CN108588433A - Calcination process is given up the method for rare earth phosphor Extraction of rare earth under a kind of low oxygen concentration atmospheric condition - Google Patents
Calcination process is given up the method for rare earth phosphor Extraction of rare earth under a kind of low oxygen concentration atmospheric condition Download PDFInfo
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- CN108588433A CN108588433A CN201810877644.7A CN201810877644A CN108588433A CN 108588433 A CN108588433 A CN 108588433A CN 201810877644 A CN201810877644 A CN 201810877644A CN 108588433 A CN108588433 A CN 108588433A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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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
The invention discloses a kind of methods of the useless rare earth phosphor Extraction of rare earth of calcination process under low oxygen concentration atmospheric condition.Useless rare earth phosphor and sodium hydroxide are mixed in a certain ratio and are placed on atmosphere kiln roasting by this method.Calcination atmosphere, including the concentration of calcination atmosphere oxygen, pre-aeration time and heat preservation duration of ventilation etc. are controlled in roasting process.After the completion of roasting, go out product of roasting with water logging, the rareearth enriching material after filtering, drying obtains rare earth feed liquid with inorganic Ore Leaching again.For the method under the premise of not introducing new impurity, total leaching rate of rare earth is higher than 99%.
Description
Technical field
The invention belongs to rare earth secondary resource recycle utilization technology fields, more specifically to a kind of low oxygen concentration gas
The method of the useless rare earth phosphor Extraction of rare earth of calcination process under the conditions of atmosphere.
Background technology
Rare earth element has the characteristics such as unique optics, electricity and magnetics, thus is widely used in luminescent material, magnetic material
The fields such as material, hydrogen storage material are referred to as " industrial monosodium glutamate ", " mother of new material " nowadays has become extremely important strategy money
Source.Wherein, rare earth luminescent material contacts the closest with people's daily life, especially in widely applied three base of lighting area
Color rare earth phosphor.According to the relevent statistics, China's fluorescent lamp yield in 2016 is with regard to 40.23 hundred million, every year discarded rare-earth fluorescent light
More than 400,000,000, wherein nearly 2300 tons of rare earth phosphor waste material content is evaluated by market value at that time in these waste phosphor powders
Rare earth resources value is up to about 1,000,000,000 yuan, and discards rare-earth fluorescent light at present and enter landfill yard with house refuse mostly, not only makes
At environmental pollution and the significant wastage of rare earth resources.
Meanwhile with the increase of rare earth demand, factors, the China such as a large amount of cheap outlets and long-term gopher are primary dilute
What soil resource accounted for world's total amount from the 1970s 74% drops to current 23% or so.Therefore, in primary rare earth resources day
Under benefit environment in short supply, as can reinforcing rare earth phosphor high efficiente callback recycling of giving up, the primary mineral products of rare earth can be not only reduced
Yield, and the industry chain of circular economy item that rare earth utilizes can be formed, the utilization benefit of rare earth resources is increased substantially, it is right
The sustainable development of rare-earth trade is of great significance.
The useless rare earth phosphor of recycling at present mainly has two class of physiochemical mutagens and chemical recovery.Physiochemical mutagens include mainly flotation
Separation centrifuges, pneumatic separating, and such method can only tentatively realize the separation of rare earth phosphor and impurity, separating obtained
Fluorescent powder is unable to meet production requirement, and therefore, industry mostly uses greatly chemical recovery.The method of chemical recovery mainly has direct acidleach
Method and alkali fusion pretreatment-acid-hatching of young eggs, the direct acid-hatching of young eggs are destroyed due to being difficult in fluorescent powder（Blue powder and green powder）Aluminum-spinel
Rock-steady structure causes rare earth leaching rate relatively low；Though and alkali fusion pretreatment can destroy aluminum-spinel structure, due in alkali fusion
Ce, Tb are easily oxidized to CeO in the process2、Tb4O7Cause Ce, Tb leaching rate low, only 60-80%, so that total receipts of rare earth
Rate is not high.To solve the problems, such as this, seminar is preferably resolved this and is asked using the useless rare earth phosphor of method processing of iron powder alkali fusion
The total recovery of topic, rare earth is higher than 99%, but the method introduces impurity ferro element, can be that Extraction of rare earth is brought subsequently from pickle liquor
Larger removal of impurities burden, for this purpose, being badly in need of one kind neither introduces new impurity, and can the thorough Extraction of rare earth from useless rare earth phosphor
Method.
Invention content
Present invention generally provides one kind under the premise of not introducing new impurity, and realization is thoroughly extracted from useless rare earth phosphor
The method of rare earth.
To achieve the above object, the present invention provides a kind of useless rare earth phosphors of calcination process under low oxygen concentration atmospheric condition
The method of Extraction of rare earth, this method be by useless rare earth phosphor and sodium hydroxide after evenly mixing, be placed in atmosphere furnace and roasted
It burns, the volumetric concentration for controlling oxygen in calcination atmosphere is 0-0.4%, obtains product of roasting, then product of roasting is washed, is filtered,
Drying obtains rareearth enriching material, and rareearth enriching material through inorganic Ore Leaching, obtains rare earth feed liquid again.
Further, the mixed proportion of the sodium hydroxide and useless rare earth phosphor is 2.8:1-3.4:1.
Further, pre-aeration is carried out before roasting, the pre-aeration time is not less than atmosphere furnace furnace volume and venting flow rate
Ratio.
Further, the holding temperature of roasting is 700-1000 DEG C.
Further, the heat preservation duration of ventilation of roasting is 2.5-4 hours.
Further, the rareearth enriching material is in concentration of hydrochloric acid 4-8mol/L, leaching time 1-4 hours, acidleach temperature
60-80 DEG C, liquid-solid ratio 10:1-15:It is leached under conditions of 1 L/kg and obtains rare earth feed liquid.
Using scheme provided by the invention, compared with prior art, realizes and do not introduce new impurity in the entire system
Under the premise of, realize that the thoroughly Extraction of rare earth from useless rare earth phosphor, the total recovery of rare earth are higher than 99%.
Specific implementation mode
To further appreciate that present disclosure, the present invention is made in conjunction with the embodiments and being further described, and unrestricted
Invention.Without departing from the premise in the spirit of the present invention, the arbitrary improvement of the invention done and replacement are protected in the present invention
Within the scope of.
Embodiment 1：
Solid NaOH and useless rare earth phosphor are pressed 2.8:1 be uniformly mixed be placed in atmosphere furnace, straight argon is passed through into atmosphere furnace
Gas, pre-aeration time to extend 20 minutes on the basis of furnace volume and gas flow ratio, control oxygen concentration in furnace atmosphere
It is 0, ventilates 2.5 hours under conditions of holding temperature is 700 DEG C, product of roasting obtains rare earth after washing, filtering and drying
Enriched substance, then with the hydrochloric acid of 8mol/L, 60 DEG C of acidleach temperature, 10:The condition of 1 liquid-solid ratio leaches 1 h, obtains rare earth material
Liquid.It is 99.26% to measure the total leaching rate of rare earth.
Embodiment 2：
Solid NaOH and useless rare earth phosphor are pressed 3:1 be uniformly mixed be placed in atmosphere furnace, be passed through into atmosphere furnace argon gas with
The mixed gas of oxygen, pre-aeration time to extend 30 minutes on the basis of furnace volume and gas flow ratio, control in stove
Oxygen concentration is 0.1% in atmosphere, is ventilated 3 hours under conditions of holding temperature is 800 DEG C, product of roasting is through washing, filtering and baking
Rareearth enriching material is obtained after dry, then with the hydrochloric acid of 4mol/L, 70 DEG C of acidleach temperature, 12.5:The condition of 1 liquid-solid ratio leaches
1.5 h, obtain rare earth feed liquid.It is 99.14% to measure the total leaching rate of rare earth.
Embodiment 3：
Solid NaOH and useless rare earth phosphor are pressed 3.2:1 be uniformly mixed be placed in tube-type atmosphere furnace, be passed through into atmosphere furnace
The mixed gas of nitrogen and oxygen, pre-aeration time to extend 35 minutes on the basis of furnace volume and gas flow ratio, are controlled
In furnace atmosphere processed oxygen concentration be 0.4%, holding temperature be 750 DEG C under conditions of ventilate 3.5 hours, product of roasting through washing,
Rareearth enriching material is obtained after filtering and drying, then with the hydrochloric acid of 6mol/L, 75 DEG C of acidleach temperature, 15:The condition of 1 liquid-solid ratio
2h is leached, rare earth feed liquid is obtained.It is 99.19% to measure the total leaching rate of rare earth.
Embodiment 4：
Solid NaOH and useless rare earth phosphor are pressed 3.4:1 is positioned in atmosphere furnace after mixing, and argon is passed through into atmosphere furnace
The mixed gas of gas and oxygen, pre-aeration time to extend 40 minutes on the basis of furnace volume and gas flow ratio, control
Oxygen concentration is 0.3% in furnace atmosphere, is ventilated 4 hours under conditions of holding temperature is 900 DEG C, product of roasting is through washing, filtering
With rareearth enriching material is obtained after drying, then with the hydrochloric acid of 5.5mol/L, 80 DEG C of acidleach temperature, 13:The condition of 1 liquid-solid ratio is soaked
Go out 3h, obtains rare earth feed liquid.It is 99.21% to measure the total leaching rate of rare earth.
Comparative example 1：
Solid NaOH and useless rare earth phosphor are pressed 3.4:1 is positioned in atmosphere furnace after mixing, and argon is passed through into atmosphere furnace
The mixed gas of gas and oxygen, pre-aeration time to extend 40 minutes on the basis of furnace volume and gas flow ratio, control
Oxygen concentration is 0.5% in furnace atmosphere, is ventilated 4 hours under conditions of holding temperature is 900 DEG C, product of roasting is through washing, filtering
With rareearth enriching material is obtained after drying, then with the hydrochloric acid of 5.5mol/L, 80 DEG C of acidleach temperature, 13:The condition of 1 liquid-solid ratio is soaked
Go out 3h, obtains rare earth feed liquid.It is 90.36% to measure the total leaching rate of rare earth.
Claims (6)
1. a kind of method of the useless rare earth phosphor Extraction of rare earth of calcination process under low oxygen concentration atmospheric condition, it is characterised in that：It will
Useless rare earth phosphor after evenly mixing, is placed in atmosphere furnace and is roasted with sodium hydroxide, controls the body of oxygen in calcination atmosphere
A concentration of 0-0.4% of product, obtains product of roasting, and product of roasting washing, filtering, drying are then obtained rareearth enriching material, and rare earth is rich
Collect object again through inorganic Ore Leaching, obtains rare earth feed liquid.
2. according to the method described in claim 1, it is characterized in that：The mass mixing of the sodium hydroxide and useless rare earth phosphor
Ratio is 2.8:1-3.4:1.
3. according to the method described in claim 1, it is characterized in that：Pre-aeration is carried out before roasting, the pre-aeration time is not less than gas
The ratio of atmosphere stove furnace volume and venting flow rate.
4. method according to any one of claim 1-3, it is characterised in that：The holding temperature of roasting is 700-1000
℃。
5. method according to any one of claim 1-3, it is characterised in that：The heat preservation duration of ventilation of roasting is 2.5-4
Hour.
6. method according to any one of claim 1-3, it is characterised in that：The rareearth enriching material is in concentration of hydrochloric acid
4-8mol/L, leaching time 1-4 hours, 60-80 DEG C of acidleach temperature, liquid-solid ratio 10:1-15:It leaches and obtains under conditions of 1L/kg
Rare earth feed liquid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810877644.7A CN108588433A (en) | 2018-08-03 | 2018-08-03 | Calcination process is given up the method for rare earth phosphor Extraction of rare earth under a kind of low oxygen concentration atmospheric condition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810877644.7A CN108588433A (en) | 2018-08-03 | 2018-08-03 | Calcination process is given up the method for rare earth phosphor Extraction of rare earth under a kind of low oxygen concentration atmospheric condition |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946896A (en) * | 2015-07-15 | 2015-09-30 | 江西理工大学 | Method for extracting rare earth from waste rare earth phosphors |
| CN106498192A (en) * | 2016-12-13 | 2017-03-15 | 江苏省冶金设计院有限公司 | A kind of revolving bed processes the method and system of rare earth ore concentrate |
| CN107630143A (en) * | 2017-09-26 | 2018-01-26 | 赣南师范大学 | Method for extracting rare earth from rare earth fluorescent powder waste and fluorine-containing rare earth electrolysis waste residue |
-
2018
- 2018-08-03 CN CN201810877644.7A patent/CN108588433A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946896A (en) * | 2015-07-15 | 2015-09-30 | 江西理工大学 | Method for extracting rare earth from waste rare earth phosphors |
| CN106498192A (en) * | 2016-12-13 | 2017-03-15 | 江苏省冶金设计院有限公司 | A kind of revolving bed processes the method and system of rare earth ore concentrate |
| CN107630143A (en) * | 2017-09-26 | 2018-01-26 | 赣南师范大学 | Method for extracting rare earth from rare earth fluorescent powder waste and fluorine-containing rare earth electrolysis waste residue |
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Application publication date: 20180928 |