CN118255442A - A high-efficiency composite defluoridation agent and a method for removing fluoride from fluoride-containing wastewater - Google Patents
A high-efficiency composite defluoridation agent and a method for removing fluoride from fluoride-containing wastewater Download PDFInfo
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- CN118255442A CN118255442A CN202410519445.4A CN202410519445A CN118255442A CN 118255442 A CN118255442 A CN 118255442A CN 202410519445 A CN202410519445 A CN 202410519445A CN 118255442 A CN118255442 A CN 118255442A
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- 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
- C02F1/583—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing fluoride or fluorine 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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Abstract
本发明提供了一种高效复合除氟剂及去除含氟废水中氟的方法，所述高效复合除氟剂，按重量百分比计包括如下组分：铝盐30‑50％、铁盐20‑40％、复合硅酸盐5‑10％、磷酸盐5‑10％和氟离子吸附剂10‑30％；其中，所述氟离子吸附剂为La改性沸石。本发明提出的一种高效复合除氟剂及去除含氟废水中氟的方法，该复合除氟剂综合了各组分的优势，在去除氟化物的同时无需投加其它絮凝剂或助凝剂，明显提高了除氟和污泥沉降效果。
The present invention provides a high-efficiency composite defluoridation agent and a method for removing fluorine from fluoride-containing wastewater, wherein the high-efficiency composite defluoridation agent comprises the following components by weight percentage: 30-50% aluminum salt, 20-40% iron salt, 5-10% composite silicate, 5-10% phosphate and 10-30% fluoride ion adsorbent; wherein the fluoride ion adsorbent is La-modified zeolite. The present invention proposes a high-efficiency composite defluoridation agent and a method for removing fluorine from fluoride-containing wastewater, wherein the composite defluoridation agent combines the advantages of each component, does not need to add other flocculants or coagulants while removing fluoride, and significantly improves the defluoridation and sludge sedimentation effects.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a high-efficiency compound fluorine removing agent and a method for removing fluorine in fluorine-containing wastewater.
Background
Certain fluorine-containing wastewater is generated in a crystal pulling link and a battery link in the photovoltaic industry and in the third-generation semiconductor industry, and the traditional treatment method is to add agents such as lime water, calcium chloride, polyaluminium chloride and polyacrylamide, so that the fluorine ions are reduced from 1000-2000mg/L to below 8mg/L, and the wastewater reaches the indirect emission standard in the Table 2 of the Battery industry pollutant emission standard (GB 3084-2013) or the water pollutant emission standard in the semiconductor industry through pretreatment devices of enterprises, namely the fluorine ions are smaller than 8mg/L. After being treated by the pretreatment device, wastewater of the photovoltaic industry or the semiconductor industry enterprises is discharged into centralized sewage treatment plants such as municipal administration and parks, the pretreated fluorine-containing wastewater needs to be further reduced by less than 1.5mg/L, and many centralized sewage treatment plants do not have fluorine removal capability or fluorine removal facilities.
Along with the vigorous development of the photovoltaic and semiconductor industries, the volume and fluoride content of wastewater are higher and higher, so that the pressure of the fluoride-containing wastewater in a pretreatment workshop by a calcium salt precipitation method in the traditional process is higher and the concentration of tail water is higher and higher. On the one hand, the calcium salt method is limited by the solubility of the product calcium fluoride, the maximum degree can only be reduced to below 8mg/L, and the F-concentration can not be continuously reduced to below 1.5 mg/L. On the other hand, government has also placed increasing emphasis on emissions of fluorine. Under double pressure, common fluorine scavengers are increasingly difficult to meet the increasingly changing environmental requirements.
Disclosure of Invention
Based on the technical problems in the background technology, the invention provides the high-efficiency compound fluorine removing agent and the method for removing fluorine in the fluorine-containing wastewater, the compound fluorine removing agent combines the advantages of all components, other flocculating agents or coagulant aids are not required to be added while removing fluoride, and the fluorine removing and sludge settling effects are obviously improved.
The invention provides a high-efficiency composite defluorinating agent, which comprises the following components in percentage by weight: 30-50% of aluminum salt, 20-40% of ferric salt, 5-10% of composite silicate, 5-10% of phosphate and 10-30% of fluoride ion adsorbent;
wherein the fluoride ion adsorbent is La modified zeolite.
In the invention, aluminum salt, ferric salt and the like in the compound defluorinating agent can form a large amount of colloid substances in water, and are condensed into floccules, so that the purpose of defluorinating is achieved by adsorbing fluorine in the water in the process of precipitation; meanwhile, la modified zeolite is used as an auxiliary material, has a ligand mutually matched with fluorine ions, so that the molecular weight of the La modified zeolite is increased, the La modified zeolite can be more effectively captured in the colloid and flocculation processes, and the fluorine removal effect is further improved.
Preferably, the aluminum salt is at least one of aluminum chloride, polyaluminum chloride, aluminum sulfate, polyaluminum ferric chloride, polyaluminum ferric sulfate or sodium metaaluminate.
Preferably, the iron salt is at least one of ferric chloride, ferric sulfate, polymeric ferric chloride, polymeric ferric sulfate, or potassium ferrate.
Preferably, the composite silicate is at least one of polyaluminosilicate, polyaluminosilicate iron, sodium silicate or magnesium aluminum silicate.
Preferably, the phosphate is at least one of disodium hydrogen phosphate or sodium dihydrogen phosphate.
Preferably, the preparation method of the La modified zeolite comprises the following steps: after modifying zeolite by an alkenyl silane coupling agent, copolymerizing the zeolite with an ammonium salt ion monomer, an alkenyl monomer and an unsaturated acid monomer, and then mixing the zeolite with a lanthanum source for reaction to obtain the La modified zeolite;
Preferably, the mass ratio of the zeolite, the alkenyl silane coupling agent, the ammonium salt ion monomer, the alkenyl monomer and the unsaturated acid monomer is 10:1-3:0.1-1:3-6:2-5.
Preferably, the alkenyl silane coupling agent is at least one of vinyl trimethoxy silane, vinyl triethoxy silane or 3- (methacryloyloxy) propyl trimethoxy silane, the ammonium salt ion monomer is at least one of methacryloyloxyethyl trimethyl ammonium chloride or methacrylamidopropyl trimethyl ammonium chloride, the alkenyl monomer is at least one of acrylamide, methacrylamide, ethyl acrylate or ethyl methacrylate, and the unsaturated acid monomer is at least one of acrylic acid, methacrylic acid, maleic acid or fumaric acid; the lanthanum source is at least one of lanthanum chloride, lanthanum nitrate or lanthanum acetate.
According to the invention, natural zeolite is used as a matrix material, alkenyl functional natural zeolite is obtained after modification by an alkenyl silane coupling agent, and is copolymerized with ammonium salt ion monomers, alkenyl monomers and unsaturated acid monomers to obtain the amphoteric polymer-coated fluorine ion adsorbent which simultaneously has ammonium radical cations and acid radical anions and penetrates through holes and pore channels of the natural zeolite, on one hand, the existence of the ammonium radical cations can play a role in adsorption flocculation reinforcement, on the other hand, the acid radical anions can be complexed with metal ions, and after mixing reaction with a lanthanum source, the acid radical anions are complexed with La to form a crosslinked network structure, so that the purpose of deep fluorine removal is achieved, and once La reacts with fluorine, the formed fluorine-lanthanum complex is difficult to release in an aqueous solution, so that the fluorine removal from water is very favorable. The book is provided with
The invention also provides a preparation method of the high-efficiency composite defluorinating agent, which comprises the following steps: and ball-milling and uniformly mixing the aluminum salt, the ferric salt, the composite silicate, the phosphate and the fluoride ion adsorbent according to the weight percentage to obtain the high-efficiency composite defluorinating agent.
The invention also provides a method for removing fluorine in the fluorine-containing wastewater, which comprises the following steps: and adding the fluorine removing agent or the fluorine removing agent prepared by the preparation method into the fluorine-containing wastewater.
Preferably, after fluorine in the fluorine-containing wastewater is removed, the concentration of fluoride ions is less than 1mg/L.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention introduces the fluoride ion adsorbent on the basis of the traditional defluorinating agent to enhance the effect of removing fluoride in water, and the raw materials used are all conventional reagents, so that the invention has low price and wide sources, can be widely applied to removing fluoride in industrial wastewater, surface water and underground water, does not contain calcium salt and magnesium salt, and does not increase the hardness of effluent after use.
(2) The invention has good defluorination effect, can stably reduce the fluoride in the wastewater with the fluoride concentration below 60mg/L to below 1mg/L, and can only produce a very small amount of sludge with the water content of 70% per ton of wastewater while meeting the deep defluorination requirement.
Drawings
FIG. 1 is a schematic structural diagram of a fluoride ion adsorbent according to example 1 of the present invention.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, which should be explicitly set forth for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a high-efficiency composite defluorinating agent, which comprises the following components in percentage by weight: 23% of polyaluminum chloride, 17% of aluminum sulfate, 28% of ferric sulfate, 8% of polysilicate, 6% of disodium hydrogen phosphate and 18% of fluoride ion adsorbent;
Wherein, the fluoride ion adsorbent is La modified zeolite, and the preparation method specifically comprises the following steps: grinding natural zeolite (mordenite) into powder, adding into absolute ethyl alcohol, dispersing uniformly, adding vinyl trimethoxy silane with the mass of 20wt% of the natural zeolite, heating to 60 ℃, stirring, reacting for 4 hours, spin-drying the solvent, adding into water, dispersing uniformly, adding methacrylic oxyethyl trimethyl ammonium chloride with the mass of 5wt% of the natural zeolite, acrylamide with the mass of 45wt% of the natural zeolite, acrylic acid with the mass of 30wt% of the natural zeolite, adding potassium persulfate with the mass of 0.5wt% of the natural zeolite under the protection of nitrogen, heating to 80 ℃, stirring, reacting for 5 hours, concentrating, drying, adding into 0.1M lanthanum chloride solution, heating to 60 ℃, oscillating, reacting for 2 hours, filtering, and drying to obtain the La modified zeolite.
The preparation method of the high-efficiency composite defluorinating agent comprises the following steps: adding the aluminum salt, the ferric salt, the composite silicate, the phosphate and the fluoride ion adsorbent into a ball mill according to the weight percentage, and ball-milling and uniformly mixing under the condition that the rotating speed is 300rpm to obtain the high-efficiency composite fluorine removing agent.
Example 2
The embodiment provides a high-efficiency composite defluorinating agent, which comprises the following components in percentage by weight: 30% of aluminum sulfate, 13% of ferric chloride, 27% of polymeric ferric chloride, 5% of polymeric aluminum ferric silicate, 10% of sodium dihydrogen phosphate and 15% of fluoride ion adsorbent;
Wherein, the fluoride ion adsorbent is La modified zeolite, and the preparation method specifically comprises the following steps: grinding natural zeolite (mordenite) into powder, adding into absolute ethyl alcohol, dispersing uniformly, adding vinyl trimethoxy silane with the mass of 20wt% of the natural zeolite, heating to 60 ℃, stirring, reacting for 4 hours, spin-drying the solvent, adding into water, dispersing uniformly, adding methacrylic oxyethyl trimethyl ammonium chloride with the mass of 5wt% of the natural zeolite, acrylamide with the mass of 45wt% of the natural zeolite, acrylic acid with the mass of 30wt% of the natural zeolite, adding potassium persulfate with the mass of 0.5wt% of the natural zeolite under the protection of nitrogen, heating to 80 ℃, stirring, reacting for 5 hours, concentrating, drying, adding into 0.1M lanthanum chloride solution, heating to 60 ℃, oscillating, reacting for 2 hours, filtering, and drying to obtain the La modified zeolite.
The preparation method of the high-efficiency composite defluorinating agent comprises the following steps: adding the aluminum salt, the ferric salt, the composite silicate, the phosphate and the fluoride ion adsorbent into a ball mill according to the weight percentage, and ball-milling and uniformly mixing under the condition that the rotating speed is 300rpm to obtain the high-efficiency composite fluorine removing agent.
Example 3
The embodiment provides a high-efficiency composite defluorinating agent, which comprises the following components in percentage by weight: 27% of polyaluminum sulfate, 23% of aluminum chloride, 20% of ferric chloride, 10% of sodium silicate, 5% of disodium hydrogen phosphate and 15% of fluoride ion adsorbent;
Wherein, the fluoride ion adsorbent is La modified zeolite, and the preparation method specifically comprises the following steps: grinding natural zeolite (mordenite) into powder, adding into absolute ethyl alcohol, dispersing uniformly, adding vinyl trimethoxy silane with the mass of 20wt% of the natural zeolite, heating to 60 ℃, stirring, reacting for 4 hours, spin-drying the solvent, adding into water, dispersing uniformly, adding methacrylic oxyethyl trimethyl ammonium chloride with the mass of 5wt% of the natural zeolite, acrylamide with the mass of 45wt% of the natural zeolite, acrylic acid with the mass of 30wt% of the natural zeolite, adding potassium persulfate with the mass of 0.5wt% of the natural zeolite under the protection of nitrogen, heating to 80 ℃, stirring, reacting for 5 hours, concentrating, drying, adding into 0.1M lanthanum chloride solution, heating to 60 ℃, oscillating, reacting for 2 hours, filtering, and drying to obtain the La modified zeolite.
The preparation method of the high-efficiency composite defluorinating agent comprises the following steps: adding the aluminum salt, the ferric salt, the composite silicate, the phosphate and the fluoride ion adsorbent into a ball mill according to the weight percentage, and ball-milling and uniformly mixing under the condition that the rotating speed is 300rpm to obtain the high-efficiency composite fluorine removing agent.
Comparative example 1
The comparative example provides a high-efficiency compound defluorinating agent, which comprises the following components in percentage by weight: 23% of polyaluminum chloride, 17% of aluminum sulfate, 28% of ferric sulfate, 8% of polysilicate, 6% of disodium hydrogen phosphate and 18% of fluoride ion adsorbent;
Wherein, the fluoride ion adsorbent is La modified zeolite, and the preparation method specifically comprises the following steps: grinding natural zeolite (mordenite) into powder, adding into 0.1M lanthanum chloride solution, heating to 60 ℃, oscillating for 2h, filtering, and drying to obtain the La modified zeolite.
The preparation method of the high-efficiency composite defluorinating agent comprises the following steps: adding the aluminum salt, the ferric salt, the composite silicate, the phosphate and the fluoride ion adsorbent into a ball mill according to the weight percentage, and ball-milling and uniformly mixing under the condition that the rotating speed is 300rpm to obtain the high-efficiency composite fluorine removing agent.
Comparative example 2
The comparative example provides a high-efficiency compound defluorinating agent, which comprises the following components in percentage by weight: 23% of polyaluminum chloride, 17% of aluminum sulfate, 28% of ferric sulfate, 8% of polysilicate, 6% of disodium hydrogen phosphate and 18% of fluoride ion adsorbent;
Wherein, the fluoride ion adsorbent is modified zeolite, and the preparation method specifically comprises the following steps: grinding natural zeolite (mordenite) into powder, adding into absolute ethyl alcohol, dispersing uniformly, adding vinyl trimethoxy silane with the mass of 20wt% of the natural zeolite, heating to 60 ℃, stirring and reacting for 4 hours, spin-drying the solvent, adding into water, dispersing uniformly, adding methacrylic oxyethyl trimethyl ammonium chloride with the mass of 5wt% of the natural zeolite, acrylamide with the mass of 45wt% of the natural zeolite, acrylic acid with the mass of 30wt% of the natural zeolite, adding potassium persulfate with the mass of 0.5wt% of the natural zeolite under the protection of nitrogen, heating to 80 ℃, stirring and reacting for 5 hours, concentrating, and drying to obtain the modified zeolite.
The preparation method of the high-efficiency composite defluorinating agent comprises the following steps: adding the aluminum salt, the ferric salt, the composite silicate, the phosphate and the fluoride ion adsorbent into a ball mill according to the weight percentage, and ball-milling and uniformly mixing under the condition that the rotating speed is 300rpm to obtain the high-efficiency composite fluorine removing agent.
Comparative example 3
The comparative example provides a high-efficiency compound defluorinating agent, which comprises the following components in percentage by weight: 23% of polyaluminum chloride, 17% of aluminum sulfate, 28% of ferric sulfate, 8% of polysilicate, 6% of disodium hydrogen phosphate and 18% of fluoride ion adsorbent;
Wherein, the fluoride ion adsorbent is modified zeolite, and the preparation method specifically comprises the following steps: grinding natural zeolite (mordenite) into powder, adding into absolute ethyl alcohol, dispersing uniformly, adding vinyl trimethoxy silane with the mass of 20wt% of the natural zeolite, heating to 60 ℃, stirring and reacting for 4 hours, spin-drying the solvent, adding into water, dispersing uniformly, adding acrylamide with the mass of 45wt% of the natural zeolite and acrylic acid with the mass of 30wt% of the natural zeolite, adding potassium persulfate with the mass of 0.5wt% of the natural zeolite under the protection of nitrogen, heating to 80 ℃, stirring and reacting for 5 hours, concentrating, drying, adding into 0.1M lanthanum chloride solution, heating to 60 ℃, oscillating and reacting for 2 hours, filtering, and drying to obtain the modified zeolite.
The preparation method of the high-efficiency composite defluorinating agent comprises the following steps: adding the aluminum salt, the ferric salt, the composite silicate, the phosphate and the fluoride ion adsorbent into a ball mill according to the weight percentage, and ball-milling and uniformly mixing under the condition that the rotating speed is 300rpm to obtain the high-efficiency composite fluorine removing agent.
(1) 1000ML of fluorine-containing wastewater having an initial concentration of 20mg/L of fluoride ion was treated with the fluorine removing agent obtained in the above examples and comparative examples, and the amount of the fluorine removing agent added was 0.1g, and the results are shown in Table 1 below.
TABLE 1
From the results in table 1 above, it can be seen that: the fluorine removing agent can reduce the concentration of fluorine ions from 20mg/L to below 1mg/L, and has high fluorine removing efficiency.
(2) 1000ML of the fluorine-containing wastewater in actual production (pH 11.5, initial concentration of fluoride ion 82mg/L, turbidity NTU 254) was treated with the fluorine-removing agent obtained in the above examples and comparative examples, and the amount of the fluorine-removing agent added was 1g/L, and the results are shown in Table 2 below.
TABLE 2
From the results in table 2 above, it can be seen that: the fluorine-containing wastewater in the actual production of the fluoride ion concentration can be reduced to below 1mg/L by adopting the fluorine-removing agent, the emission limit requirement of fluoride is completely met, and suspended matters in the fluorine-containing wastewater can be efficiently treated while the fluoride is removed, so that the turbidity of the treated mine water can be stabilized below 10 NTU.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The efficient composite defluorinating agent is characterized by comprising the following components in percentage by weight: 30-50% of aluminum salt, 20-40% of ferric salt, 5-10% of composite silicate, 5-10% of phosphate and 10-30% of fluoride ion adsorbent;
wherein the fluoride ion adsorbent is La modified zeolite.
2. The efficient composite defluorinating agent as claimed in claim 1, wherein the aluminum salt is at least one of aluminum chloride, polyaluminum chloride, aluminum sulfate, polyaluminum ferric chloride, polyaluminum ferric sulfate or sodium metaaluminate.
3. The efficient composite defluorinating agent according to claim 1 or 2, wherein the ferric salt is at least one of ferric chloride, ferric sulfate, polymeric ferric chloride, polymeric ferric sulfate or potassium ferrate.
4. A high efficiency composite fluorine scavenger according to any of claims 1-3 wherein the composite silicate is at least one of polyaluminosilicate, polymeric ferric silicate, polymeric ferric aluminum silicate, sodium silicate or magnesium aluminum silicate.
5. The efficient composite fluorine removing agent according to any one of claims 1 to 4, wherein the phosphate is at least one of disodium hydrogen phosphate or sodium dihydrogen phosphate.
6. The efficient composite fluorine removing agent according to any one of claims 1 to 5, wherein the preparation method of the La modified zeolite comprises: after modifying zeolite by an alkenyl silane coupling agent, copolymerizing the zeolite with an ammonium salt ion monomer, an alkenyl monomer and an unsaturated acid monomer, and then mixing the zeolite with a lanthanum source for reaction to obtain the La modified zeolite;
Preferably, the mass ratio of the zeolite, the alkenyl silane coupling agent, the ammonium salt ion monomer, the alkenyl monomer and the unsaturated acid monomer is 10:1-3:0.1-1:3-6:2-5.
7. The efficient composite fluorine removing agent according to claim 6, wherein the alkenyl silane coupling agent is at least one of vinyl trimethoxy silane, vinyl triethoxy silane or 3- (methacryloyloxy) propyl trimethoxy silane, the ammonium salt ion monomer is at least one of methacryloyloxyethyl trimethyl ammonium chloride or methacrylamidopropyl trimethyl ammonium chloride, the alkenyl monomer is at least one of acrylamide, methacrylamide, ethyl acrylate or ethyl methacrylate, and the unsaturated acid monomer is at least one of acrylic acid, methacrylic acid, maleic acid or fumaric acid; the lanthanum source is at least one of lanthanum chloride, lanthanum nitrate or lanthanum acetate.
8. A method of preparing the high efficiency composite fluorine removal agent of any one of claims 1-7, comprising: and ball-milling and uniformly mixing the aluminum salt, the ferric salt, the composite silicate, the phosphate and the fluoride ion adsorbent according to the weight percentage to obtain the high-efficiency composite defluorinating agent.
9. A method for removing fluorine from fluorine-containing wastewater, comprising: adding the fluorine removing agent in any one of claims 1-7 or the fluorine removing agent prepared by the preparation method in claim 8 into the fluorine-containing wastewater.
10. The method for removing fluorine from fluorine-containing wastewater according to claim 9, wherein after the fluorine in the fluorine-containing wastewater is removed, the concentration of fluorine ions is < 1mg/L.
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