CN115594280A - Pretreatment process of wastewater containing fluorine sulfonate - Google Patents
Pretreatment process of wastewater containing fluorine sulfonate Download PDFInfo
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- CN115594280A CN115594280A CN202211391899.5A CN202211391899A CN115594280A CN 115594280 A CN115594280 A CN 115594280A CN 202211391899 A CN202211391899 A CN 202211391899A CN 115594280 A CN115594280 A CN 115594280A
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- fluorosulfonate
- fluorine
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- 239000002351 wastewater Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000008569 process Effects 0.000 title claims abstract description 28
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 24
- 239000011737 fluorine Substances 0.000 title claims abstract description 24
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- UQSQSQZYBQSBJZ-UHFFFAOYSA-M fluorosulfonate Chemical compound [O-]S(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-M 0.000 claims description 11
- 238000005243 fluidization Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002910 solid waste Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 5
- 238000010561 standard procedure Methods 0.000 abstract description 5
- 238000006115 defluorination reaction Methods 0.000 abstract description 4
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 3
- 230000004888 barrier function Effects 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 238000005086 pumping Methods 0.000 abstract description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 4
- 229910001628 calcium chloride Inorganic materials 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- CHHOPPGAFVFXFS-UHFFFAOYSA-M [Li+].[O-]S(F)(=O)=O Chemical compound [Li+].[O-]S(F)(=O)=O CHHOPPGAFVFXFS-UHFFFAOYSA-M 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229910052747 lanthanoid Inorganic materials 0.000 description 3
- 150000002602 lanthanoids Chemical class 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000012163 sequencing technique Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Images
Classifications
-
- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- 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
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
-
- 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
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
Abstract
The invention relates to a pretreatment process of fluorine-containing sulfonate wastewater, which comprises the following steps: s1, adding sodium hydroxide into the fluorine-containing sulfonate wastewater, heating to 90-95 ℃, and stirring for reaction; s2, pumping the wastewater of the S1 into a defluorination reaction kettle, adding a composite defluorination agent and PAC, and stirring for reaction; and S3, adding PAM into the S2 wastewater after the reaction is finished, removing precipitates, and allowing the supernatant to enter a subsequent process. Breaks through the technical barrier of pretreatment of the wastewater containing the fluorine sulfonate, can achieve the purpose of pretreatment process with the fluorine sulfonate less than or equal to 2ppm and LAS (national standard method) less than or equal to 2ppm, and enters a biochemical treatment system for deep removal of COD, ammonia nitrogen and total nitrogen after pretreatment.
Description
Technical Field
The invention belongs to the field of environmental protection, relates to a pretreatment process of industrial wastewater, and particularly relates to a pretreatment process of fluorine-containing sulfonate production wastewater.
Background
Lithium fluorosulfonate is a novel lithium salt that can be used as an electrolyte for lithium ion battery electrolytes. When lithium is used as an electrolyte for a lithium ion battery, the high-temperature charge-discharge cycle characteristics of the lithium battery can be greatly improved, and a high capacity retention rate of the battery can be maintained.
In the known methods for producing lithium fluorosulfonate, most of the processes for producing lithium fluorosulfonate involve reaction of lithium salt with fluorosulfonic acid or chlorosulfonic acid, which results in a large amount of waste gas and is difficult to handle, and in the presence of many side reactions, which result in many impurities and affect the yield.
The physical and chemical precipitation and resin adsorption widely applied in the field of wastewater treatment at present have very little removal effect and higher operation cost. The fluorosulfonic acid is dissolved in water, which has serious interference on the detection of anionic surfactants, and the detection value of the water quality is abnormally increased, but the problem cannot be fundamentally solved only from the aspect of anionic surface activity, and the treatment of the wastewater is more difficult. Through published literature data inquiry, the technical vacuum exists in domestic treatment research or engineering application aiming at the wastewater, and with the increasing strictness of the wastewater discharge standard, the requirements of deep fluorine and phosphorus removal of the wastewater are more urgent.
Chinese patent document CN115072912A discloses a combined treatment method for fluororesin production wastewater, which treats wastewater by resin adsorption and electrochemistry, and the process can reduce the index of an anionic surfactant, but has huge operation cost and generates other pollutants.
Disclosure of Invention
The invention aims to provide a pretreatment process for wastewater containing fluorosulfonate, which solves the problems of fluorine removal and phosphorus removal of wastewater produced by lithium battery electrolyte.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a pretreatment process of fluorine-containing sulfonate wastewater, which comprises the following steps:
s1, adding sodium hydroxide into the fluorine-containing sulfonate wastewater, heating to 90-95 ℃, and stirring for reaction;
s2, pumping the wastewater of the S1 into a defluorination reaction kettle, adding a composite defluorination agent and PAC, and stirring for reaction;
and S3, adding PAM into the S2 wastewater after the reaction is finished, removing precipitates, and allowing the supernatant to enter a subsequent process.
Preferably, the wastewater is treated in the form of stirring circulating fluidization in S1 and/or S2 and/or S3.
Further, the rotating speed of the stirrer in S1 and/or S2 is kept at 300r/m, the reaction retention time of S1 is 2-4h, the reaction retention time of S2 is 30min-45min, the rotating speed of the stirrer in S3 is kept at 60r/m, and the reaction retention time is 10min-15min.
Preferably, the waste water is heated by passing steam into the waste water.
Preferably, S1 adds sodium hydroxide into the wastewater, the pH value is more than or equal to 13 after the addition is finished, and the pH value is more than or equal to 12 after the reaction is finished by adding for multiple times in the reaction process.
Preferably, the complete mixed solution in S1 and S2 is subjected to the next treatment procedure, and the supernatant in S3 is subjected to the subsequent treatment procedure, and the solid waste is discharged for further treatment.
Preferably, S1, S2 and S3 are used for treating wastewater by using a sequencing batch fluidized bed or a reaction kettle.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the pretreatment process of the fluorine-containing sulfonate wastewater breaks through the technical barrier of the pretreatment of the fluorine-containing sulfonate wastewater, can achieve the purpose of the pretreatment process of the fluorine sulfonate being less than or equal to 2ppm and LAS (national standard method) being less than or equal to 2ppm, and enters a biochemical treatment system for deep removal of COD, ammonia nitrogen and total nitrogen after pretreatment.
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 diagram of the steps of a preferred embodiment of the present invention.
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.
The fluorine-containing sulfonate wastewater pretreatment process shown in figure 1 comprises the following steps:
s1, adding sodium hydroxide into the fluorine-containing sulfonate wastewater, heating to 90-95 ℃, stirring for reaction, adjusting the pH value to be more than or equal to 13, adding for multiple times in the reaction process, ensuring that the pH value is more than or equal to 12 after the reaction is finished, and keeping the reaction for 2-4 hours;
s2, adding a composite defluorinating agent and PAC into the wastewater obtained in the S1, and stirring for reaction, wherein the composite defluorinating agent is a mixture of calcium hydroxide, calcium chloride, aluminum chloride and lanthanide metal;
and S3, adding PAM into the S2 wastewater after the reaction is finished, removing precipitates, and allowing the supernatant to enter a subsequent process.
In S1, fluorosulfonate is sufficiently hydrolyzable.
Although this example uses this kind of composite fluorine removing agent (a mixture of calcium hydroxide, calcium chloride, aluminum chloride, and a lanthanide metal), in other ways, the fluorine removing agent may be any one of calcium hydroxide, calcium chloride, aluminum chloride, and a lanthanide metal, or a mixture of any two or more of them.
The invention breaks through the technical barrier of deep pretreatment of the wastewater containing the fluorosulfonate, can achieve the purpose of pretreatment process with the fluorosulfonate less than or equal to 2ppm and LAS (national standard method) less than or equal to 2ppm, has good removal effect and economy, and then enters a biochemical treatment system for deep removal of COD, ammonia nitrogen and total nitrogen.
The present example employed an experiment to examine the wastewater treatment results as follows.
Taking two liters of fluorine-containing sulfonate wastewater, wherein the fluorine-containing sulfonate wastewater is 1000ppm, LAS (national standard method) is 100ppm, adding 45g of sodium hydroxide solid into the wastewater, heating to 95 ℃, starting a stirrer, adjusting the rotating speed to 300r/min, stirring at constant temperature for 4h, adding calcium chloride after the reaction is finished, adding PAC, stirring for 0.5h, adding PAM, adjusting the rotating speed to 60r/min, stirring for 10min, standing, precipitating, taking supernatant, testing and analyzing, and finally obtaining the detection result that the fluorine sulfonate is less than or equal to 2ppm and the LAS (national standard method) is less than or equal to 2ppm.
The process has the following advantages: the embodiment adopts a multistage series fluidized bed process, has simple route, good mixing and homogenizing reaction effect and strong impact resistance; the process control parameters are few and easy to quantify, the types of medicines are conventional, and the operation cost is low; moreover, automatic operation can be realized, labor cost is greatly saved, and process operation control risk is reduced.
The present embodiment adopts a series continuous flow fluidized bed process operation, if a sequencing batch fluidized bed or a reaction kettle type operation device is adopted, the pretreatment effect can be achieved by adopting the operation parameters of the present invention, and the present invention has only slightly low efficiency, belongs to the simple change of the present invention, and is also within the protection scope of the present invention.
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 (8)
1. A pretreatment process of wastewater containing fluorine sulfonate comprises the following steps:
s1, adding sodium hydroxide into the fluorine-containing sulfonate wastewater, heating to 90-95 ℃, and stirring for reaction;
s2, adding a fluorine removal agent and PAC into the S1 wastewater, and stirring for reaction;
and S3, adding PAM into the S2 wastewater after the reaction is finished, removing precipitates, and allowing the supernatant to enter a subsequent process.
2. The process of pretreating fluorosulfonate-containing wastewater according to claim 1, wherein: s1, adding NaOH into the wastewater, adjusting the pH value to be more than or equal to 13, and adding the NaOH for multiple times in the reaction process to ensure that the pH value is more than or equal to 12 after the reaction is finished.
3. The process of pretreating fluorosulfonate-containing wastewater according to claim 1, wherein: the reaction residence time in S1 is 2-4h.
4. The fluorosulfonate-containing wastewater pretreatment process according to claim 1, characterized in that: and in the S1 and/or S2 and/or S3, the wastewater is treated in a stirring circulating fluidization mode.
5. The fluorosulfonate-containing wastewater pretreatment process according to claim 1, characterized in that: the waste water is heated by introducing steam into the waste water.
6. The fluorosulfonate-containing wastewater pretreatment process according to claim 1, characterized in that: s1 and S2 are that the complete mixed solution enters the next treatment procedure, and S3 is that the supernatant enters the next treatment procedure, and the solid waste is discharged for further treatment.
7. The fluorosulfonate-containing wastewater pretreatment process according to claim 1, characterized in that: and S1, S2 and S3 adopt a reaction kettle to treat the wastewater.
8. The fluorosulfonate-containing wastewater pretreatment process according to claim 1, characterized in that: s1, S2 and S3 adopt a serial continuous flow fluidized bed to treat the wastewater.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211391899.5A CN115594280A (en) | 2022-11-08 | 2022-11-08 | Pretreatment process of wastewater containing fluorine sulfonate |
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| CN202211391899.5A CN115594280A (en) | 2022-11-08 | 2022-11-08 | Pretreatment process of wastewater containing fluorine sulfonate |
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