CN105200230A - Production method and device for extracting rare earth from monazite ores - Google Patents
Production method and device for extracting rare earth from monazite ores Download PDFInfo
- Publication number
- CN105200230A CN105200230A CN201510735519.9A CN201510735519A CN105200230A CN 105200230 A CN105200230 A CN 105200230A CN 201510735519 A CN201510735519 A CN 201510735519A CN 105200230 A CN105200230 A CN 105200230A
- Authority
- CN
- China
- Prior art keywords
- enters
- rare earth
- chamber
- receiving tank
- branch road
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a method and a device for extracting rare earth, in particular to a production method and device for extracting the rare earth from monazite ores. The production operation stability is guaranteed by means of a caustic decomposition procedure, a washing procedure, a chlorination procedure, a phosphorus base liquor fine filtration and crystallization procedure as well as a special JQL reactor and a full-automatic metering system; by the aid of the JQL reactor as caustic decomposition equipment, fully-enclosed continuous and automatic operation is realized, heat energy consumption and alkali consumption are reduced, the labor intensity of workers is reduced, wastewater emission is avoided in a production process, the production efficiency is high, the rare earth yield is increased, and the worker bodies are prevented from radiation injury caused by radioactive substances. The clean, automatic, and fully-enclosed continuous production operation mode is realized by the aid of equipment, the utilization rate of the equipment is increased greatly, and the operation cost of the equipment is reduced.
Description
Technical field
The present invention relates to a kind of square law device of Extraction of rare earth, particularly relate to a kind of production method and device of Extraction of rare earth from solitary stone ore.
Background technology
Solitary stone ore primary chemical consists of (Ce, La, Nd, Th) [PO4], crystal belongs to monoclinic phosphate mineral.Solitary stone ore is main rare-earth mineral, and light rare earths (cerium group) oxide compound accounts for 39-74%, and heavy rare earths (yttrium group) oxide compound accounts for 0 ~ 5%, and color is based on yellow, and secondary is pale yellow or yellow-white.Rare earth element is widely used in black and nonferrous metallurgy, glass and Production of Ceramics, electronics, electric lighting, TV and laser technology, chemical engineering industry, medical treatment and agricultural production.Also output is had in the hydrothermal deposit relevant with grouan.In addition, often enrichment placer can be formed.Monazite is the important raw mineral materials extracting cerium race rare earth element.Cerium is replaced, ThO owing to often there being thorium in composition
2content can reach 30% at most, when extracting cerium, comprehensively can extract thorium.Natural resources is very abundant, but owing to smelting the aspects such as isolation technique, cost, environmental protection, Solid state fermentation, seldom has enterprise to process.
The production and processing technology of current solitary stone ore is very original, and adopt monomer batch production pattern to extract, its technical process is: monazite breeze carries out magnetic separation after abrasive dust, after getting rid of zircon and xenotime, uses alkali process to process.Treatment process: after monazite breeze mixes with liquid caustic soda after magnetic separation, about 120 DEG C are warmed up in single devices, be incubated and decompose for more than 16 hours, then the later slurries of decomposition are carried out dilution washing, mother liquor removal of impurities also reclaims tertiary sodium phosphate, wash qualified slurries and after the operation such as dissolving with hydrochloric acid, removal of impurities, obtain re chloride after press filtration, waste residue is deposited in special waste residue storage vault.
This technique adopts monomer batch production, and production cost is high, energy consumption is high, production efficiency is low, has discharge of wastewater in production process, and labor strength is large, and production environment is poor, easily damages the health of operator.
Summary of the invention
The object of the present invention is to provide a kind of production method and device of Extraction of rare earth from solitary stone ore; the method is non-wastewater discharge in process of production, and production efficiency is high, and energy consumption is low; reduce production cost, and the health not raying injury of energy available protecting operator.This equipment configuration achieves automatization, totally-enclosed continuous seepage operation, greatly improves the utilization ratio of equipment, reduces equipment running cost.
Technical scheme of the present invention:
A device for Extraction of rare earth from solitary stone ore, comprising: pneumatic conveyer is connected with weight-loss metering helix balance by pipeline, and weight-loss metering helix balance is connected with the import of JQL reactor content, and wash water is connected with JQL reactor by pipeline; JQL reactor outlet is connected with band filter fluid inlet by pipeline, three output branch roads and an input branch road be connected with water source is divided into filter, band filter one is exported branch road and is connected with the first receiving tank by pipeline, first receiving tank is connected with dissolving tank by pipeline, dissolving tank is connected with surface filter and hydrochloric acid hold-up vessel respectively, surface filter is two branch roads, and a branch road is connected with the second receiving tank, and another branch road is connected with the 3rd receiving tank; Second receiving tank is connected with deblending slot, and deblending slot is connected with removal of impurities medicament storage tank; Deblending slot outlet is connected with surface filter, and surface filter divides two branch roads, and a branch road is connected with the 3rd receiving tank, and another branch road is connected with storage pool; 3rd receiving tank is connected with surface filter, and surface filter is divided into two branch roads, and a branch road is connected with waste residue automatic packing machine, another branch road reuse; Band filter second branch road is connected with surface filter, and surface filter is divided into two branch roads, and the first branch road is connected with cooling tower, and another branch road is connected with wash water receiving tank; Cooling tower is connected with the second band filter, and the second band filter is divided into two branch roads, and the first branch road is connected with finished product automatic packing machine, another branch road and reuse; Band filter the 3rd branch road is connected with wash water hold-up vessel by wash water pipeline.
Described oar liquid and liquid line are equipped with fully automatic culculating system, and fully automatic culculating system comprises: liquid caustic soda adopts constant pressure pump, magnetic flow meter, motorized valve, electro connecting pressure gauge.
Described dissolving tank comprises: cell body, cell body is separated at least two-stage chamber by end plate, described first step chamber is respectively equipped with material channel, slurry passage and fixing material channel have potential difference, the chamber of every grade is equipped with slurry channel, slurry channel has potential difference, and the end plate of last step chamber is provided with discharge port, establishes whipping appts in the chamber of every grade.
JQL reactor comprises: cell body, cell body is separated at least two-stage chamber by end plate, the baffle plate perpendicular to base plate is provided with in each chamber, chamber cavity forms octagon structure, and described first step chamber is respectively equipped with material channel, and slurry passage and fixing material channel have potential difference, the chamber of every grade is equipped with slurry channel, slurry channel has potential difference, and the end plate of last step chamber is provided with discharge port, establishes whipping appts in the chamber of every grade.
Described material channel comprises: solid tunnel, fluid passage and slurry channel, on described every grade of chamber, the fluid passage of two-stage plate has vertical parallax, on every grade of chamber, in two-stage plate, slurry channel has vertical parallax, and fluid passage and slurry channel can be to setting or asymmetric setting.
Described cell body is provided with lid, is provided with sealing member between lid and cell body.
Whipping appts on described lid penetrates between hole and whipping appts and is provided with sealing member.
A kind of production method of Extraction of rare earth from solitary stone ore:
Processing step:
1 caustic digestion operation
Granularity is that the monazite breeze of more than 200 orders enters weight-loss metering helix balance by pneumatic conveyer by pipeline, promote to enter in JQL reactor first step chamber from fixing material channel by weight-loss metering helix balance, liquid caustic soda enters in JQL reactor first step chamber by fluid passage, start reaction, beginning through after whipping appts stirs from the first step enters in subordinate's chamber, arrive in last step chamber through stirring step by step, in reaction process, temperature controls to adopt electric temperature control valve to carry out temperature regulable control, span of control is 130-170 DEG C, by inlet amount and thin up level regulable control reaction times within 160-260min, ore deposit liquor ratio is 1:1-10, breeze rate of decomposition can reach more than 99%.Slip after stirring enters the band filter first step by pipeline with overflow type and carries out drip washing and solid-liquid separation after JQL reactor last step adds washing lotion dilution washing.
2. washing procedure
Washing procedure adopts band filter to carry out drip washing and solid-liquid separation.Dilution rear slurry enters the band filter first step to carry out phosphorus alkali lye and is separated with alkali cake, phosphorus alkali lye enters phosphorus alkali lye essence filter Crystallization Procedure, alkali cake enters the band filter second stage and washs, through the band filter third stage, fourth stage washing, washing is countercurrent washing, water enters from the fourth stage, and wash water flows out to wash water receiving tank from the second stage, for caustic digestion operation dilution washing; Alkali cake enters band filter level V and dewaters, and the alkali cake after separation enters the first receiving tank, and the first receiving tank to be sized mixing tank for alkali cake slurries after sizing mixing by acid dissolution slag washing lotion, and alkali cake removes chloride process after sizing mixing.This technique significantly reduces the consumption of water, decreases the removal of impurities operation in former technique, reduces the introducing of production run cost and impurity, and phosphorus alkali lye thoroughly recycles the full reuse with wash water simultaneously, achieves wastewater zero discharge and continuous seepage.
3. chloride process
Alkali cake dissolution equipment adopts the dissolving tank of our company's independent research.In hydrochloric acid and the first receiving tank, alkali cake slurries enter the first step of dissolving tank by constant pressure pump, magnetic flow meter, motorized valve, electro connecting pressure gauge, in reaction process, by electric temperature control valve control temperature at 60-90 DEG C, dissolve, by slip inlet amount and hydrochloric acid flow control and adjusting reaction time within 100-150min, flow is 1-1000L/min; PH value controls 4 ~ 4.5, uses online pH meter to detect, links with flow mediation system; Slurries after dissolving by after the first precision surface metre filter, achieve the separation of solution, waste residue with overflow type; Solution enters the second receiving tank, and waste residue enters the 3rd receiving tank and carries out washery slag.Solution and slagging-off medicament all adopt constant pressure pump, magnetic flow meter, motorized valve, electro connecting pressure gauge joint control mode is carried out flow control and is entered deblending slot the 1st grade and carry out removal of impurities, in reaction process, temperature controls to adopt electric temperature control valve to carry out temperature regulable control, control at 60-90 DEG C, by mass flow control and adjusting reaction time within 20-100min, flow range is 1-1000L/min, after removal of impurities rear slurry passes through second surface metre filter with overflow type, obtain qualified rare earth chloride liquid and waste residue, feed liquid enters storage pool, use as next procedure, waste residue enters the 3rd receiving tank and carries out washery slag, and add water acid elution, and pH value controls 2 ~ 2.5, and use online pH meter to detect, the reaction times controls within 15-100min, qualified rear slurry carries out solid-liquid separation by the 3rd precision surface strainer, and waste residue stores after using Full-automatic quantitative wrapping machine packaging, washing lotion is used for alkali cake and sizes mixing operation.
4. phosphorus alkali lye essence filter Crystallization Procedure
After the phosphorus alkali lye of washing procedure output removes entrained solid particulate matter after the 4th precision surface strainer, qualified phosphorus alkali lye enters cooling tower and carries out crystallisation by cooling; Waste residue enters wash water storage pool, and crystallisation by cooling rear slurry uses band filter to carry out solid-liquid separation, and the solid that band filter is produced is finished product tertiary sodium phosphate, carries out quantitative package by device of full automatic packaging, stores and sells; Liquid is waste lye, for the liquid caustic soda preparation reuse of caustic digestion operation.
Above in each production process, whole employing automatic control device, on-the-spot operative employee only needs to patrol and examine equipment and keep a public place clean, do not need to intervene production run process, all operations and parameter adjustment and production run control to be completed by DCS robot control system(RCS), and all right teletransmission of the instant data in production run process is to relevant departments, facilitate all departments and understand production run process and production scene situation in time, and production operation situation and the production run data of random time section can be checked, achieve instant messages and share; This technology passes through process optimization, swivel link in minimizing, accurate control, reduces energy consumption, has saved transfer and cost of labor, achieve lean to produce, thoroughly solve employee in production run process and contact a difficult problem for radioactivity material, ensure that employee's is healthy, meet the relevant code requirements of occupational health health, meanwhile, this technology achieves the zero release of waste water.
Advantage of the present invention:
The present invention's " HQD production technique ", from the charging of caustic digestion operation, have employed fully automatic culculating system, ensure that the stability of production run; Caustic digestion equipment " JQL reactor ", achieves totally-enclosed continuous and automatic operation, reduces heat energy consumption and alkali consumption, alleviates the labour intensity of employee.
This production technique environmental protection, clean, low consumption, non-wastewater discharge in process of production, production efficiency is high, energy consumption is low, both reduced production run cost, turn improved rare-earth yield, in production run process, employee does not need directly to contact material, avoids the health of operator not by the radiation injury of radioactive substance.This equipment configuration achieve clean, automatization, totally-enclosed continuous seepage work pattern, greatly improve the utilization ratio of equipment, reduce equipment running cost.
Accompanying drawing explanation
Fig. 1 is present invention process schema;
Fig. 2 is JQL reactor front view of the present invention;
Fig. 3 is the vertical view of Fig. 2;
Fig. 4 is Fig. 2 cover plate structural representation.
Embodiment
The present invention includes: pneumatic conveyer 1 is connected with weight-loss metering helix balance 2 by pipeline, weight-loss metering helix balance 2 is connected with the solids inlet of JQL reactor 3, and wash water is connected with JQL reactor 3 by wash water pipeline; JQL reactor 3 is exported and is connected with the first band filter 4 fluid inlet by pipeline, first band filter 4 is divided into three output branch roads and an input branch road be connected with water source, first band filter 4 one is exported branch road and is connected with the first receiving tank 5 by pipeline, slurries and the hydrochloric acid hold-up vessel of the first receiving tank 5 are connected with dissolving tank 6 by liquid line, dissolving tank 6 is connected with first surface strainer 7 respectively by pipeline, surface filter 7 is two branch roads, one branch road is connected with the second receiving tank 8, and another branch road is connected with the 3rd receiving tank 9; Second receiving tank 8 is connected with deblending slot 10, and deblending slot 10 is connected with removal of impurities medicament storage tank 11; Deblending slot goes out 10 mouthfuls and is connected with second surface strainer 12, second surface strainer 12 points of two branch roads, and a branch road is connected with the 3rd receiving tank 9, and another branch road is connected with storage pool 13; 3rd receiving tank 9 is connected with the 3rd surface filter 14, and the 3rd surface filter 14 is divided into two branch roads, and a branch road is connected with waste residue automatic packing machine 15, and another branch road flows into the reuse of washing lotion receiving tank 22 by liquid line; First band filter 4 second branch road is connected with the 4th surface filter 16, and the 4th surface filter 16 is divided into two branch roads, and the first branch road is connected with cooling tower 17, and another branch road is connected with wash water hold-up vessel 18; Cooling tower 17 is connected with the second band filter 19, and the second band filter 19 is divided into two branch roads, and the first branch road is connected with finished product automatic packing machine 20, and another branch road enters caustic soda liquid preparation tank 21 by liquid line reuse; Band filter 4 the 3rd branch road is connected with wash water hold-up vessel 18 by wash water pipeline.
Described hydrochloric acid, wash water, water source, enter on pipeline and liquid line and be equipped with fully automatic culculating system, fully automatic culculating system comprises: constant pressure pump, magnetic flow meter, motorized valve, electro connecting pressure gauge.
Described dissolving tank 6 comprises: cell body, cell body is separated at least two-stage chamber by end plate, described first step chamber is respectively equipped with material channel, slurry passage and fixing material channel have potential difference, the chamber of every grade is equipped with slurry channel, slurry channel has potential difference, and the end plate of last step chamber is provided with discharge port, establishes whipping appts in the chamber of every grade.
JQL reactor 3 comprises: cell body, cell body is separated at least two-stage chamber by end plate, the baffle plate perpendicular to base plate is provided with in each chamber, chamber cavity forms octagon structure, and described first step chamber is respectively equipped with solid materials passage and fluid passage and slurry channel, slurry passage and fixing material channel have potential difference, the chamber of every grade is equipped with slurry channel, slurry channel has potential difference, and the end plate of last step chamber is provided with discharge port, establishes whipping appts in the chamber of every grade.
The potential difference of the slurry channel of described every grade of chamber is vertical parallax or left and right potential difference,
Described cell body is provided with lid, is provided with sealing member between lid and cell body.
Whipping appts on described lid penetrates between hole and whipping appts and is provided with sealing member.
A kind of production method of Extraction of rare earth from solitary stone ore:
Processing step:
1. caustic digestion operation
Granularity is that the monazite breeze of more than 320 orders enters weight-loss metering helix balance 2 by pneumatic conveyer 1 by pipeline, promote to enter in JQL reactor 3 first step chamber from fixing material channel by weight-loss metering helix balance 2, liquid caustic soda enters in JQL reactor 3 first step chamber by fluid passage, start reaction, beginning through after whipping appts stirs from the first step enters in subordinate's chamber, arrive in last step chamber through stirring step by step, in reaction process, temperature controls to adopt electric temperature control valve to carry out temperature regulable control, span of control is 130-170 DEG C, by inlet amount and thin up level regulable control reaction times within 160-260min, ore deposit liquor ratio is 1:1-10, breeze rate of decomposition can reach more than 99%.Slip after stirring enters band filter 4 first step by pipeline with overflow type and carries out drip washing and solid-liquid separation after JQL reactor 3 last step adds washing lotion dilution washing.
2. washing procedure
Washing procedure adopts the first band filter 4 to carry out drip washing and solid-liquid separation.Dilution rear slurry enters first band filter 4 first step to carry out phosphorus alkali lye and is separated with alkali cake, phosphorus alkali lye enters phosphorus alkali lye essence filter Crystallization Procedure, alkali cake enters first band filter 4 second stage and washs, through first band filter 4 third stage, fourth stage washing, washing is countercurrent washing, water enters from the fourth stage, and wash water flows out to wash water hold-up vessel 18 from the second stage, for caustic digestion operation dilution washing; Alkali cake enters the first band filter 4 level V and dewaters, and the alkali cake after separation enters the first receiving tank 5, first receiving tank 5 for alkali cake slurries after sizing mixing by acid dissolution slag washing lotion and to size mixing tank, and alkali cake removes chloride process after sizing mixing.This technique significantly reduces the consumption of water, decreases the removal of impurities operation in former technique, reduces the introducing of production run cost and impurity, and phosphorus alkali lye thoroughly recycles the full reuse with wash water simultaneously, achieves wastewater zero discharge and continuous seepage.
3. chloride process
Alkali cake dissolution equipment adopts the dissolving tank 6 of our company's independent research.In hydrochloric acid and the first receiving tank, alkali cake slurries enter the first step of dissolving tank 6 by constant pressure pump, magnetic flow meter, motorized valve, electro connecting pressure gauge, in reaction process, by electric temperature control valve control temperature at 60-90 DEG C, dissolve, by slip inlet amount and hydrochloric acid flow control and adjusting reaction time within 100-150min, flow is 1-1000L; PH value controls 4 ~ 4.5, uses online pH meter to detect, links with flow mediation system; Slurries after dissolving achieve the separation of solution, waste residue after being filtered by the first precision surface strainer 7 with overflow type; Solution enters the second receiving tank 8, and waste residue enters the 3rd receiving tank 9 and carries out washery slag.Solution and removal of impurities medicament all adopt constant pressure pump, magnetic flow meter, motorized valve, electro connecting pressure gauge joint control mode is carried out flow control and is entered deblending slot 10 first step and carry out removal of impurities, in reaction process, temperature controls to adopt electric temperature control valve to carry out temperature regulable control, control at 60-90 DEG C, by mass flow control and adjusting reaction time within 20-100min, flow range is 1-1000L, after removal of impurities rear slurry is filtered by second surface strainer 12 with overflow type, obtain qualified rare earth chloride liquid and waste residue, feed liquid enters storage pool 13, use as next procedure, waste residue enters the 3rd receiving tank 9 and carries out washery slag, and add water acid elution, and pH value controls 2 ~ 2.5, and use online pH meter to detect, the reaction times controls within 60-100min, qualified rear slurry carries out solid-liquid separation by the 3rd surface filter 14, and waste residue uses Full-automatic quantitative wrapping machine 15 to pack rear storage, washing lotion flows into washing lotion receiving tank 22 and to size mixing operation for alkali cake.
4. phosphorus alkali lye essence filter Crystallization Procedure
After the phosphorus alkali lye of washing procedure output removes entrained solid particulate matter after the 4th surface filter 16, qualified phosphorus alkali lye enters cooling tower 17 and carries out crystallisation by cooling; Waste residue enters wash water hold-up vessel 18, and crystallisation by cooling rear slurry uses the second band filter 19 to carry out solid-liquid separation, and the solid that the second band filter 19 is produced is finished product tertiary sodium phosphate, carries out quantitative package by finished product automatic packing machine 20, stores and sells; Liquid is waste lye, enters caustic soda liquid preparation tank 21, for the liquid caustic soda preparation reuse of caustic digestion operation.
Embodiment 1:
Be 53% monazite breeze 300g, temperature 155 DEG C for 320 orders, content of rare earth
Processing step:
1. taking 300g monazite breeze adds in reactor;
2. with content be 96% solid caustic soda 288g and 1006ml water prepare NaOH solution and add in reactor;
3. start reactor stirrer and well heater, agitation revolution adjusts to 180 revs/min, starts timing after boiling;
4. constant temperature when temperature is elevated to 155 DEG C, control at 155 ± 5 DEG C, the reaction times controls at 240 ± 10 minutes;
5. degradation production dilutes, filters, washs, drains, cumulative volume 3568ml, bath water 1200ml after dilution; Output phosphorus alkali lye 3425ml, output alkali cake 325.2g;
6. by phosphorus alkali lye crystallisation by cooling, start when temperature is reduced to 40 degree to filter, output 400g tertiary sodium phosphate, output waste lye 1006ml, retain for experiment next time;
7. alkali cake concentration is that 5.78N, volume 525ml hydrochloric acid are excellent molten, and temperature controls at 75 ± 5 DEG C, and the reaction times controls at about 120 ± 10min, and pH value controls to filter after 4 ~ 4.5, obtains a rare earth chloride liquid and an acid dissolution slag;
8. a rare earth chloride liquid adds ammonium sulfate 1.4g and bariumchloride 2.9g removal of impurities, and temperature controls at 75 ± 5 DEG C, and time controling filters at about 60min, obtains product rare earth chloride liquid, and waste residue returns acid dissolution slag slurries;
9. an acid dissolution slag adds wash water and sizes mixing, and with hydrochloric acid, pH value is transferred to 2 ~ 2.5, and stir 30min and filter, filtrate returns alkali cake and sizes mixing, and filter cake fresh water rinses to pH value 5 deslagging;
10. product rare earth chloride liquid is by spray-dryer, and temperature controls at 500 ± 10 DEG C, obtains the anhydrous powder rare earth chloride of 264g.
Embodiment 2:
Be 53% monazite breeze 300g, temperature 130 DEG C for 320 orders, content of rare earth
Processing step:
1. taking 300g monazite breeze adds in reactor;
2. with content be 96% solid caustic soda 288g and 1006ml water prepare NaOH solution and add in reactor;
3. start reactor stirrer and well heater, agitation revolution adjusts to 180 revs/min, starts timing after boiling;
4. constant temperature when temperature is elevated to 130 DEG C, control at 130 ± 5 DEG C, the reaction times controls at 380 ± 10 minutes;
5. degradation production dilutes, filters, washs, drains, cumulative volume 3592ml, bath water 1200ml after dilution; Output phosphorus alkali lye 3425ml, output alkali cake 325.2g;
6. by phosphorus alkali lye crystallisation by cooling, start when temperature is reduced to 40 degree to filter, output 398g tertiary sodium phosphate, output waste lye 1006ml, retain for experiment next time;
7. alkali cake concentration is that 5.78N, volume 525ml hydrochloric acid are excellent molten, and temperature controls at 75 ± 5 DEG C, and the reaction times controls at about 120 ± 10min, and pH value controls to filter after 4 ~ 4.5, obtains a rare earth chloride liquid and an acid dissolution slag;
8. a rare earth chloride liquid adds ammonium sulfate 1.4g and bariumchloride 2.9g removal of impurities, and temperature controls at 75 ± 5 DEG C, and time controling filters at about 90min, obtains product rare earth chloride liquid, and waste residue returns acid dissolution slag slurries;
9. an acid dissolution slag adds wash water and sizes mixing, and with hydrochloric acid, pH value is transferred to 2 ~ 2.5, and stir 30min and filter, filtrate returns alkali cake and sizes mixing, and filter cake fresh water rinses to pH value 5 deslagging;
10. product rare earth chloride liquid is by spray-dryer, and temperature controls at 500 ± 10 DEG C, obtains the anhydrous powder rare earth chloride of 262.4g.
Embodiment 3:
Be 53% monazite breeze 300g, temperature 170 DEG C for 320 orders, content of rare earth
Processing step:
1. taking 300g monazite breeze adds in reactor;
2. with content be 96% solid caustic soda 288g and 1006ml water prepare NaOH solution and add in reactor;
3. start reactor stirrer and well heater, agitation revolution adjusts to 180 revs/min, starts timing after boiling;
4. constant temperature when temperature is elevated to 170 DEG C, control at 170 ± 5 DEG C, the reaction times controls at 240 ± 10 minutes;
5. degradation production dilutes, filters, washs, drains, cumulative volume 3521ml, bath water 1200ml after dilution; Output phosphorus alkali lye 3420ml, output alkali cake 325g;
6. by phosphorus alkali lye crystallisation by cooling, start when temperature is reduced to 40 degree to filter, output 399g tertiary sodium phosphate, output waste lye 1007ml, retain for experiment next time;
7. alkali cake concentration is that 5.78N, volume 525ml hydrochloric acid are excellent molten, and temperature controls at 75 ± 5 DEG C, and the reaction times controls at about 120 ± 10min, and pH value controls to filter after 4 ~ 4.5, obtains a rare earth chloride liquid and an acid dissolution slag;
8. a rare earth chloride liquid adds ammonium sulfate 1.4g and bariumchloride 2.9g removal of impurities, and temperature controls at 75 ± 5 DEG C, and time controling filters at about 60min, obtains product rare earth chloride liquid, and waste residue returns acid dissolution slag slurries;
9. an acid dissolution slag adds wash water and sizes mixing, and with hydrochloric acid, pH value is transferred to 2 ~ 2.5, and stir 30min and filter, filtrate returns alkali cake and sizes mixing, and filter cake fresh water rinses to pH value 5 deslagging;
10. product rare earth chloride liquid is by spray-dryer, and temperature controls at 500 ± 10 DEG C, obtains the anhydrous powder rare earth chloride of 263.2g.
Claims (8)
1. the production method of Extraction of rare earth from solitary stone ore, is characterized in that, comprise the steps:
1) caustic digestion operation
Granularity is that the monazite breeze of more than 200 orders enters weight-loss metering helix balance by pneumatic conveyer by pipeline, promote to enter in JQL reactor first step chamber from fixing material channel by weight-loss metering helix balance, liquid caustic soda and wash water enter JQL reactor by fluid passage and stir in arrival last step chamber step by step, in reaction process, temperature controlling range is 130-170 DEG C, reaction times is within 160-260min, solid-to-liquid ratio is 1:1-10, breeze rate of decomposition can reach more than 99%, slip after stirring enters the band filter first step from JQL reactor last step with overflow type and carries out drip washing and solid-liquid separation,
2) washing procedure
Washing procedure adopts band filter to carry out drip washing and solid-liquid separation, dilution rear slurry enters the band filter first step to carry out phosphorus alkali lye and is separated with alkali cake, phosphorus alkali lye enters phosphorus alkali lye essence filter Crystallization Procedure, alkali cake enters band filter and washs step by step, washing is countercurrent washing, wash water flows into wash water receiving tank, for caustic digestion operation dilution washing; Alkali cake band filter dewaters, and the alkali cake after separation enters the first receiving tank, and the first receiving tank to be sized mixing tank for alkali cake slurries after sizing mixing by acid dissolution slag washing lotion, and alkali cake removes chloride process after sizing mixing;
3) chloride process
Hydrochloric acid enters by slurry channels the dissolving that dissolving tank carries out step by step by alkali cake slurries in fluid passage, the first receiving tank respectively, in reaction process, temperature controls at 60-90 DEG C, control flow is 1-1000L/min, reaction times is within 100-150min, pH value controls 4 ~ 4.5, uses online pH meter to detect, links with flow mediation system; Slurries after dissolving are filtered by surface filter with overflow type, complete the separation of solution, waste residue; Solution enters the second receiving tank, and waste residue enters the 3rd receiving tank and carries out washery slag; Solution and removal of impurities medicament are that 1-1000L/min enters deblending slot and carries out removal of impurities step by step with flow range respectively by fluid passage, in reaction process, temperature controls at 60-90 DEG C, removal of impurities mixing time is within 20-100min, after removal of impurities rear slurry is filtered by surface filter with overflow type, obtain qualified rare earth chloride liquid and waste residue, feed liquid enters storage pool, uses as next procedure; Waste residue enters the 3rd receiving tank and carries out washery slag, and pH value controls 2 ~ 2.5, and use online pH meter to detect, the reaction times controls within 15-100min; Qualified rear slurry carries out solid-liquid separation by surface filter, and waste residue stores after using Full-automatic quantitative wrapping machine packaging; Washing lotion is used for alkali cake and sizes mixing operation;
4) phosphorus alkali lye essence filter Crystallization Procedure
After the phosphorus alkali lye of washing procedure output removes entrained solid particulate matter after surface filter, qualified phosphorus alkali lye enters cooling tower and carries out crystallisation by cooling; Waste residue enters wash water storage pool, and crystallisation by cooling rear slurry uses band filter to carry out solid-liquid separation, and the solid that band filter is produced is finished product tertiary sodium phosphate, carries out quantitative package by device of full automatic packaging, stores and sells; Liquid is waste lye, for the liquid caustic soda preparation reuse of caustic digestion operation.
2. the device of an Extraction of rare earth from solitary stone ore, it is characterized in that, comprise: pneumatic conveyer is connected with weight-loss metering helix balance by pipeline, weight-loss metering helix balance is connected with the solids inlet of JQL reactor, and liquid is connected with JQL reactor by fluid passage; JQL reactor outlet is connected with band filter fluid inlet by pipeline, band filter is divided into three output branch roads and a liquid input branch road, band filter one is exported branch road and is connected with the first receiving tank by pipeline, slurries and the liquid storage tank of the first receiving tank are connected with dissolving tank by liquid line, dissolving tank is connected with surface filter respectively by pipeline, surface filter is two branch roads, and a branch road is connected with the second receiving tank, and another branch road is connected with the 3rd receiving tank; Second receiving tank is connected with deblending slot by fluid passage, and deblending slot is connected with removal of impurities medicament storage tank; Deblending slot outlet is connected with surface filter, and surface filter divides two branch roads, and a branch road is connected with the 3rd receiving tank, and another branch road is connected with storage pool; 3rd receiving tank is connected with surface filter by slurry channels, and surface filter is divided into two branch roads, and a branch road is connected with waste residue automatic packing machine, and another branch road is by fluid passage reuse; Band filter second branch road is connected with surface filter, and surface filter is divided into two branch roads, and the first branch road is connected with cooling tower, and another branch road is connected with wash water receiving tank; Cooling tower is connected with band filter, and band filter is divided into two branch roads, and the first branch road is connected with finished product automatic packing machine, and another branch road is by fluid passage reuse; Band filter the 3rd branch road is connected with wash water hold-up vessel by wash water pipeline.
3. the device of a kind of Extraction of rare earth from solitary stone ore according to claim 2, it is characterized in that, described oar liquid passage and fluid passage are equipped with fully automatic culculating system, and described fully automatic culculating system comprises: liquid caustic soda adopts constant pressure pump, magnetic flow meter, motorized valve, electro connecting pressure gauge.
4. the device of a kind of Extraction of rare earth from solitary stone ore according to claim 2, it is characterized in that, JQL reactor comprises: cell body, cell body is separated at least two-stage chamber by end plate, the baffle plate perpendicular to base plate is provided with in each chamber, chamber cavity forms octagon structure, described first step chamber is respectively equipped with solid materials passage and fluid passage and slurry channel, slurry passage and fixing material channel have potential difference, the chamber of every grade is equipped with slurry channel, slurry channel has potential difference, the end plate of last step chamber is provided with discharge port, whipping appts is established in the chamber of every grade.
5. the device of a kind of Extraction of rare earth from solitary stone ore according to claim 4, is characterized in that, the potential difference of the slurry channel of every grade of chamber is vertical parallax or left and right potential difference.
6. the device of a kind of Extraction of rare earth from solitary stone ore according to claim 4, it is characterized in that, described cell body is provided with lid, is provided with sealing member between lid and cell body.
7. the device of a kind of Extraction of rare earth from solitary stone ore according to claim 6, it is characterized in that, the whipping appts on described lid penetrates between hole and whipping appts and is provided with sealing member.
8. the device of a kind of Extraction of rare earth from solitary stone ore according to claim 2, it is characterized in that, described dissolving tank comprises: cell body, cell body is separated at least two-stage chamber by end plate, and described first step chamber is respectively equipped with material channel, and slurry passage and fixing material channel have potential difference, the chamber of every grade is equipped with slurry channel, slurry channel has potential difference, and the end plate of last step chamber is provided with discharge port, establishes whipping appts in the chamber of every grade.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510735519.9A CN105200230A (en) | 2015-10-18 | 2015-11-03 | Production method and device for extracting rare earth from monazite ores |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510668971 | 2015-10-18 | ||
| CN2015106689718 | 2015-10-18 | ||
| CN201510735519.9A CN105200230A (en) | 2015-10-18 | 2015-11-03 | Production method and device for extracting rare earth from monazite ores |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105200230A true CN105200230A (en) | 2015-12-30 |
Family
ID=54948183
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520867018.1U Expired - Fee Related CN205313638U (en) | 2015-10-18 | 2015-11-03 | Draw device of tombarthite among solitary quarry of follow |
| CN201510735519.9A Pending CN105200230A (en) | 2015-10-18 | 2015-11-03 | Production method and device for extracting rare earth from monazite ores |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520867018.1U Expired - Fee Related CN205313638U (en) | 2015-10-18 | 2015-11-03 | Draw device of tombarthite among solitary quarry of follow |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN205313638U (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591607A (en) * | 2016-12-10 | 2017-04-26 | 包头稀土研究院 | Liquid alkali decomposition method of high-grade mixed rare earth ore concentrate |
| CN107699717A (en) * | 2017-09-29 | 2018-02-16 | 永州市零陵远达新材料有限公司 | A kind of method that solitary stone ore of zircon sand association is processed into rare earth chloride |
| CN108130433A (en) * | 2017-11-29 | 2018-06-08 | 中铝广西国盛稀土开发有限公司 | A kind of method that rare-earth precipitation process effectively removes chlorine, sodium ion |
| CN110129559A (en) * | 2019-06-21 | 2019-08-16 | 缙云松弛自动化科技有限公司 | A kind of rare earth ore residue purification processes device |
| CN111004932A (en) * | 2019-12-26 | 2020-04-14 | 湖南中核金原新材料有限责任公司 | Six-tank continuous hydrochloric acid preferential dissolution method for monazite alkali cake |
| CN111039316A (en) * | 2019-12-26 | 2020-04-21 | 湖南中核金原新材料有限责任公司 | Continuous multi-stage countercurrent washing method for monazite alkali bottom slurry decomposition |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205313638U (en) * | 2015-10-18 | 2016-06-15 | 包头市锦园化工科技有限公司 | Draw device of tombarthite among solitary quarry of follow |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2811411A (en) * | 1951-10-16 | 1957-10-29 | George D Calkins | Method of processing monazite sand |
| CN1384214A (en) * | 2001-04-29 | 2002-12-11 | 路远 | Carbon reducting roast process of producing RE chloride with mixed RE concentrate |
| CN102251106A (en) * | 2011-06-04 | 2011-11-23 | 内蒙古科技大学 | Method for decomposing rare earth concentrate in Baotou by alkaline process |
| CN103045851A (en) * | 2013-01-17 | 2013-04-17 | 中国科学院长春应用化学研究所 | Technique for decomposing Baotou rare-earth ores |
| CN204589269U (en) * | 2015-04-21 | 2015-08-26 | 永州市湘江稀土有限责任公司 | A kind of mengite rare-earth mine alkaline process decomposing system adopting far-infrared heating |
| CN205313638U (en) * | 2015-10-18 | 2016-06-15 | 包头市锦园化工科技有限公司 | Draw device of tombarthite among solitary quarry of follow |
-
2015
- 2015-11-03 CN CN201520867018.1U patent/CN205313638U/en not_active Expired - Fee Related
- 2015-11-03 CN CN201510735519.9A patent/CN105200230A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2811411A (en) * | 1951-10-16 | 1957-10-29 | George D Calkins | Method of processing monazite sand |
| CN1384214A (en) * | 2001-04-29 | 2002-12-11 | 路远 | Carbon reducting roast process of producing RE chloride with mixed RE concentrate |
| CN102251106A (en) * | 2011-06-04 | 2011-11-23 | 内蒙古科技大学 | Method for decomposing rare earth concentrate in Baotou by alkaline process |
| CN103045851A (en) * | 2013-01-17 | 2013-04-17 | 中国科学院长春应用化学研究所 | Technique for decomposing Baotou rare-earth ores |
| CN204589269U (en) * | 2015-04-21 | 2015-08-26 | 永州市湘江稀土有限责任公司 | A kind of mengite rare-earth mine alkaline process decomposing system adopting far-infrared heating |
| CN205313638U (en) * | 2015-10-18 | 2016-06-15 | 包头市锦园化工科技有限公司 | Draw device of tombarthite among solitary quarry of follow |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591607A (en) * | 2016-12-10 | 2017-04-26 | 包头稀土研究院 | Liquid alkali decomposition method of high-grade mixed rare earth ore concentrate |
| CN107699717A (en) * | 2017-09-29 | 2018-02-16 | 永州市零陵远达新材料有限公司 | A kind of method that solitary stone ore of zircon sand association is processed into rare earth chloride |
| CN108130433A (en) * | 2017-11-29 | 2018-06-08 | 中铝广西国盛稀土开发有限公司 | A kind of method that rare-earth precipitation process effectively removes chlorine, sodium ion |
| CN110129559A (en) * | 2019-06-21 | 2019-08-16 | 缙云松弛自动化科技有限公司 | A kind of rare earth ore residue purification processes device |
| CN111004932A (en) * | 2019-12-26 | 2020-04-14 | 湖南中核金原新材料有限责任公司 | Six-tank continuous hydrochloric acid preferential dissolution method for monazite alkali cake |
| CN111039316A (en) * | 2019-12-26 | 2020-04-21 | 湖南中核金原新材料有限责任公司 | Continuous multi-stage countercurrent washing method for monazite alkali bottom slurry decomposition |
Also Published As
| Publication number | Publication date |
|---|---|
| CN205313638U (en) | 2016-06-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN205313638U (en) | Draw device of tombarthite among solitary quarry of follow | |
| CN102001636B (en) | Method for producing broad-concentration phosphoric acid and clean plaster by middle-low grade phosphorus ore wet process | |
| CN105271333B (en) | A kind of method that potassium dihydrogen phosphate and aluminium hydroxide are produced by potassium feldspar | |
| CN105905933B (en) | Fluoride waste reclaims the artificial fluorite technique of high purity | |
| CN102887535A (en) | Method for recycling high-purity fluorine and phosphorus from wastewater of phosphogypsum residue field | |
| CN103342375B (en) | The method of aluminum oxide, silicon-dioxide and other metal ingredient is reclaimed from flyash | |
| CN103693670B (en) | Production method of calcium sulphate dehydrate and production device thereof | |
| CN105256143A (en) | Method for extracting scandium and other rare earth from zirconium oxychloride acid pickle | |
| CN102732731A (en) | Method for extracting valuable metals and refining zinc sulphate monohydrate from zinc-containing waste material | |
| CN108034816A (en) | A kind of rare earths separation method in monazite | |
| CN207845730U (en) | A kind of wet method carries cobalt device | |
| CN102515114B (en) | A kind of method that titanium white waste acid high level efficiently utilizes | |
| CN104030327B (en) | A kind of Bischofite in Salt lake continuous-dissolution produces the method for high density magnesium chloride solution | |
| CN103215451B (en) | Recovery method of rare earth elements in ionic rare earth smelting acid dissolution slag | |
| CN103771461B (en) | Double decomposition method for preparing potassium nitrate | |
| CN104445281A (en) | Waste residue comprehensive utilization method for trichlorosilane leaching system | |
| CN103602837A (en) | Method for collecting scandium oxide from anatase associated scandium mineral | |
| CN108950250B (en) | Method for recovering rare earth in neodymium iron boron waste acid-soluble slag | |
| CN104711428B (en) | Method for preparing and recovering metal in pickling sludge | |
| CN104261371B (en) | A kind of method by high impurity phosphorus ore production diammonium phosphate | |
| CN102560158A (en) | Transformation method for mixed rare earth concentrate and concentrated sulfuric acid low-temperature roasted ore | |
| CN102976382B (en) | Method for regenerating cryolite from electrolytic aluminum waste material | |
| CN105152195A (en) | Treatment method and apparatus for controlled filter cakes in Bayer process for alumina production | |
| CN104692442A (en) | Method for preparing high-purity and high-strength gypsum through medium- and low-level phosphorite associated calcium sources | |
| CN204550084U (en) | For the tripping device of useful component in Bayer process red mud |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20151230 |
|
| WD01 | Invention patent application deemed withdrawn after publication |