CN110451551A - The method that purification hydro-thermal method production LiFePO4 waste water prepares nano barium sulfate simultaneously - Google Patents
The method that purification hydro-thermal method production LiFePO4 waste water prepares nano barium sulfate simultaneously Download PDFInfo
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- CN110451551A CN110451551A CN201910851261.7A CN201910851261A CN110451551A CN 110451551 A CN110451551 A CN 110451551A CN 201910851261 A CN201910851261 A CN 201910851261A CN 110451551 A CN110451551 A CN 110451551A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/462—Sulfates of Sr or Ba
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Inorganic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The present invention relates to a kind of methods that purification hydro-thermal method production LiFePO4 waste water prepares nano barium sulfate simultaneously, it is reacted under the action of catalyst with the lithium sulfate waste water generated in hydro-thermal method LiFePO4 production process using cheap high-pruity barium carbonate, nanoprecipitation barium sulfate and the technique of hydro-thermal method LiFePO4 wastewater treatment are combined together, sulfate radical while producing nano barium sulfate in purification removal hydro-thermal method production LiFePO4 waste water, production technology of the present invention more optimizes, and the cost of production reduces, wastewater discharge is reduced, overall investment is less.
Description
Technical field
The present invention relates to LiFePO4 waste water treatment and reclamations, same more particularly, to purification hydro-thermal method production LiFePO4 waste water
When prepare nano barium sulfate method.
Background technique
LiFePO4 is to have now been found that safest cell positive material, and hydro-thermal method produces LiFePO4 and uses certain proportion
The one step hydrothermal synthesis of raw materials high temperature and pressure such as high-purity ferrous sulfate, lithium hydroxide, phosphoric acid, after being filtered, washed, dry, crushing
Obtain LiFePO4.Contain a large amount of lithium sulfate in the filtrate that hydro-thermal method production process generates, sulfuric acid lithium content reaches 30%.Water
The LiFePO4 of thermal method production has the advantages that low temperature resistant, Gao Fang electricity, circulation discharge time is more, production energy consumption is low etc..But hydro-thermal
Method is unique compared to traditional solid phase method the disadvantage is that sulfur acid lithium wastewater flow rate is big, and the solubility of lithium ion in water is excessive.
Recovery Purifying is realized in order to take out the sulfate radical in sulfur acid lithium waste water, and traditional purification method is usually used eight
Water barium hydroxide is made a return journey sulfate radical using blanc fixe, but there are barium hydroxide production barium sulfate reaction process slowly and
React incomplete problem.Secondly LiFePO4 per ton needs 3 tons of barium hydroxides to handle, high-purity barium hydroxide valence
Lattice are per ton up to 8000 yuan, and the barium sulfate granularity of generation can only be handled greatly as low-grade barium sulfate even waste residue very much.
Nanoprecipitation barium sulfate (BaSO4) is a kind of widely used industrial chemicals, can be used for plastics, coating, ink etc.
In, while part titanium white powder pigment can be replaced.The traditional handicraft of blanc fixe is that high-pruity barium carbonate and sulfuric acid are made in catalyst
It is made with after lower reaction by washing-drying-disintegrating process.Its added value is low, high production cost, and high-concentration sulfuric acid is direct
It is larger to participate in reactivity hazard.
Summary of the invention
It is an object of the invention to overcome the deficiency of the above-mentioned prior art, a kind of purification hydro-thermal method production LiFePO4 is provided
The method that waste water prepares nano barium sulfate simultaneously, the present invention is by nanoprecipitation barium sulfate and hydro-thermal method LiFePO4 wastewater treatment
Technique is combined together, sulfate radical while producing nano barium sulfate in purification removal hydro-thermal method production LiFePO4 waste water,
Production technology more optimizes, and the cost of production reduces, wastewater discharge is reduced, overall investment is less.
The purpose of the present invention is achieved by the following technical programs:
A method of purification hydro-thermal method production LiFePO4 waste water prepares nano barium sulfate simultaneously, comprising the following steps:
S1, the waste water of hydro-thermal method production LiFePO4 is settled, takes supernatant；
S2, it takes the part supernatant in step S1 as solution A, excessive barium carbonate is added in solution A, sufficiently after reaction
The barium sulfate generated is filtered off with the sieve sieving below of 400 mesh, obtains the suspension C containing barium carbonate；The barium carbonate of addition is
High-pruity barium carbonate, partial size should can be by the sieves of 400 mesh, therefore using can obtain after 400 mesh the screen to filtrate below
Suspension containing barium carbonate；
S3, it takes the part supernatant in step S1 as solution B, catalyst is added in solution B, the catalyst is salt
One of acid or nitric acid, obtain solution D；
S4, suspension C are added in solution D, are sufficiently reacted, and the solution E containing precipitating is obtained；
S5, solution E is filtered, obtains filtrate F and filter residue G.The filtrate F of acquisition is high-purity after removing sulfate radical
The lithium ion solution of degree, filter residue G are nanoprecipitation barium sulfate.
Further, the molal quantity for the barium carbonate being added in step S2 is greater than the overall sulfate radical of both solution A and solution B
Molal quantity.It enables the molal quantity of barium carbonate be greater than the molal quantity of the overall sulfate radical of both solution A and solution B, can guarantee have with this
Enough barium ions are in conjunction with sulfate radical, to remove the sulfate radical in solution A and solution B.
Further, the molal quantity for the barium carbonate being added in step S2: both solution A and solution B totality sulfate radical rub
That number=1:(0.5~0.95).
Further, in step S4, solution D is slowly added to suspension C under high-speed stirred state, until the pH of solution E
Stop that suspension C is added when value is 1-1.5.Be slowly added to the suspension C containing barium carbonate, can make be added after solution D with
Suspension C is uniformly mixed, and by between the pH value control of mixed solution E again 1-1.5, can be guaranteed at lower ph,
The dissolved carbonate of barium carbonate is in conjunction with hydrogen ion, and production carbon dioxide volatilizes, to remove carbanion.
Further, it after stopping to suspension C is added in solution D, is stirred to react 20 minutes or more.
Further, after step s4, detection, specific detection method are as follows: from solution E are sampled to solution E
It samples and is filtered, sulfuric acid is added dropwise into obtained filtrate, has seen whether precipitating.Detection is sampled to solution E, it can
It detects whether there is excessive barium ions in solution E, judges whether to need further operating removal is new to introduce according to testing result
Barium ions impurity, to guarantee the purity of lithium ion solution finally obtained.
Further, after being sampled detection, if testing result is to have sediment generation, to molten made from step S4
Supernatant obtained in step S1 is added in liquid E, after addition and repeats sampling Detection operation, until in testing result without precipitating
Occur, and the pH value range of solution E carries out step S5 between 1-1.5 again later；If having precipitating after sulfuric acid is added dropwise in sampling
Occur, then prove that there are excessive barium ions in solution E, continuously add supernatant according to judging result in solution E, with removal
Whole barium ions in solution E；
After being sampled detection, if testing result deposit-free generates, step S5 is carried out.
Further, after obtaining filter residue G in step s 5, filter residue G is washed, dried, is crushed, nanoprecipitation is obtained
Barium sulfate.
Further, after step S3 obtained solution D, solution D is added in high speed shear reaction kettle, in high speed shear
Step S4 is carried out in reaction kettle.
The invention has the following beneficial effects: the present invention provides a kind of purification hydro-thermal methods to produce LiFePO4 waste water simultaneously
The method for preparing nano barium sulfate was produced with hydro-thermal method LiFePO4 under the action of catalyst using cheap high-pruity barium carbonate
The lithium sulfate waste water generated in journey is reacted, by the technique knot of nanoprecipitation barium sulfate and hydro-thermal method LiFePO4 wastewater treatment
It is combined, sulfate radical while producing nano barium sulfate in purification removal hydro-thermal method production LiFePO4 waste water, the present invention
Production technology more optimizes, and the cost of production reduces, wastewater discharge is reduced, overall investment is less.
Specific embodiment
Below with reference to the embodiment provided, invention is further described in detail.
Embodiment 1
1000ml factory hydro-thermal method production LiFePO4 waste water containing lithium ion (waste water itself is in acid) is taken, wherein lithium is detected
Ion concentration 18%, sulfate concentration 24%.Solution is divided into 200ml solution A and 800ml solution B.
131.4g barium carbonate is weighed in solution A, is sufficiently sieved to obtain suspension C after reaction by 400 mesh screens.
2ml hydrochloric acid is added in solution B, after being stirred 15 minutes, slowly suspension C is added, obtains solution E.
The pH value for measuring solution E when measuring pH value is 1 stops that suspension C is added.
Sampling filtering, discovery is without precipitating after sulfuric acid is added dropwise in filtrate.
Solution E is filtered.Filter residue is finished product nanoprecipitation barium sulfate after repeatedly washing, dry, crushing.Meanwhile obtaining
Filtrate is high purity lithium solion.
Through examining, nanoprecipitation barium sulfate detection granularity made above is 200nm, and dry powder whiteness is up to 99.2, BaSO4Contain
It measures up to 98.8%.After purification the lithium ion content of the waste water containing lithium ion up to 17.4%, sulfate radical content 0.13%, without barium ions,
Reach hydro-thermal method production LiFePO4 reuse standard.
Embodiment 2
2500ml factory hydro-thermal method production LiFePO4 waste water containing lithium ion (waste water itself is in acid) is taken, wherein lithium is detected
Ion concentration 15%, sulfate concentration 26%.Solution is divided into 500ml solution A and 2000ml solution B.
350g barium carbonate is weighed in solution A, is sufficiently sieved to obtain suspension C after reaction by 400 mesh screens.
10ml hydrochloric acid is added in solution B, after being stirred 15 minutes, slowly suspension C is added, obtains solution E.
The pH value for measuring solution E when measuring pH value is 1.5 stops that suspension C is added.
Sampling filtering, discovery is without precipitating after sulfuric acid is added dropwise in filtrate.
Solution E is filtered.Filter residue is finished product nanoprecipitation barium sulfate after repeatedly washing, dry, crushing.Meanwhile obtaining
Filtrate is high purity lithium solion.
Through examining, nanoprecipitation barium sulfate detection granularity made above is 220nm, and dry powder whiteness is up to 98.5, BaSO4Contain
It measures up to 98.9%.After purification the lithium ion content of the waste water containing lithium ion up to 14.2%, sulfate radical content 0.21%, without barium ions,
Reach hydro-thermal method production LiFePO4 reuse standard.
As described above, only presently preferred embodiments of the present invention, when cannot be limited the scope of implementation of the present invention with this,
All still belong to this hair according to simple equivalent changes and modifications made by scope of the present invention patent and invention description content generally
In the range of bright patent covers.
Claims (9)
1. a kind of method that purification hydro-thermal method production LiFePO4 waste water prepares nano barium sulfate simultaneously, which is characterized in that including
Following steps:
S1, the waste water of hydro-thermal method production LiFePO4 is settled, takes supernatant；
S2, it takes the part supernatant in step S1 as solution A, excessive barium carbonate is added in solution A, is sufficiently used after reaction
The sieve sieving below of 400 mesh filters off the barium sulfate generated, obtains the suspension C containing barium carbonate；
S3, take part supernatant in step S1 as solution B, be added catalyst in solution B, the catalyst be hydrochloric acid or
One of nitric acid obtains solution D；
S4, suspension C are added in solution D, are sufficiently reacted, and the solution E containing precipitating is obtained；
S5, solution E is filtered, obtains filtrate F and filter residue G.
2. the side that a kind of purification hydro-thermal method production LiFePO4 waste water as described in claim 1 prepares nano barium sulfate simultaneously
Method, which is characterized in that
The molal quantity for the barium carbonate being added in step S2 is greater than the molal quantity of the overall sulfate radical of both solution A and solution B.
3. the side that a kind of purification hydro-thermal method production LiFePO4 waste water as claimed in claim 2 prepares nano barium sulfate simultaneously
Method, which is characterized in that
The molal quantity for the barium carbonate being added in step S2: molal quantity=1:(0.5 of both solution A and solution B totality sulfate radical~
0.95)。
4. the side that a kind of purification hydro-thermal method production LiFePO4 waste water as claimed in claim 2 prepares nano barium sulfate simultaneously
Method, which is characterized in that
In step S4, solution D is slowly added to suspension C under high-speed stirred state, until the pH value of solution E is stopped when being 1-1.5
Suspension C is only added.
5. the side that a kind of purification hydro-thermal method production LiFePO4 waste water as claimed in claim 4 prepares nano barium sulfate simultaneously
Method, which is characterized in that
After stopping to suspension C is added in solution D, it is stirred to react 20 minutes or more.
6. the side that a kind of purification hydro-thermal method production LiFePO4 waste water as claimed in claim 4 prepares nano barium sulfate simultaneously
Method, which is characterized in that
After step s4, detection, specific detection method are sampled to solution E are as follows: sample and carried out from solution E
Filter, is added dropwise sulfuric acid into obtained filtrate, has seen whether precipitating.
7. the side that a kind of purification hydro-thermal method production LiFePO4 waste water as claimed in claim 6 prepares nano barium sulfate simultaneously
Method, which is characterized in that
After being sampled detection, if testing result is to have sediment generation, step is added into solution E made from step S4
Obtained supernatant in S1 after addition and repeats sampling Detection operation, until occurring in testing result without precipitating, and solution E
PH value range between 1-1.5, carry out step S5 again later；
After being sampled detection, if testing result deposit-free generates, step S5 is carried out.
8. the side that a kind of purification hydro-thermal method production LiFePO4 waste water as described in claim 1 prepares nano barium sulfate simultaneously
Method, which is characterized in that
After obtaining filter residue G in step s 5, filter residue G is washed, dried, is crushed, nanoprecipitation barium sulfate is obtained.
9. the side that a kind of purification hydro-thermal method production LiFePO4 waste water as described in claim 1 prepares nano barium sulfate simultaneously
Method, which is characterized in that
After step S3 obtained solution D, solution D is added in high speed shear reaction kettle, is carried out in high speed shear reaction kettle
Step S4.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910851261.7A CN110451551A (en) | 2019-09-10 | 2019-09-10 | The method that purification hydro-thermal method production LiFePO4 waste water prepares nano barium sulfate simultaneously |
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| CN201910851261.7A CN110451551A (en) | 2019-09-10 | 2019-09-10 | The method that purification hydro-thermal method production LiFePO4 waste water prepares nano barium sulfate simultaneously |
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