CN106586995B - A kind of method of efficient process lithium phosphate reclaimed materials - Google Patents
A kind of method of efficient process lithium phosphate reclaimed materials Download PDFInfo
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- CN106586995B CN106586995B CN201611206808.0A CN201611206808A CN106586995B CN 106586995 B CN106586995 B CN 106586995B CN 201611206808 A CN201611206808 A CN 201611206808A CN 106586995 B CN106586995 B CN 106586995B
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- lithium
- lithium phosphate
- reclaimed materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
Abstract
The present invention relates to the methods for separating from Resource recovery and extracting valuable material, and in particular to a kind of method of efficient process lithium phosphate reclaimed materials belongs to resource circulation utilization field.It is an object of the invention to the technical deficiencies of the processing for existing lithium phosphate reclaimed materials, there is provided a kind of processing step is simple and efficient, processing cost is cheap, be suitble to industrialized production efficient process lithium phosphate reclaimed materials method, inorganic acid solution dissolving phosphoric acid lithium reclaimed materials is used in this method, then lye and iron salt solutions are added thereto, slurry filters pressing and soluble lithium salt and phosphoric acid molysite slag is can be obtained into phosphoric acid molysite slag countercurrent washing after separation of solid and liquid, this method industrial Applicability is strong, process is at low cost, is suitble to industrially promote and apply.
Description
Technical field
The present invention relates to the methods for separating from Resource recovery and extracting valuable material, and in particular to a kind of efficient process phosphorus
The method of sour lithium reclaimed materials belongs to resource circulation utilization field.
Background technique
Lithium is to be currently known most light, the smallest silvery white alkali metal of radius, because there are many distinctive excellent for lithium and its compound
Benign energy, they are widely used in battery, glass, ceramics, lubrication, electronics, metallurgy, medicine, refrigeration, aerospace, nuclear industry
And the fields such as photoelectricity.Surging with clean energy resource demand, deep effect human lives are referred to as " 21 century by the lithium energy
Energy upstart ".But lithium resource total amount is being reduced year by year, how rationally fully to be made good use of existing lithium resource, is promoted new energy
The healthy and stable development of source industry is the problem of meriting attention.
Since lithium is very widely used, in the leaching of lithium and the production of lithium compound, a large amount of low concentration is had
Mother liquor containing lithium cannot make full use of, in order to improve the recovery utilization rate of lithium resource, many enterprises can in conjunction with own actual situation with
And the characteristic of lithium compound is added phosphoric acid or phosphate, generates the lesser lithium phosphate (Ksp=of solubility product by adjusting pH
3.2×10-9, 25 DEG C) and it precipitates to recycle lithium.
Lithium phosphate is used as catalyst mainly for the production of color phosphor, special glass, optical disk materials etc., color for production
Color fluorescent powder is used.Since the application range of lithium phosphate is smaller, production Fluorescence Grade lithium phosphate process is more complex, therefore returns to lithium phosphate
Transition processing, the comprehensive utilization of rewinding seem that very it is necessary to develop and use lithium phosphate reclaimed materials, will generate significant society's effect
Beneficial and considerable economic benefit.
Iron phosphate compound is widely used, and be can be used for traditional agricultural, glass-ceramic, steel, surface passivation and ion and is handed over
In terms of change etc. and emerging catalyst and electrode material of lithium battery.Alternatively property catalyst, it can be by isopropyl acid oxygen
Fluidized dehydrogenation obtains methacrylic acid, and the latter is the raw material for synthesizing various polymer；(less than 500 under mild reaction temperature
DEG C), ferric phosphate can by methane selectively be oxidized to methanol or formaldehyde.Ferric iron source ferric phosphate and LiFePO4 structure are very
It is similar, thus become a kind of important presoma for preparing LiFePO4, with ferric phosphate synthesizing iron lithium phosphate, this method technique letter
It is single, without additionally incorporating phosphorus source, advantageously reduce cost.
LiFePO4 is a kind of new type lithium ion battery electrode material.The LiFePO of orthogonal olivine structural4Positive electrode
It has been increasingly becoming research hotspot new both at home and abroad.Studies have shown that the novel anode material has concentrated LiCoO2、LiNiO2、
LiMn2O4And its respective advantage of derivative positive electrode: noble element is free of, raw material is cheap, resource extreme enrichment；Work electricity
Press moderate (3.4V)；Platform identity is good, and voltage pole is steady (can match in excellence or beauty with regulated power supply)；Theoretical capacity is big (170mAh/g)；Knot
Structure is stablized, and security performance is splendid (O and P are firmly combined with strong covalent bond, and material is made to be difficult to analyse oxygen solution)；High-temperature behavior and heat are steady
It is qualitative to be substantially better than known other positive electrodes；Good cycle；Volume-diminished when charging, when cooperating with carbon negative pole material
Bulk effect is good；With most of electrolyte system good compatibilities, storge quality is good；It is nontoxic, it is real green material.With
LiCoO2、LiNiO2、LiMn2O4And its derivative positive electrode is compared, LiFePO4Positive electrode is in cost, high-temperature behavior, safety
Property aspect have advantage outstanding, it is expected to as middle large capacity, the positive electrode of middle high power lithium ion cell first choice.
Patent of invention (ZL 201510374978.9) discloses a kind of recycling battery-level lithium carbonate sinker mother liquor and prepares lithium salts
Method, which carries out mentioning lithium using phosphoric acid to lithium carbonate sinker mother liquor, obtains lithium phosphate, then pass through inorganic acid solution phosphoric acid
After lithium, calcium salt and liquid alkaline is added, so that phosphate radical is precipitated as calcium phosphate, lithium, which is dissolved into solution, recycles lithium.The work
It has brought a large amount of calcium ion in the lithium salt solution that skill obtains into, will affect subsequent processing；8~10, liquid alkaline consumes for terminal pH control
Amount is excessive, and processing cost is higher, while at the pH, has part lithium phosphate and precipitates again, so that treatment effect reduces.
Summary of the invention
It is an object of the invention to the technical deficiencies of the processing for existing lithium phosphate reclaimed materials, provide a kind of processing step
Be simple and efficient, processing cost is cheap, be suitble to industrialized production efficient process lithium phosphate reclaimed materials method, use in this method
Then lye and iron salt solutions are added in inorganic acid solution dissolving phosphoric acid lithium reclaimed materials thereto, slurry filters pressing is simultaneously after separation of solid and liquid
Soluble lithium salt is can be obtained into phosphoric acid molysite slag countercurrent washing, this method industrial Applicability is strong, and process is at low cost, is suitble to
Industrially promote and apply.
The method of efficient process lithium phosphate reclaimed materials of the present invention can be realized:
(1) lithium phosphate is transformed into soluble lithium salt and phosphoric acid molysite, short flow high efficiency extracts valuable element, improves resource
Comprehensive utilization ratio；
(2) soluble lithium salt obtained is high containing lithium concentration, and the impurity element brought into is few, can be used for the life of lithium-containing compound
It produces；Phosphoric acid molysite can be used for producing Olivine-type Cathode Material in Li-ion Batteries LiFePO4, can sell or use by oneself outside；
(3) the extraction lithium of high-recovery, total system close water, and no discharge is environmentally friendly；
(4) the common easy purchase of supplementary material, the workshop sections such as no heating, freezing, evaporation and concentration, low cost, low energy consumption.
The present invention, which adopts the following technical scheme that, realizes above-mentioned technical purpose:
A kind of method of efficient process lithium phosphate reclaimed materials, obtains soluble lithium salt and phosphoric acid molysite slag comprising following
Step:
1) weighing matches liquid: weighing quantitative lithium phosphate reclaimed materials；Weigh the trivalent with reaction equivalents such as lithium phosphate reclaimed materials
Pure water or washing water are added into trivalent iron salt for molysite, and stirring evenly is completely dissolved molysite；It is prepared using pure water or washing water
Inorganic acid solution；
2) feed intake transition: lithium phosphate reclaimed materials being added into inorganic acid solution, is stirred to react 15~60min, makes lithium phosphate
Soluble lithium salt is dissolved and be transformed into, the solution that makes the transition that feeds intake is obtained, wherein the usage amount of inorganic acid solution is to keep lithium phosphate complete
The amount of dissolution；
3) it reaction precipitating: makes the transition in solution to feeding intake while lye and ferric salt solution, control reaction process pH is added
It is 1.5~2.0, is stirred to react 60~180min, reaction continues stirring 120~240min of ageing, obtains reaction paste after ends；
4) be separated by solid-liquid separation: by reaction paste filters pressing, by phosphoric acid molysite slag countercurrent washing 2~4 times, obtain soluble lithium salt and
Phosphoric acid molysite wet slag after washing is used for ingredient in washing water return step 1.
Preferably, trivalent iron salt described in the method for efficient process lithium phosphate reclaimed materials of the present invention is technical grade FeCl3、
Technical grade Fe (NO3)3One of or it is a variety of.
Preferably, inorganic acid described in the method for efficient process lithium phosphate reclaimed materials of the present invention is technical grade HCl, industry
Grade HNO3One of or it is a variety of.
It preferably, is technical grade liquid alkaline NaOH solution or technical grade in the method for efficient process lithium phosphate reclaimed materials of the present invention
One or both of liquefied ammonia (ammonium hydroxide).
As a kind of embodiment preferred for this invention, in the method for efficient process lithium phosphate reclaimed materials of the present invention
The trivalent iron salt preferentially uses technical grade FeCl3, inorganic acid preferentially uses technical grade HCl, and lye preferentially uses technical grade
Liquid alkaline NaOH solution.
The chemical equation of step 2 of the present invention is as follows:
Li3PO4(s)+2H+(l)→LiH2PO4(l)+2Li+(l)
The chemical equation of step 3 of the present invention is as follows:
LiH2PO4(l)+Fe3+(l)+2NaOH(l)→FePO4(s)+Li+(l)+2Na+(l)+2H2O
The present invention has the following advantages that and good effect:
(1) transition of the trivalent iron salt being added in the method for efficient process lithium phosphate reclaimed materials of the present invention to phosphate radical
Effect is good, can effectively improve the rate of recovery of lithium and reduce the content of impurity element phosphorus in soluble lithium salt solution；
(2) inorganic acid being added in the method for efficient process lithium phosphate reclaimed materials of the present invention is inorganic acid, to phosphorus
The solute effect of sour lithium is good, and it is good that dosage lacks effect, so that the rate of recovery of lithium is higher in the present invention；
(3) the phosphoric acid molysite that the present invention obtains can be used for producing Olivine-type Cathode Material in Li-ion Batteries LiFePO4, will
It is directly significant to reduce production cost；
(4) present invention can obtain the higher soluble lithium salt containing lithium concentration, and it is few to bring impurity element into, can be used for producing containing lithium
Compound has biggish flexibility to the extraction process selection of lithium, can require according to different lithium compounds and subsequent technique,
Select different trivalent iron salt and corresponding inorganic acid；
(5) washing water of the present invention, which returns, matches lysate, forms closed circulation, improves the same of resource recycling rate
When accomplished without discharge, it is non-hazardous to environment；
(6) present invention reduces production energy consumption and production cost without workshop sections such as freezing, evaporation and concentration, and simple process is high
Effect is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is the process flow chart of the method for efficient process lithium phosphate reclaimed materials of the present invention.
Specific embodiment
The present invention is further detailed combined with specific embodiments below, illustrated embodiment is served only for explaining this hair
It is bright, it is not intended to limit the scope of the present invention.
The embodiment of the present invention 1, embodiment 2, embodiment 3, lithium phosphate reclaimed materials wet slag is aqueous used in embodiment 4 is divided into
53.4%, butt contains Li2O is 33.17%, and butt is 22.92% containing P, and butt is 5.95% containing Na.5 institute of the embodiment of the present invention
Lithium phosphate reclaimed materials wet slag is aqueous to be divided into 32.0%, and butt contains Li2O is 33.17%, and butt is 22.92% containing P, butt
It is 5.95% containing Na.
A kind of method of the efficient process lithium phosphate reclaimed materials of embodiment 1
1) weighing matches liquid: weighing lithium phosphate reclaimed materials wet slag 1260Kg；Weigh 734Kg content be 96% it is anhydrous
FeCl3, and past FeCl3Middle addition pure water 800L, stirring evenly is completely dissolved molysite；Add in the HCl that 920Kg concentration is 31%
Enter 760L pure water, is configured to acid solution；
2) feed intake transition: the lithium phosphate wet slag 1260Kg weighed up being added into acid solution, is stirred to react 15min, makes lithium phosphate
Soluble lithium salt is dissolved and be transformed into, the solution that makes the transition that feeds intake is obtained, wherein the usage amount of inorganic acid solution is to keep lithium phosphate complete
The amount of dissolution；
3) reaction precipitating: the NaOH solution 1190Kg of concentration 31% is stirred while be added in solution and is prepared to feeding intake to make the transition
Iron salt solutions, control reaction process pH is 2.0 or so, is stirred to react 60min, and reaction continues stirring ageing after ending
120min；
4) it is separated by solid-liquid separation: the slurry filters pressing that step 3) is obtained, then by phosphoric acid molysite slag countercurrent washing 3 times, obtain solvable
Property lithium salt solution 3030L and three wash rear phosphoric acid molysite wet slag 1482Kg, washing water return step 1) in for ingredient use.
A kind of method of the efficient process lithium phosphate reclaimed materials of embodiment 2
1) weighing matches liquid: weighing lithium phosphate reclaimed materials wet slag 1260Kg；Weigh 734Kg content be 96% it is anhydrous
FeCl3, and past FeCl3Middle addition pure water 800L, stirring evenly is completely dissolved molysite；Add in the HCl that 970Kg concentration is 31%
Enter 200L pure water, is configured to acid solution；
2) feed intake transition: the lithium phosphate wet slag 1260Kg weighed up being added into acid solution, is stirred to react 30min, makes lithium phosphate
It dissolves and is transformed into soluble lithium salt；The solution that makes the transition that feeds intake is obtained, wherein the usage amount of inorganic acid solution is to keep lithium phosphate complete
The amount of dissolution；
3) it reaction precipitating: makes the transition in solution to feeding intake while the NaOH solution 1250Kg of concentration 31% and prepared is added
Iron salt solutions, control reaction process pH are 1.5 or so, are stirred to react 120min, and reaction continues stirring ageing 180min after ending；
F, it is separated by solid-liquid separation: the slurry filters pressing that step 3) is obtained, then by phosphoric acid molysite slag countercurrent washing 3 times, obtain solvable
Property lithium salt solution 2540L and three wash rear phosphoric acid molysite wet slag 1478Kg, washing water return step 1) in for ingredient use.
A kind of method of the efficient process lithium phosphate reclaimed materials of embodiment 3
1) weighing matches liquid: weighing lithium phosphate reclaimed materials wet slag 1260Kg；Weigh 734Kg content be 96% it is anhydrous
FeCl3, and past FeCl3Middle addition pure water 800L, stirring evenly is completely dissolved molysite；In the HCl that 1020Kg concentration is 31% not
Pure water is added；
2) feed intake transition: the lithium phosphate wet slag 1260Kg weighed up being added into acid solution, is stirred to react 60min, makes lithium phosphate
Soluble lithium salt is dissolved and be transformed into, the solution that makes the transition that feeds intake is obtained, wherein the usage amount of inorganic acid solution is to keep lithium phosphate complete
The amount of dissolution；
3) it reaction precipitating: makes the transition in solution to feeding intake while the NaOH solution 1310Kg of concentration 31% and prepared is added
Iron salt solutions, control reaction process pH are 1.7 or so, are stirred to react 180min, and reaction continues stirring ageing 240min after ending；
4) it is separated by solid-liquid separation: the slurry filters pressing that step 3) is obtained, then by phosphoric acid molysite slag countercurrent washing 3 times, obtain solvable
Property lithium salt solution 2460L and three wash rear phosphoric acid molysite wet slag 1470Kg, washing water return step 1) in for ingredient use.
A kind of method of the efficient process lithium phosphate reclaimed materials of embodiment 4
1) weighing matches liquid: weighing lithium phosphate reclaimed materials wet slag 1260Kg；Weigh the Fe that 1790Kg content is 98%
(NO3)3·9H2O, and pure water 800L is added, stirring evenly is completely dissolved molysite；The HNO that 780Kg concentration is 65%3In not plus
Enter pure water；
2) feed intake transition: the lithium phosphate wet slag 1260Kg weighed up being added into acid solution, is stirred to react 60min, makes lithium phosphate
It dissolves and is transformed into soluble lithium salt；The solution that makes the transition that feeds intake is obtained, wherein the usage amount of inorganic acid solution is to keep lithium phosphate complete
The amount of dissolution；
3) it reaction precipitating: makes the transition in solution to feeding intake while the NaOH solution 1250Kg of concentration 31% and prepared is added
Iron salt solutions, control reaction process pH are 2.0 or so, are stirred to react 180min, and reaction continues stirring ageing 240min after ending；
4) it is separated by solid-liquid separation: the slurry filters pressing that step 3) is obtained, then by phosphoric acid molysite slag countercurrent washing 3 times, obtain solvable
Property lithium salt solution 2710L and three wash rear phosphoric acid molysite wet slag 1488Kg, washing water return step 1) in for ingredient use.
A kind of method of the efficient process lithium phosphate reclaimed materials of embodiment 5
1) liquid is matched in weighing: weighing lithium phosphate reclaimed materials wet slag 864Kg, (this case column lithium phosphate reclaimed materials wet slag used contains
Moisture is 32.0%, and butt contains Li2O is 33.17%, and butt is 22.92% containing P, 5.95%) butt is containing Na.Weigh 734Kg
The anhydrous FeCl that content is 96%3, and past FeCl3Middle addition pure water 800L, stirring evenly is completely dissolved molysite；1020Kg is dense
Pure water is not added in the HCl that degree is 31%；
2) feed intake transition: the lithium phosphate wet slag 864Kg weighed up being added into acid solution, is stirred to react 60min, keeps lithium phosphate molten
It solves and is transformed into soluble lithium salt；The solution that makes the transition that feeds intake is obtained, wherein the usage amount of inorganic acid solution is to keep lithium phosphate completely molten
The amount of solution；
3) reaction precipitating: to feed intake make the transition in solution with 180min and meanwhile be added the NaOH solution 1280Kg of concentration 31% with
Prepared iron salt solutions, control reaction process pH are 2.0 or so, and reaction continues stirring ageing 240min after ending；
4) it is separated by solid-liquid separation: the slurry filters pressing that step 3) is obtained, then by phosphoric acid molysite slag countercurrent washing 3 times, obtain solvable
Property lithium salt solution 2020L and three wash rear phosphoric acid molysite wet slag 1475Kg, washing water return step 1) in for ingredient use.
The quality condition for the lithium salt solution that above-described embodiment obtains is as shown in table 1:
Table 1: the recovery process and effect of the method for efficient process lithium phosphate reclaimed materials of the present invention
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Any modification, equivalent replacement, improvement and so within principle, should all be included in the protection scope of the present invention.
Claims (1)
1. a kind of method of efficient process lithium phosphate reclaimed materials, obtains soluble lithium salt and phosphoric acid molysite slag, which is characterized in that packet
Include following steps:
1) weighing matches liquid: weighing quantitative lithium phosphate reclaimed materials；Weigh the ferric iron with reaction equivalents such as lithium phosphate reclaimed materials
Pure water or washing water are added into trivalent iron salt for salt, and stirring evenly is completely dissolved molysite；Nothing is prepared using pure water or washing water
Machine acid solution；
2) feed intake transition: lithium phosphate reclaimed materials being added into inorganic acid solution, is stirred to react 15~60min, dissolves lithium phosphate
And it is transformed into soluble lithium salt, the solution that makes the transition that feeds intake is obtained, wherein the usage amount of inorganic acid solution is to be completely dissolved lithium phosphate
Amount；
3) it reaction precipitating: makes the transition in solution to feeding intake while lye and ferric salt solution is added, control reaction process pH is 1.5
~2.0, it is stirred to react 60~180min, reaction continues stirring 120~240min of ageing, obtains reaction paste after ending；
4) it is separated by solid-liquid separation: reaction paste filters pressing is obtained into soluble lithium salt and washing for phosphoric acid molysite slag countercurrent washing 2~4 times
Phosphoric acid molysite wet slag afterwards, washing water return step 1) in for ingredient use；
Wherein the trivalent iron salt uses technical grade FeCl3, using technical grade HCl, the lye uses the inorganic acid
Technical grade liquid alkaline NaOH solution.
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| CN108394919A (en) * | 2018-02-02 | 2018-08-14 | 东北石油大学 | Application of the complexing of metal ion agent in waste lithium iron phosphate battery removal process |
| CN109896510A (en) * | 2019-03-13 | 2019-06-18 | 乳源东阳光磁性材料有限公司 | Method for washing iron phosphate |
| CN109809382B (en) * | 2019-03-28 | 2020-12-11 | 衢州华友钴新材料有限公司 | Method for synthesizing iron phosphate by using waste phosphate generated by precipitating trace heavy metals |
| CN110342483B (en) * | 2019-06-04 | 2020-11-03 | 湖南雅城新材料有限公司 | Method for preparing battery-grade iron phosphate by using lithium phosphate waste |
| CN110624933B (en) * | 2019-09-24 | 2021-05-07 | 中国恩菲工程技术有限公司 | Method for washing and removing ammonia from metallurgical waste residues |
| CN112320781A (en) * | 2020-11-23 | 2021-02-05 | 湖南金源新材料股份有限公司 | Method for regenerating iron phosphate by lithium extraction residues of lithium iron phosphate waste |
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