CN110921899B - Lithium hexafluorophosphate and low-fluorine lithium phosphate compound wastewater treatment process and device - Google Patents
Lithium hexafluorophosphate and low-fluorine lithium phosphate compound wastewater treatment process and device Download PDFInfo
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- CN110921899B CN110921899B CN201911238430.6A CN201911238430A CN110921899B CN 110921899 B CN110921899 B CN 110921899B CN 201911238430 A CN201911238430 A CN 201911238430A CN 110921899 B CN110921899 B CN 110921899B
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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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
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
Abstract
The invention relates to a process for treating waste water containing lithium hexafluorophosphate and lithium difluorophosphate compounds, which comprises the following steps: s1, sequentially adding alkali and calcium-containing compounds into the wastewater, and filtering the precipitate; s2, adding acid and a catalytic substance into the wastewater; s3, adding alkali into the wastewater, and heating the wastewater; s4, adding a phosphorus removing agent into the wastewater. Still relate to a lithium hexafluorophosphate and low lithium fluorophosphate compound effluent treatment plant, it includes that the upper and lower reaches set up: the alkali analysis component comprises an alkali reaction tank I and a sedimentation tank I; the catalytic hydrolysis component comprises an acid reaction tank and a catalytic material arranged in the acid reaction tank; the alkaline hydrolysis component comprises an alkaline reaction tank II and a sedimentation tank II; the dephosphorization assembly comprises a dephosphorization tank and a sedimentation tank III. Can meet the requirement of removing total phosphorus in the waste water of the lithium hexafluorophosphate and the lithium low fluorophosphate compounds.
Description
Technical Field
The invention relates to a process for treating wastewater containing lithium hexafluorophosphate and lithium low-fluoride phosphate compounds, and also relates to a device for treating wastewater containing lithium hexafluorophosphate and lithium low-fluoride phosphate compounds.
Background
Along with the rise of intelligent mobile equipment, the application market of lithium batteries is huge, brings huge production capacity demand of lithium batteries, as the most important conductive medium in the lithium battery industry, the application of lithium hexafluorophosphate in the lithium battery industry is very common, but a large amount of sewage can be produced in the production process of lithium hexafluorophosphate, and the wastewater belongs to the wastewater which is difficult to degrade and is difficult to treat and is a bottleneck which restricts the environmental protection problem of the industry all the time. The lithium hexafluorophosphate production wastewater has the characteristics of high concentration, complex components, strong pungent smell, large pollution and high treatment difficulty, and the treatment of the wastewater by some lithium hexafluorophosphate production enterprises at present always has the problems of substandard and unstable treatment, so the problem is also an environmental protection industrial problem to be solved urgently.
The TP (total phosphorus) of lithium hexafluorophosphate wastewater of a common lithium hexafluorophosphate enterprise is approximately 300-500ppm, and the COD is within 500ppm, but TP and F ions in the wastewater are the main treatment targets, but the general physical and chemical treatment method is difficult to realize the complete removal of TP and F-, so that the wastewater treatment does not reach the standard, and the adverse effect is brought to the enterprise production.
Disclosure of Invention
The invention aims to provide a process for treating lithium hexafluorophosphate and lithium low-fluoride phosphate compound wastewater, which can meet the requirement of removing total phosphorus in lithium hexafluorophosphate and lithium low-fluoride phosphate compound wastewater.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a process for treating waste water containing lithium hexafluorophosphate and lithium difluorophosphate compounds, which comprises the following steps:
s1, sequentially adding alkali, a calcium-containing compound and a flocculating agent into the wastewater, and separating precipitates;
s2, adding acid into the wastewater, and enabling the wastewater to pass through a fixed bed catalytic filler;
s3, adding alkali into the wastewater, and heating the wastewater;
s4, adding a phosphorus removing agent and a flocculating agent into the wastewater.
Alternatively, in S1, the precipitate is filtered after the alkali is added, then the calcium-containing compound is added, and the precipitate is filtered again.
Optionally, the calcium-containing compound is quicklime or calcium chloride.
Optionally, the catalytic material is a mixture of elemental iron, elemental carbon and titanium oxide.
Optionally, in the step S3, the pH value is adjusted to 9.5-10, the wastewater is heated to 50-70 ℃, and the reaction time is 5-7 hours.
Optionally, in the step S2, the pH is adjusted to 2-3, and the wastewater is heated to 60-70 ℃.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
in the process for treating waste water containing lithium hexafluorophosphate and lithium difluorophosphate compounds of the present invention, in S1, the waste water is charged with alkali to remove lithium as a precipitate by filtration, and the waste water is charged with a calcium-containing compound to remove fluorine ions as a precipitate by filtration, so that lithium hexafluorophosphate in the waste water is partially hydrolyzed into lithium difluorophosphate (for example, lithium trifluorophosphate, lithium difluorophosphate, lithium monofluorophosphate); subsequently, the wastewater is adjusted to be acidic in S2, and the lithium hexafluorophosphate intermediate product is accelerated to be hydrolyzed into lithium difluorophosphate and lithium monofluorophosphate by a catalytic agent; then, under the conditions of alkalinity and heating temperature, products of catalytic hydrolysis in S2 are completely hydrolyzed in S3, and finally phosphorus is removed by phosphorus removal agent in S4. Therefore, the method can effectively treat the lithium hexafluorophosphate and the low lithium hexafluorophosphate compound wastewater, and the treatment of the lithium hexafluorophosphate wastewater can reach the first-class A standard.
The invention also provides a device for treating the wastewater containing the lithium hexafluorophosphate and the lithium difluorophosphate compounds, which comprises the following components in parts by weight:
the alkali analysis component comprises an alkali reaction tank I and a sedimentation tank I;
the catalytic hydrolysis component comprises an acid reaction tank and a catalytic material arranged in the acid reaction tank;
the alkaline hydrolysis component comprises an alkaline reaction tank II and a sedimentation tank II;
the dephosphorization assembly comprises a dephosphorization tank and a sedimentation tank III.
Optionally, the caustic analysis assembly is provided in two sets in series.
Optionally, a heating mechanism is further arranged in the catalytic hydrolysis assembly and/or the alkaline hydrolysis assembly.
Optionally, the catalytic filler is a mixture of elemental iron, elemental carbon, and titanium oxide.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the device for treating the waste water containing the lithium hexafluorophosphate and the lithium low fluorophosphate compounds, the fluorine is removed by the alkali precipitation assembly under the alkaline condition; catalyzing by a catalytic hydrolysis component under an acidic condition to accelerate the degradation of lithium hexafluorophosphate and lithium low-fluoride phosphate compounds into lithium low-fluoride phosphate compounds; further degrading the lithium-low-fluorophosphate compound by the alkaline hydrolysis module; phosphorus is removed by the phosphorus removal component, so that the lithium hexafluorophosphate and low lithium fluorophosphate compound wastewater is effectively treated.
Drawings
Some specific embodiments of the invention will be described in detail hereinafter, by way of illustration and not limitation, with reference to the accompanying drawings. The same reference numbers in the drawings identify the same or similar elements or components. Those skilled in the art will appreciate that the drawings are not necessarily drawn to scale. In the drawings:
FIG. 1 is a schematic representation of the steps of a preferred embodiment of the present invention for the treatment of lithium hexafluorophosphate and lithium difluorophosphate compound wastewater;
FIG. 2 is a schematic structural view of a preferred embodiment of a wastewater treatment apparatus for lithium hexafluorophosphate and lithium difluorophosphate compounds of the present invention;
wherein the reference numerals are as follows:
1. a caustic separation assembly;
2. a catalytic hydrolysis component;
3. an alkaline hydrolysis module;
4. a phosphorus removal component;
5. an alkaline reaction tank I;
6. a sedimentation tank I;
7. an acid reaction tank;
8. a catalytic substance;
9. an alkali reaction tank II;
10. a sedimentation tank II;
11. a phosphorus removal tank;
12. a sedimentation tank III;
13. a stirring mechanism;
14. adding a coagulant into the tank I;
15. and adding a coagulant into the pool II.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in figure 1, the process for treating the waste water containing lithium hexafluorophosphate and lithium difluorophosphate compounds comprises the following steps:
s1, sequentially adding alkali and calcium-containing compounds into the wastewater, and filtering the precipitate;
s2, adding acid and a catalytic substance into the wastewater;
s3, adding alkali into the wastewater, and heating the wastewater;
s4, adding a phosphorus removing agent into the wastewater.
In S1, the alkali to be added is sodium hydroxide, the pH of the wastewater (raw water containing lithium hexafluorophosphate) is adjusted to 9 to 10, and alkali precipitation is performed during the stirring. The added calcium-containing compound is quicklime or calcium chloride, so that F ions in the wastewater are further removed, and the precipitate is filtered out after flocculation is carried out by adding a coagulant. In this step, only one final precipitation step may be performed, for example, at low lithium hexafluorophosphate concentrations; alternatively, the alkali may be added and then precipitated, and then the quick lime may be added and then precipitated again, for example, when the lithium hexafluorophosphate concentration is high.
After the alkaline hydrolysis process of S1, most of the original lithium hexafluorophosphate in the wastewater can be degraded to become some lithium low-fluorophosphates, but this time, the TP (total phosphorus) removal is not enough, and further hydrolysis is needed.
In S2, adding hydrochloric acid (hydrogen chloride) as an acid into the wastewater, adjusting the pH of the wastewater to 2-3, controlling the temperature to be 60-70 ℃, and promoting lithium hexafluorophosphate to be hydrolyzed into lithium monofluorophosphate and lithium difluorophosphate more fully by a catalyst. The catalyst is a mixture of iron simple substance, carbon simple substance and titanium oxide, and is put into the wastewater in a filling mode to contact with the wastewater. In this step, some precipitates are generated and can be removed first, but for low-concentration lithium hexafluorophosphate, the treatment may be suspended and the precipitation in S3 may be waited for.
Through the hydrolysis reaction of the first two steps, the phosphorus removal is thoroughly carried out through further alkaline hydrolysis.
In S3, adding alkali (sodium hydroxide) into the wastewater, adjusting the pH value to 9.5-10, heating the wastewater to the reaction temperature of 50-70 ℃, and carrying out the reaction for 5-7 hours (preferably about 6 hours) to completely hydrolyze the lithium low-fluorophosphates (lithium monofluorophosphate and lithium difluorophosphate). After the reaction is finished, lime is added, and coagulant is added for flocculation and precipitation.
And S4, adding a phosphorus removal agent and a coagulant into the wastewater for flocculation, so that pollutants such as TP, F, Li and the like in the wastewater are completely removed, and the wastewater is treated to reach the standard.
Through the multistep hydrolysis process of lithium hexafluorophosphate, the complete hydrolysis of lithium hexafluorophosphate is realized, and the method has the characteristics of practicality, economy and high efficiency: (1) by removing fluorine through S1, hydrolysis can be promoted, and complex formation of subsequent products or medicaments by high-concentration lithium ions can be avoided, so that hexafluorophosphoric acid cannot be thoroughly degraded, and phosphorus and fluorine cannot be thoroughly removed; (2) by adopting the catalytic filler in S2, the hydrolysis can be accelerated, the dosage can be saved, and the wastewater treatment operation cost can be saved; (3) through S3 alkaline hydrolysis and control of reaction temperature, the complete hydrolysis of the hexafluorophosphoric acid can be realized, so that the treatment of the hexafluorophosphoric acid wastewater becomes practical; (4) by reasonably adding the final phosphorus removal agent S4, the TP of the final effluent can be 1ppm, and the TP of the effluent can be within 0.5ppm under the optimized condition; (5) the whole treatment process is efficient, high in stability and strong in impact resistance, and TP of lithium hexafluorophosphate wastewater can meet the discharge requirement; (6) the method has the advantages that the treatment cost is low, the economic benefit is good, when the concentration of TP of the incoming water is 400ppm, and when the concentration of TP of treated effluent is within 1ppm, the treatment cost is within 7 yuan/ton probably; (7) meanwhile, the process is also suitable for treating wastewater containing trifluoro phosphoric acid, lithium difluorophosphate and lithium monofluorophosphate.
See the experimental case below, where TP (total phosphorus) in raw water was 414 mg/L.
TABLE 1 Experimental conditions
As can be seen from the experimental data in Table 1, the experimental example 1 has the best effect and very obvious treatment effect, can degrade TP of lithium hexafluorophosphate wastewater from 400ppm to within 3ppm, can remove the pungent odor of the wastewater, and has very strong applicability to lithium hexafluorophosphate production enterprises.
FIG. 2 is a schematic view showing the construction of a wastewater treatment apparatus according to the present invention.
Lithium hexafluorophosphate and lithium low fluorophosphate compound effluent treatment plant is including the alkali of setting gradually and analyse subassembly 1, catalytic hydrolysis subassembly 2, alkaline hydrolysis subassembly 3 and dephosphorization subassembly 4. Wherein the alkaline-leaching assemblies 1 are provided in two groups.
The alkaline analysis module 1 corresponds to step S1 described above. Each group of alkali analysis assemblies 1 comprises an alkali reaction tank I5, a coagulant adding tank I14 and a sedimentation tank I6.
Waste water gets into alkali reaction tank I5 from A entry, is connected with alkali reaction tank I5 and still is provided with alkali and adds the mechanism (not shown in the figure) to adjust the pH of waste water in alkali reaction tank I5 to 9~10, carry out the alkali through the stirring of rabbling mechanism 13 and separate out. Then, the wastewater enters a coagulant addition tank I14, PAC and PAM are added into the coagulant addition tank I14, and stirring is performed by a stirring mechanism 13 arranged therein. And then the wastewater enters a sedimentation tank I6 for sedimentation, and the sedimentation tank I6 is an inclined plate sedimentation tank. Sludge is discharged from an outlet B arranged at the bottom of the sedimentation tank I6.
As shown in fig. 2, another set of the alkaline analysis module 1 on the right is also provided, and the reagent added to the alkaline reaction tank i 5 is different from that added to the previous set (left) of the alkaline analysis module 1. In the basic analysis component 1, a calcium-containing compound (lime or calcium chloride) is added into a basic reaction tank I5. The present caustic precipitation module 1 is mainly used for removing fluoride ions.
By removing fluorine through the two sets of alkaline separation assemblies 1, the hydrolysis can be promoted, and the formation of a complex compound of high-concentration lithium ions on subsequent products or medicaments can be avoided, so that hexafluorophosphoric acid can not be degraded completely, and phosphorus and fluorine can not be removed completely.
The catalytic hydrolysis module 2 comprises an acid reaction tank 7 and a catalytic material 8 (catalytic packing) disposed in the acid reaction tank 7. An acid adding mechanism (not shown) is connected to the acid reaction tank 7 to add hydrochloric acid to the acid reaction tank 7. The catalytic hydrolysis component 2 is also provided with a heating mechanism (not shown in the figure) for heating the wastewater to 60-70 ℃. The catalyst is a mixture of iron simple substance, carbon simple substance and titanium oxide, is similar to a sphere, and is loaded in the acid reaction tank 7.
The alkaline hydrolysis component 3 comprises an alkaline reaction tank II 9 and a sedimentation tank II 10 (inclined plate sedimentation tank). The alkali reaction tank II 9 is provided with a stirring mechanism 13 and a heating mechanism (not shown) for controlling the reaction conditions. The control conditions in the alkali reaction tank II 9 are as follows: the pH is 9.5-10, and the temperature is 50-70 ℃. The wastewater is precipitated in the sedimentation tank II 10 (coagulant is added before the precipitation), and sludge is discharged from an outlet D arranged at the bottom of the sedimentation tank II 10.
The dephosphorization component 4 comprises a dephosphorization pool 11, a coagulant adding pool II 15 and a sedimentation pool III 12. Wherein, a phosphorus removing agent adding mechanism (not shown in the figure) is connected with the phosphorus removing tank 11 to add the phosphorus removing agent into the phosphorus removing tank 11, and a heating mechanism (not shown in the figure) is also arranged in the phosphorus removing tank 11 to heat the wastewater. The dephosphorization pool 11 is provided with a stirring mechanism 13 so as to accelerate the reaction.
A coagulant addition mechanism (not shown in the figure) is connected to the coagulant addition tank ii 15 to add a coagulant to the coagulant addition tank ii 15. The coagulant is stirred by the stirring mechanism 13 to be sufficiently mixed with the wastewater.
The wastewater is precipitated in a precipitation tank III 12. And discharging sludge from an outlet E arranged at the bottom of the sedimentation tank III 12, and discharging water from an outlet F arranged at the upper part of the sedimentation tank III 12.
In conclusion, the lithium hexafluorophosphate and lithium low-fluoride phosphate compound wastewater treatment process and device can fully hydrolyze the lithium hexafluorophosphate and lithium low-fluoride phosphate compound, remove TP, F and Li in wastewater, and meet the removal requirement of total phosphorus in wastewater in the industry.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (6)
1. A process for treating waste water containing lithium hexafluorophosphate and lithium difluorophosphate compounds is characterized by comprising the following steps:
s1, adding alkali into the wastewater for alkali precipitation, adjusting the pH to 9-10, then adding a calcium-containing compound and a flocculating agent, and separating precipitates;
s2, adding acid into the wastewater, adjusting the pH to 2-3, heating the wastewater to 60-70 ℃, and enabling the wastewater to pass through a fixed bed catalytic filler, wherein the catalytic filler comprises an iron simple substance, a carbon simple substance and titanium oxide;
s3, adding alkali into the wastewater, adjusting the pH value to 9.5-10, heating the wastewater to 50-70 ℃, carrying out hydrolysis reaction for 5-7 hours, and adding lime into the wastewater after the hydrolysis reaction is finished;
s4, adding a phosphorus removing agent and a flocculating agent into the wastewater.
2. The process for treating wastewater containing lithium hexafluorophosphate and lithium difluorophosphate compounds according to claim 1, wherein: in S1, the precipitate is separated after the alkali is added, the calcium-containing compound is added, and the precipitate is filtered again.
3. The process for treating wastewater containing lithium hexafluorophosphate and lithium difluorophosphate compounds according to claim 1, wherein: the calcium-containing compound is quicklime or calcium chloride.
4. The utility model provides a lithium hexafluorophosphate and lithium low fluorophosphate compound effluent treatment plant which characterized in that, it includes that the upper and lower reaches set up:
the alkali analysis assembly (1) comprises an alkali reaction tank I (5) and a sedimentation tank I (6);
the catalytic hydrolysis assembly (2) comprises an acid reaction tank (7) and a catalytic filler (8) arranged in the acid reaction tank (7), wherein the catalytic filler (8) comprises a simple substance of iron, a simple substance of carbon and titanium oxide;
the alkaline hydrolysis component (3), the alkaline hydrolysis component (3) comprises an alkaline reaction tank II (9) and a sedimentation tank II (10);
the dephosphorization component (4), the dephosphorization component (4) includes dephosphorization pond (11) and sedimentation tank III (12).
5. The apparatus for treating wastewater containing lithium hexafluorophosphate and lithium difluorophosphate compounds according to claim 4, wherein: the alkali analysis component (1) is provided with two sets which are connected in series.
6. The apparatus for treating wastewater containing lithium hexafluorophosphate and lithium difluorophosphate compounds according to claim 4, wherein: the catalytic hydrolysis component (2) and/or the alkaline hydrolysis component (3) are/is also provided with a heating mechanism.
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