CN106967891B - A method of the gradient recovering rare earth from rare earth phosphor mixing waste - Google Patents
A method of the gradient recovering rare earth from rare earth phosphor mixing waste Download PDFInfo
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Abstract
The present invention relates to a kind of methods of gradient recovering rare earth in mixing waste from rare earth phosphor, and rare earth phosphor mixing waste is first carried out direct acidleach, obtain the re dip solution rich in Y and Eu and direct acid leaching residue；For direct acid leaching residue after alkali converts, output alkali converts rare earth material；Alkali conversion rare earth material is stirred leaching dealuminzation, obtains the conversion rare earth material of the alkali after dealuminzation；Finally, the alkali conversion rare earth material after dealuminzation carries out reducing leaching, obtains the re dip solution rich in Ce and Tb.Rare earth leaching rate of the present invention reaches 98.00wt% or more, has the advantages that rare earth leaching rate is high, re dip solution composition is simple, re dip solution is easily isolated purification, reagent consumes less, processing cost is low etc..
Description
Technical field
The invention belongs to secondary rare earth resources recycling fields, and in particular to one kind is from rare earth phosphor mixing waste
The method of gradient recovering rare earth.
Background technology
With the use of the products such as fluorescent lamp, high-end display screen, the yield of rare earth phosphor gradually increases, therefore rare earth is glimmering
Light powder mixing waste increases year by year.And rare earth is the indispensable raw material of high-end product, is constantly subjected to the great attention of country.If
Can from rare earth phosphor mixing waste economically synthetical recovery rare earth, it is horizontal on the one hand to improve rare earth resources recycling, and
National strategy rare earth resources are increased, another aspect environmental protection will be with great strategic importance and realistic meaning.At present
The method that mainly uses of the country be directly with Ore Leaching or or oxygenation pretreatment after acidleach again, finally obtain mixed rare earth solution.Its
In, the major defect of direct acidleach is that rare earth leaching rate is low；And the major defect of acidleach is that quantity of alkali consumption is big again after oxygenation pretreatment,
And mixed rare earth solution includes rare earth element all in rare earth phosphor mixing waste, and it is complex in composition, lead to follow-up rare earth
Separation is more difficult, therefore cost is higher.
Invention content
The purpose of the present invention is be directed at present from rare earth phosphor mixing waste recovering rare earth that there are rare earth yields is low,
The problems such as reagent consumption is big, re dip solution rare earth elements type is more, of high cost provides a kind of from rare earth phosphor mixing
The method of gradient recovering rare earth in waste material, makes rare earth leaching rate reach 98% or more.
The present invention takes following technical scheme, a method of the gradient recovering rare earth from rare earth phosphor mixing waste,
Include the steps that next coming in order carry out：
Step (1), the direct acidleach of rare earth phosphor mixing waste：It is incorporated hydrochloric acid into rare earth phosphor mixing waste and stirs
It mixes, endpoint pH, extraction temperature, extraction time and liquid-solid ratio (mL/g) are leached in control, are separated by solid-liquid separation, are obtained after leaching
To containing Rare Earth Y and Eu re dip solution and direct acid leaching residue；
Step (2), the direct acid leaching residue alkali that step (1) is obtained convert：Control mass ratio, the alkali of alkali and direct acid leaching residue
Conversion temperature and time are cooled to room temperature (25 DEG C) after reaction, and output alkali converts rare earth material；
Step (3), the alkali that step (2) is obtained convert rare earth material dealuminzation：In order to improve rare earth leaching rate and reduction
Aluminium content in re dip solution is stirred leaching aluminium；Water is only added in leaching process, when controlling extraction temperature, leaching
Between and liquid-solid ratio (mL/g), obtain the alkali after aluminium leachate and dealuminzation conversion rare earth material, aluminium leachate otherwise processed；
Step (4), the alkali after the dealuminzation that step (3) is obtained convert rare earth material acidleach：It is dilute toward the alkali conversion after dealuminzation
It is incorporated hydrochloric acid and reducing agent in local product material and stirs, endpoint pH, reductant concentration, extraction temperature, extraction time are leached in control
It with liquid-solid ratio (mL/g), is separated by solid-liquid separation after leaching, obtains the re dip solution containing Rare-Earth Ce and Tb and rare earth acidleach
Slag.
Salt Ore Leaching endpoint pH in the step (1) is 2.0~4.0, and extraction temperature is 80 DEG C~95 DEG C, when leaching
Between be 60min~120min, liquid-solid ratio (mg/L) be 4：1~10：1.
The mass ratio of alkali in the step (2) and direct acid leaching residue is 0.9~1.0, alkali conversion temperature is 830 DEG C~
950 DEG C, alkali transformation time is 100min~160min.
Extraction temperature in the step (3) is 80 DEG C~95 DEG C, and extraction time is 30min~60min, liquid-solid ratio (mL/
G) it is 3：1~4：1.
Leaching endpoint pH in the step (4) is 2.0~4.0, and reductant concentration is 1.5mol/L~1.7mol/L,
Extraction temperature is 80 DEG C~95 DEG C, and extraction time is 60min~120min, and liquid-solid ratio (mg/L) is 4：1~10：1.
The alkali used in the step (2) is NaOH, Na2CO3, KOH or K2CO3In one kind.
Reducing agent in the step (4) is one kind in sodium nitrite or hydrogen peroxide.
Mixing speed in step (1), step (3), step (4) is 360r/min~500r/min.
The rare earth leaching rate of the present invention reaches 98.00wt% or more, and rare earth leaching rate is high, respectively obtains rich in Y's and Eu
Re dip solution and re dip solution rich in Ce and Tb, realize the purpose of gradient recovering rare earth, alleviate follow-up rare earth point
Burden from purification, and reduce the dosage of alkali, therefore reduce production cost.
Specific implementation mode
The present invention is further described with reference to embodiments, but is not meant to limiting the scope of the invention：
Embodiment 1
Take RE containing rare earth oxide2O349.32wt%, Al2O3The rare earth phosphor mixing waste of 40.39wt%, wherein
RE2O3Partition (form) be Y2O382.36wt%, CeO26.77wt%, Eu2O36.50wt%, Th4O74.18wt%,
Er2O30.19wt%.
First, rare earth phosphor mixing waste directly stirs acidleach, and leaching condition is：Salt Ore Leaching endpoint pH is 2.0,
Extraction temperature is 80 DEG C, extraction time 60min, and liquid-solid ratio (mg/L) is 4：1, mixing speed 360r/min.Leaching terminates
After be filtered, respectively obtain re dip solution containing Y and Eu and with direct acid leaching residue, the rare earth leaching rate of direct acidleach is
85.13%, and Y in re dip solution and Eu account for the 96wt% or more of total rare earth (TRE) in re dip solution.
Secondly, direct acid leaching residue is subjected to alkali conversion, alkali conversion condition is：K2CO3Mass ratio with direct acid leaching residue is
1.0, alkali conversion temperature is 950 DEG C, and alkali transformation time is 160min.After alkali converts, it is cooled to room temperature (25 DEG C), output alkali
Convert rare earth material.
Then, alkali conversion rare earth material carries out dealuminzation, and water, specific leaching condition are only added in dealumination process
For：Temperature is 80 DEG C, extraction time 60min, and liquid-solid ratio (mL/g) is 4：1, mixing speed 500r/min.Leaching terminates
Afterwards, it is filtered, respectively obtains the conversion rare earth material of the alkali after aluminium leachate and dealuminzation, aluminium leachate otherwise processed.
Finally, the alkali conversion rare earth material after dealuminzation carries out acidleach, and leaching condition is：Salt Ore Leaching endpoint pH is
2.0, a concentration of 1.6mol/L of sodium nitrite, extraction temperature are 80 DEG C, extraction time 60min, and liquid-solid ratio (mg/L) is 4：1,
Mixing speed is 360r/min.It after leaching, is filtered, respectively obtains re dip solution and rare earth containing Rare-Earth Ce and Tb
Acid leaching residue, the rare earth leaching rate of the alkali conversion rare earth material acidleach after dealuminzation are 90.21wt%, and the Ce in re dip solution and
Tb accounts for the 92wt% or more of total rare earth (TRE) in re dip solution.
The present embodiment respectively obtains the re dip solution containing Rare Earth Y and Eu and the re dip solution containing Rare-Earth Ce and Tb, leaching
Go out that liquid rare earth elements are simple, reduces the difficulty of later separation purification, be in this two kinds of total leaching rates of leachate middle rare earth
98.54wt% achievees the purpose that gradient recovering rare earth, advantageously reduces production cost.
Embodiment 2
Take RE containing rare earth oxide2O349.32wt%, Al2O3The rare earth phosphor mixing waste of 40.39wt%, wherein
RE2O3Partition (form) be Y2O382.36wt%, CeO26.77wt%, Eu2O36.50wt%, Th4O74.18wt%,
Er2O30.19wt%.
First, rare earth phosphor mixing waste directly stirs acidleach, and leaching condition is：Salt Ore Leaching endpoint pH is 3.0,
Extraction temperature is 95 DEG C, extraction time 90min, and liquid-solid ratio (mg/L) is 10：1, mixing speed 500r/min.Leaching terminates
After be filtered, obtain re dip solution containing Y and Eu and with direct acid leaching residue, the rare earth leaching rate of direct acidleach is
84.28%, and Y in re dip solution and Eu account for the 96wt% or more of total rare earth (TRE) in re dip solution.
Secondly, direct acid leaching residue is subjected to alkali conversion, alkali conversion condition is：The mass ratio of KOH and direct acid leaching residue is
0.95, alkali conversion temperature is 890 DEG C, and alkali transformation time is 120min.After alkali converts, it is cooled to room temperature (25 DEG C), output
Alkali converts rare earth material.
Then, alkali conversion rare earth material carries out dealuminzation, and water, specific leaching condition are only added in dealumination process
For：Temperature is 90 DEG C, extraction time 45min, and liquid-solid ratio (mL/g) is 3.5：1, mixing speed 430r/min.Leaching terminates
Afterwards, it is filtered, respectively obtains the conversion rare earth material of the alkali after aluminium leachate and dealuminzation, aluminium leachate otherwise processed.
Finally, the alkali conversion rare earth material after dealuminzation carries out acidleach, and leaching condition is：Salt Ore Leaching endpoint pH is
3.0, hydrogen peroxide concentration 1.7mol/L, extraction temperature are 95 DEG C, extraction time 120min, and liquid-solid ratio (mg/L) is 10：1,
Mixing speed is 500r/min.It after leaching, is filtered, respectively obtains re dip solution and rare earth containing Rare-Earth Ce and Tb
Acid leaching residue, the rare earth leaching rate of the alkali conversion rare earth material acidleach after dealuminzation are 89.98wt%, and the Ce in re dip solution and
Tb accounts for the 92wt% or more of total rare earth (TRE) in re dip solution.
The present embodiment respectively obtains the re dip solution mainly containing Rare Earth Y and Eu and is leached containing the rare earth of Rare-Earth Ce and Tb
Liquid, leachate rare earth elements are simple, reduce the difficulty of later separation purification, always leached in this two kinds of leachate middle rare earth
Rate is 98.42wt%, achievees the purpose that gradient recovering rare earth, advantageously reduces production cost.
Embodiment 3
Take RE containing rare earth oxide2O349.32wt%, Al2O3The rare earth phosphor mixing waste of 40.39wt%, wherein
RE2O3Partition (form) be Y2O382.36wt%, CeO26.77wt%, Eu2O36.50wt%, Th4O74.18wt%,
Er2O30.19wt%.
First, rare earth phosphor mixing waste directly stirs acidleach, and leaching condition is：Salt Ore Leaching endpoint pH is 4.0,
Extraction temperature is 87 DEG C, extraction time 120min, and liquid-solid ratio (mg/L) is 7：1, mixing speed 430r/min.Leaching terminates
After be filtered, obtain re dip solution containing Y and Eu and with direct acid leaching residue, the rare earth leaching rate of direct acidleach is
85.77%, and Y in re dip solution and Eu account for the 96wt% or more of total rare earth (TRE) in re dip solution.
Secondly, direct acid leaching residue is subjected to alkali conversion, alkali conversion condition is：The mass ratio of NaOH and direct acid leaching residue is
1.0, alkali conversion temperature is 830 DEG C, and alkali transformation time is 100min.After alkali converts, it is cooled to room temperature (25 DEG C), output alkali
Convert rare earth material.
Then, alkali conversion rare earth material carries out dealuminzation, and water, specific leaching condition are only added in dealumination process
For：Temperature is 95 DEG C, extraction time 30min, and liquid-solid ratio (mL/g) is 3：1, mixing speed 360r/min.Leaching terminates
Afterwards, it is filtered, respectively obtains the conversion rare earth material of the alkali after aluminium leachate and dealuminzation, aluminium leachate otherwise processed.
Finally, the alkali conversion rare earth material after dealuminzation carries out acidleach, and leaching condition is：Salt Ore Leaching endpoint pH is
4.0, hydrogen peroxide concentration is 1.5mol/L~1.7mol/L, and extraction temperature is 88 DEG C, extraction time 90min, liquid-solid ratio (mg/
L it is) 7：1, mixing speed 430r/min.It after leaching, is filtered, respectively obtains and leached containing the rare earth of Rare-Earth Ce and Tb
Liquid and rare earth acid leaching residue, the rare earth leaching rate of the alkali conversion rare earth material acidleach after dealuminzation are 90.31wt%, and re dip solution
In Ce and Tb account for the 92wt% or more of total rare earth (TRE) in re dip solution..
The present embodiment respectively obtains the re dip solution containing Rare Earth Y and Eu and the re dip solution containing Rare-Earth Ce and Tb, leaching
Go out that liquid rare earth elements are simple, reduces the difficulty of later separation purification, be in this two kinds of total leaching rates of leachate middle rare earth
98.62wt% achievees the purpose that gradient recovering rare earth, advantageously reduces production cost.
Embodiment 4
Take RE containing rare earth oxide2O349.32wt%, Al2O3The rare earth phosphor mixing waste of 40.39wt%, wherein
RE2O3Partition (form) be Y2O382.36wt%, CeO26.77wt%, Eu2O36.50wt%, Th4O74.18wt%,
Er2O30.19wt%.
First, rare earth phosphor mixing waste directly stirs acidleach, and leaching condition is：Salt Ore Leaching endpoint pH is 2.5,
Extraction temperature is 90 DEG C, extraction time 100min, and liquid-solid ratio (mg/L) is 5：1, mixing speed 400r/min.Leaching terminates
After be filtered, obtain re dip solution containing Y and Eu and with direct acid leaching residue, the rare earth leaching rate of direct acidleach is
84.89%, and Y in re dip solution and Eu account for the 96wt% or more of total rare earth (TRE) in re dip solution.
Secondly, direct acid leaching residue is subjected to alkali conversion, alkali conversion condition is：Na2CO3Mass ratio with direct acid leaching residue is
0.98, alkali conversion temperature is 930 DEG C, and alkali transformation time is 140min.After alkali converts, it is cooled to room temperature (25 DEG C), output
Alkali converts rare earth material.
Then, alkali conversion rare earth material carries out dealuminzation, and water, specific leaching condition are only added in dealumination process
For：Temperature is 92 DEG C, extraction time 50min, and liquid-solid ratio (mL/g) is 3：1, mixing speed 400r/min.Leaching terminates
Afterwards, it is filtered, respectively obtains the conversion rare earth material of the alkali after aluminium leachate and dealuminzation, aluminium leachate otherwise processed.
Finally, the alkali conversion rare earth material after dealuminzation carries out acidleach, and leaching condition is：Salt Ore Leaching endpoint pH is
2.0~4.0, a concentration of 1.7mol/L of sodium nitrite, extraction temperature are 90 DEG C, extraction time 100min, liquid-solid ratio (mg/L)
It is 5：1, mixing speed 400r/min.It after leaching, is filtered, respectively obtains the re dip solution containing Rare-Earth Ce and Tb
Rare earth leaching rate with rare earth acid leaching residue, the alkali conversion rare earth material acidleach after dealuminzation is 89.85wt%, and in re dip solution
Ce and Tb account for the 92wt% or more of total rare earth (TRE) in re dip solution..
The present embodiment respectively obtains the re dip solution containing Rare Earth Y and Eu and the re dip solution containing Rare-Earth Ce and Tb, leaching
Go out that liquid rare earth elements are simple, reduces the difficulty of later separation purification, be in this two kinds of total leaching rates of leachate middle rare earth
98.47wt% achievees the purpose that gradient recovering rare earth, advantageously reduces production cost.
Claims (2)
1. a kind of method of gradient recovering rare earth in mixing waste from rare earth phosphor includes the steps that next coming in order carry out：
Step (1), the direct acidleach of rare earth phosphor mixing waste：It is incorporated hydrochloric acid into rare earth phosphor mixing waste and stirs,
Endpoint pH, extraction temperature, extraction time and liquid-solid ratio are leached in control, are separated by solid-liquid separation after leaching, obtain containing Rare Earth Y
Re dip solution with Eu and direct acid leaching residue；
Step (2), the direct acid leaching residue alkali that step (1) is obtained convert：Control the mass ratio of alkali and direct acid leaching residue, alkali converts
Temperature and time is cooled to room temperature after reaction, and output alkali converts rare earth material；
Step (3), the alkali that step (2) is obtained convert rare earth material dealuminzation：In order to improve rare earth leaching rate and reduce rare earth
Aluminium content in leachate is stirred leaching aluminium；Only be added water in leaching process, control extraction temperature, extraction time and
Liquid-solid ratio obtains the conversion rare earth material of the alkali after aluminium leachate and dealuminzation, aluminium leachate otherwise processed；
Step (4), the alkali after the dealuminzation that step (3) is obtained convert rare earth material acidleach：Rare earth object is converted toward the alkali after dealuminzation
It is incorporated hydrochloric acid and reducing agent in material and stirs, endpoint pH, reductant concentration, extraction temperature, extraction time and liquid are leached in control
Gu ratio, is separated by solid-liquid separation after leaching, obtains the re dip solution containing Rare-Earth Ce and Tb and rare earth acid leaching residue；
Salt Ore Leaching endpoint pH in the step (1) is 2.0~4.0, and extraction temperature is 80 DEG C~95 DEG C, and extraction time is
60min~120min, liquid-solid ratio mg/L are 4：1~10：1；
The mass ratio of alkali and direct acid leaching residue in the step (2) is 0.9~1.0, and alkali conversion temperature is 830 DEG C~950 DEG C,
Alkali transformation time is 100min~160min；
Extraction temperature in the step (3) is 80 DEG C~95 DEG C, and extraction time is 30min~60min, and liquid-solid ratio mL/g is 3：
1~4：1；
Leaching endpoint pH in the step (4) is 2.0~4.0, and reductant concentration is 1.5mol/L~1.7mol/L, is leached
Temperature is 80 DEG C~95 DEG C, and extraction time is 60min~120min, and liquid-solid ratio mg/L is 4：1~10：1；
The alkali used in the step (2) is NaOH, Na2CO3, KOH or K2CO3In one kind；
Reducing agent in the step (4) is one kind in sodium nitrite or hydrogen peroxide.
2. the method for gradient recovering rare earth, feature in a kind of mixing waste from rare earth phosphor according to claim 1
It is：Mixing speed in step (1), step (3), step (4) is 360r/min~500r/min.
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| CN107630143B (en) * | 2017-09-26 | 2019-10-25 | 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 |
| CN110983038A (en) * | 2020-01-03 | 2020-04-10 | 四川省冕宁县方兴稀土有限公司 | Method for inhibiting chlorine generation of acid-leaching rare earth ore and acid leaching method of fluorine-carbon-cerium roasted ore |
| CN112725622B (en) * | 2020-12-02 | 2022-09-09 | 北京工业大学 | Method for recovering rare earth in waste cerium-based rare earth polishing powder by two-step acid leaching gradient separation |
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