continuously available the crystal carbonated rare earth that quality is stable, is easy to filter and wash.
Technical solution is as follows:
A kind of device of continuous production crystal carbonated rare earth, comprising:
Flow control system, for conveying precipitant solution, earth solution to settling system, comprising: the first Electromagnetic Flow Meter, the second electromagnetic flowmeter, the first regulating valve, the second regulating valve, precipitating reagent transfer pipeline, Tu Rongyeshusongguanlu;First electricity Magnetic flowmeter, the first regulating valve are arranged on precipitating reagent transfer pipeline, and precipitating reagent transfer pipeline connects under first order precipitation tank Portion;Second electromagnetic flowmeter, the second regulating valve are arranged on earth solution transfer pipeline, earth solution transfer pipeline connection first The bottom of grade precipitation tank, earth solution enter first order precipitation tank after flowing through the second electromagnetic flowmeter, the second regulating valve;
Crystal seed return-flow system, for underflow liquid and supernatant to be sent back to settling system, comprising: third electromagnetic flowmeter, Third regulating valve, return line, third electromagnetic flowmeter, third regulating valve are arranged on return line;Return line one end point Not Lian Jie variable frequency pump, supernatant produce pump, the other end connects the first order precipitation tank of settling system;Underflow liquid and supernatant flow through Enter first order precipitation tank after third electromagnetic flowmeter, third regulating valve;
Settling system, including multiple concatenated precipitation tanks, precipitation tank are provided with variable-frequency motor, are provided on the top of side wall Overflow port, the overflow port of upper level precipitation tank pass through the lower part of piping connection next stage precipitation tank;
Dense system, for separating the rare earth salt particle in slurries, comprising: dense slot, variable frequency pump, dense slot variable-frequency electric Machine;Dense slot variable-frequency motor is arranged on dense slot, and the overflow port of afterbody precipitation tank passes through under the dense slot of piping connection Portion, for the clear liquid overflow port on dense slot top by piping connection supernatant storage tank, the underflow liquid outlet of lower part is provided with variable frequency pump, Underflow liquid is sent into return line by piping connection return line, variable frequency pump by variable frequency pump;
Supernatant storage tank, for storing supernatant, the liquid outlet in lower part is provided with supernatant and produces pump, and supernatant produces By piping connection return line, supernatant produces the supernatant that pumping goes out and enters return line pump.
Further, the quantity of precipitation tank is determined according to the series of Process configuration, and the series of precipitation tank is according to Crystallization Time requirement determine that the Crystallization time series of long then precipitation tank is more, the series of Crystallization time short then precipitation tank It is few.
Further, slurries a part of variable frequency pump extraction is by third electromagnetic flowmeter and third regulating valve, as crystal seed It accurately feeds in first order precipitation tank, remaining underflow liquid realizes that solid-liquid is kept completely separate through filtering.
Further, precipitant solution passes through the first electromagnetic flowmeter, the first regulating valve accurate flow adjustment;Earth solution is logical Cross the second electromagnetic flowmeter, the second regulating valve accurate flow adjustment;Underflow liquid and supernatant pass through third electromagnetic flowmeter, third Regulating valve accurate flow adjustment.
A kind of method of continuous production crystal carbonated rare earth, comprising:
Precipitant solution enters first order precipitation tank, precipitant solution after flowing through the first electromagnetic flowmeter, the first regulating valve Valve regulating flow is adjusted by the first electromagnetic flowmeter, first;After earth solution flows through the second electromagnetic flowmeter, the second regulating valve Into first order precipitation tank, earth solution adjusts valve regulating flow by the second electromagnetic flowmeter, second;
Supernatant and underflow liquid enter first order precipitation tank, supernatant after flowing through third electromagnetic flowmeter, third regulating valve Valve regulating flow is adjusted by third electromagnetic flowmeter, third with underflow liquid;
Precipitant solution, earth solution, supernatant and underflow liquid are reacted in precipitation tank, react the slurries of generation by frequency conversion Motor stirs evenly, and slurries flow in next stage reactive tank from overflow port, and slurries enter dense slot after complete reaction;
The underflow liquid a part extracted out in dense slot is sent to third electromagnetic flowmeter and third tune as crystal seed by variable frequency pump Valve is saved, remaining underflow liquid after filtering comes out rare-earth salts particle filtering therein;Supernatant in dense slot enters supernatant Liquid storage tank produces the supernatant entrance that pumping goes out through supernatant and flows back into first order precipitation tank.
Preferably, the supernatant that supernatant produces that pumping goes out further recycles the carbonate particle wherein to suspend through filtering.
Preferably, keep the temperature of precipitation tank between 20-60 DEG C, the solution concentration of precipitating reagent is 0-4mol/L, rare earth The concentration of solution is 0-300g/L;Crystal seed includes supernatant and underflow liquid, and solid-liquid volume ratio is 1:10-1:2.
Preferably, the extracted amount for the underflow liquid that variable frequency pump produces, supernatant produce the flow for the supernatant that pump produces and sink Shallow lake agent solution, earth solution total inlet match.
The technology of the present invention effect includes:
In the present invention, the device production carbonated rare earth of continuous production crystal carbonated rare earth has the characteristics that efficient, continuous, reality The Automatic Control of existing carbonated rare earth production, by equipment control sedimentation time, temperature and precipitation seed adding manner and Additional amount is continuously available the crystal carbonated rare earth that quality is stable, is easy to filter and wash.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the device of continuous production crystal carbonated rare earth in the present invention;
Specific embodiment
Be described below and specific embodiments of the present invention be fully shown, with enable those skilled in the art to practice and It reproduces.
As shown in Figure 1, being the structural schematic diagram of the device of continuous production crystal carbonated rare earth in the present invention.
The present invention by adjusting earth solution and precipitant solution addition speed and be continuously added to the amount of crystal seed, control is anti- The speed of growth for answering each conversion zone rare earth ion concentration and precipitant concentration and precipitated crystal in system, was easy to Filter, the low crystal carbonated rare earth of impurity content.
The device of continuous production crystal carbonated rare earth, comprising: flow control system 1, crystal seed return-flow system 2, settling system 3, dense system 4, supernatant storage tank 5.
Flow control system 1 is used to convey precipitant solution, earth solution to settling system 3 (first order precipitation tank 31), Its structure includes: the first electromagnetic flowmeter 11, the second electromagnetic flowmeter 12, the first regulating valve 13, the second regulating valve 14, precipitating reagent Transfer pipeline 15, native solution conveyor tube road 16.
First electromagnetic flowmeter 11, the first regulating valve 13 are arranged on precipitating reagent transfer pipeline 16, precipitating reagent transfer pipeline The lower part of 15 connection first order precipitation tanks 31, precipitant solution enter after flowing through the first electromagnetic flowmeter 11, the first regulating valve 13 First order precipitation tank 31, precipitant solution pass through the first electromagnetic flowmeter 11,13 accurate flow adjustment of the first regulating valve.
Second electromagnetic flowmeter 12, the second regulating valve 14 are arranged on earth solution transfer pipeline 16, earth solution conveying Pipeline 16 connects the bottom of first order precipitation tank 31, and it is laggard that earth solution flows through the second electromagnetic flowmeter 12, the second regulating valve 14 Enter first order precipitation tank 31, earth solution passes through the second electromagnetic flowmeter 12,14 accurate flow adjustment of the second regulating valve.
Crystal seed return-flow system 2 is used to underflow liquid and supernatant sending back to settling system 3 (first order precipitation tank 31).It is tied Structure includes: third electromagnetic flowmeter 21, third regulating valve 22, return line 23, third electromagnetic flowmeter 21, third regulating valve 22 It is arranged on return line 23;23 one end of return line is separately connected variable frequency pump 42, supernatant produces pump 51, and other end connection is heavy Shallow lake system 3 (first order precipitation tank 31);Return line 23 connects the bottom of first order precipitation tank 31, and underflow liquid and supernatant flow through Enter first order precipitation tank 31 after third electromagnetic flowmeter 21, third regulating valve 22;Underflow liquid and supernatant pass through third electromagnetism Flowmeter 21,22 accurate flow adjustment of third regulating valve.
Settling system 3 includes multiple concatenated precipitation tanks 31, and precipitation tank 31 is provided with variable-frequency motor 32, on the top of side wall It is provided with overflow port 33.The overflow port 33 of upper level precipitation tank 31 passes through the lower part of piping connection next stage precipitation tank 31.Pass through Variable-frequency motor 32 controls the revolving speed stirred in precipitation tank 31, guarantees constantly feeding with feed liquid, reacts the slurries stirring of generation Uniformly, slurries flow in next stage reactive tank 31 from overflow port 33.The quantity of precipitation tank 31 is according to the series of Process configuration come really Fixed, for the series of precipitation tank 31 depending on the time requirement of Crystallization, the Crystallization time series of long then precipitation tank 31 is more, The Crystallization time series of short then precipitation tank 31 is few.
Dense system 4 is used to separate the rare earth salt particle in slurries.Its structure includes: dense slot 41, variable frequency pump 42, dense Slot variable-frequency motor 43;Dense slot variable-frequency motor 43 is arranged on dense slot 41, and the overflow port 33 of afterbody precipitation tank 31 passes through The clear liquid overflow port of the lower part of the dense slot 41 of piping connection, dense 41 top of slot passes through piping connection supernatant storage tank 5, lower part Underflow liquid outlet is provided with variable frequency pump 42, and underflow liquid is sent by variable frequency pump 42 by piping connection return line 23, variable frequency pump 42 Return line 23.After complete reaction, slurries enter in dense slot 41, according to the gravity properties for generating precipitating, adjust dense Slot variable-frequency motor 43 reduces speed of agitator, guarantees that the rare earth salt particle (carbonated rare earth) generated is deposited in the lower half of dense slot 41 Part.Slurries a part that variable frequency pump 42 is extracted out is accurate as crystal seed by third electromagnetic flowmeter 22 and third regulating valve 21 It feeds in first order precipitation tank 31, remaining underflow liquid realizes that solid-liquid is kept completely separate through filtering.
For storing supernatant, the liquid outlet in lower part is provided with supernatant and produces pump 51 supernatant storage tank 5, and supernatant turns Pump 51 passes through piping connection return line 23 out.The supernatant that supernatant produces 51 extraction of pump enters return line 23, further Recycle the carbonate particle wherein to suspend.
The method of continuous production crystal carbonated rare earth, specifically includes the following steps:
Step 1: precipitant solution enters first order precipitation tank after flowing through the first electromagnetic flowmeter 11, the first regulating valve 13 31, precipitant solution passes through the first electromagnetic flowmeter 11,13 accurate flow adjustment of the first regulating valve;Earth solution flows through the second electricity Enter first order precipitation tank 31 after magnetic flowmeter 12, the second regulating valve 14, earth solution passes through the second electromagnetic flowmeter 12, second 14 accurate flow adjustment of regulating valve;
Step 2: crystal seed (supernatant and underflow liquid) enters first after flowing through third electromagnetic flowmeter 22, third regulating valve 21 Grade precipitation tank 31, supernatant and underflow liquid pass through third electromagnetic flowmeter 22,21 accurate flow adjustment of third regulating valve;
Step 3: feed liquid (precipitant solution, earth solution, supernatant and underflow liquid) is reacted in precipitation tank 31, and reaction produces Raw slurries are stirred evenly by variable-frequency motor 32, and slurries flow in next stage reactive tank 31 from overflow port 33, after complete reaction Slurries enter dense slot 41;
Keep the temperature of precipitation tank 31 between 20-60 DEG C, no pressure requirement.The extraction for the underflow liquid that variable frequency pump 42 produces The flow that amount, supernatant produce the supernatant that pump 51 produces matches with precipitant solution, total inlet of earth solution.Precipitating The solution concentration of agent is 0-4mol/L, and the concentration of earth solution is 0-300g/L, and the solid-liquid volume ratio of crystal seed is 1:10-1:2.
Step 4: the underflow liquid a part extracted out in dense slot 41 is sent to third Electromagnetic Flow as crystal seed by variable frequency pump 42 Meter 22 and third regulating valve 21, remaining underflow liquid after filtering come out rare-earth salts particle filtering therein;In dense slot 41 Supernatant enter supernatant storage tank 5, through supernatant produce pump 51 extraction supernatant enter return line 23.
The supernatant that supernatant produces 51 extraction of pump may also pass through filter, further recycle the carbonate wherein to suspend Grain.
It should be understood that the foregoing is merely a specific embodiment of the invention, but protection scope of the present invention is not It is confined to this, anyone skilled in the art in the technical scope disclosed by the present invention, can readily occur in variation Or replacement, it should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the claim Protection scope subject to.

Claims (8)

1. a kind of device of continuous production crystal carbonated rare earth characterized by comprising
Flow control system, for conveying precipitant solution, earth solution to settling system, comprising: the first electromagnetic flowmeter, Two electromagnetic flowmeters, the first regulating valve, the second regulating valve, precipitating reagent transfer pipeline, Tu Rongyeshusongguanlu;First Electromagnetic Flow Meter, the first regulating valve are arranged on precipitating reagent transfer pipeline, and precipitating reagent transfer pipeline connects the lower part of first order precipitation tank;Second Electromagnetic flowmeter, the second regulating valve are arranged on earth solution transfer pipeline, and earth solution transfer pipeline connects first order precipitating The bottom of slot, earth solution enter first order precipitation tank after flowing through the second electromagnetic flowmeter, the second regulating valve;
Crystal seed return-flow system, for underflow liquid and supernatant to be sent back to settling system, comprising: third electromagnetic flowmeter, third Regulating valve, return line, third electromagnetic flowmeter, third regulating valve are arranged on return line;Return line one end connects respectively Connect variable frequency pump, supernatant produces pump, the first order precipitation tank of other end connection settling system;Underflow liquid and supernatant flow through third Enter first order precipitation tank after electromagnetic flowmeter, third regulating valve;
Settling system, including multiple concatenated precipitation tanks, precipitation tank are provided with variable-frequency motor, and the top of side wall is provided with overflow Mouthful, the overflow port of upper level precipitation tank passes through the lower part of piping connection next stage precipitation tank;
Dense system, for separating the rare earth salt particle in slurries, comprising: dense slot, variable frequency pump, dense slot variable-frequency motor;It is dense Close slot variable-frequency motor is arranged on dense slot, and the overflow port of afterbody precipitation tank passes through the lower part of the dense slot of piping connection, dense The clear liquid overflow port on close slot top is provided with variable frequency pump, frequency conversion by piping connection supernatant storage tank, the underflow liquid outlet of lower part Underflow liquid is sent into return line by piping connection return line, variable frequency pump by pump;
Supernatant storage tank, for storing supernatant, the liquid outlet in lower part is provided with supernatant and produces pump, and it is logical that supernatant produces pump Piping connection return line is crossed, supernatant produces the supernatant that pumping goes out and enters return line.
2. the device of continuous production crystal carbonated rare earth as described in claim 1, which is characterized in that the quantity of precipitation tank is according to work The series of skill configuration determines that the series of precipitation tank determines according to the time requirement of Crystallization, and the Crystallization time is long then The series of precipitation tank is more, and the Crystallization time series of short then precipitation tank is few.
3. the device of continuous production crystal carbonated rare earth as described in claim 1, which is characterized in that the slurries one of variable frequency pump extraction Part is accurately fed in first order precipitation tank, remaining is dense by third electromagnetic flowmeter and third regulating valve as crystal seed Slurries realize that solid-liquid is kept completely separate through filtering.
4. the device of continuous production crystal carbonated rare earth as described in claim 1, which is characterized in that precipitant solution passes through first Electromagnetic flowmeter, the first regulating valve accurate flow adjustment;Earth solution is accurately adjusted by the second electromagnetic flowmeter, the second regulating valve Amount of restriction;Underflow liquid and supernatant pass through third electromagnetic flowmeter, third regulating valve accurate flow adjustment.
5. a kind of method of continuous production crystal carbonated rare earth, comprising:
Precipitant solution enters first order precipitation tank after flowing through the first electromagnetic flowmeter, the first regulating valve, and precipitant solution passes through First electromagnetic flowmeter, first adjust valve regulating flow;Earth solution enters after flowing through the second electromagnetic flowmeter, the second regulating valve First order precipitation tank, earth solution adjust valve regulating flow by the second electromagnetic flowmeter, second;
Supernatant and underflow liquid, which flow through, enters first order precipitation tank after third electromagnetic flowmeter, third regulating valve, supernatant and dense Slurries adjust valve regulating flow by third electromagnetic flowmeter, third;
Precipitant solution, earth solution, supernatant and underflow liquid are reacted in precipitation tank, react the slurries of generation by variable-frequency motor It stirs evenly, slurries flow in next stage reactive tank from overflow port, and slurries enter dense slot after complete reaction;
The underflow liquid a part extracted out in dense slot is sent to third electromagnetic flowmeter and third regulating valve as crystal seed by variable frequency pump, Remaining underflow liquid after filtering comes out rare-earth salts particle filtering therein;Supernatant in dense slot enters supernatant storage Slot produces the supernatant entrance that pumping goes out through supernatant and flows back into first order precipitation tank.
6. the method for continuous production crystal carbonated rare earth as claimed in claim 5, which is characterized in that supernatant produces what pumping went out Supernatant further recycles the carbonate particle wherein to suspend through filtering.
7. the method for continuous production crystal carbonated rare earth as claimed in claim 5, which is characterized in that the temperature of precipitation tank is kept to exist Between 20-60 DEG C, the solution concentration of precipitating reagent is 0-4mol/L, and the concentration of earth solution is 0-300g/L;Crystal seed includes supernatant Liquid and underflow liquid, solid-liquid volume ratio are 1:10-1:2.
8. the method for continuous production crystal carbonated rare earth as claimed in claim 5, which is characterized in that the underflow liquid that variable frequency pump produces Extracted amount, supernatant produces the flow of supernatant that pump produces and matches with precipitant solution, total inlet of earth solution.
CN201811342451.8A 2018-11-13 2018-11-13 The devices and methods therefor of continuous production crystal carbonated rare earth Pending CN109264763A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101306828A (en) * 2007-05-17 2008-11-19 北京有色金属研究总院 Device and process for preparing rare-earth compound uniform micro powder
JP2011072998A (en) * 2010-11-24 2011-04-14 Mitsubishi Gas Chemical Co Inc Crystallization method and apparatus
CN106947861A (en) * 2017-05-18 2017-07-14 赣州晨光稀土新材料股份有限公司 A kind of continuous device for making of rare earth compound precipitation
CN107188215A (en) * 2017-05-24 2017-09-22 中国北方稀土(集团)高科技股份有限公司 The method that reaction end is automatically adjusted in carbonated rare earth continuous precipitation production process
CN209291982U (en) * 2018-11-13 2019-08-23 中国北方稀土(集团)高科技股份有限公司 The device of continuous production crystal carbonated rare earth

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101306828A (en) * 2007-05-17 2008-11-19 北京有色金属研究总院 Device and process for preparing rare-earth compound uniform micro powder
JP2011072998A (en) * 2010-11-24 2011-04-14 Mitsubishi Gas Chemical Co Inc Crystallization method and apparatus
CN106947861A (en) * 2017-05-18 2017-07-14 赣州晨光稀土新材料股份有限公司 A kind of continuous device for making of rare earth compound precipitation
CN107188215A (en) * 2017-05-24 2017-09-22 中国北方稀土(集团)高科技股份有限公司 The method that reaction end is automatically adjusted in carbonated rare earth continuous precipitation production process
CN209291982U (en) * 2018-11-13 2019-08-23 中国北方稀土(集团)高科技股份有限公司 The device of continuous production crystal carbonated rare earth

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Application publication date: 20190125