CN116789201B - A method for catalytic degradation of pollutants - Google Patents
A method for catalytic degradation of pollutantsInfo
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- CN116789201B CN116789201B CN202310800156.7A CN202310800156A CN116789201B CN 116789201 B CN116789201 B CN 116789201B CN 202310800156 A CN202310800156 A CN 202310800156A CN 116789201 B CN116789201 B CN 116789201B
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- bismuth
- ferrate
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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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
Abstract
本发明公开了一种催化降解污染物的方法，包括将三价铋盐水溶液加入缓冲盐溶液和含酚类污染物的水体混合液中，在混合液中原位生成氢氧化铋，再利用所述氢氧化铋催化高铁酸盐降解水体污染物。本发明解决了如何原位生成氢氧化铋后高效催化Fe(VI)与水体中有机污染物的问题。由于Bi(III)自身极易水解生成氢氧化物沉淀的特性，对于水体中原位生成的氢氧化铋沉淀易于回收处理，不会引起二次污染且能够多次循环利用，配合高铁酸盐能够有效实现对水体中多种酚类的高效去除，将其应用于Fe(VI)催化反应增效具备优越的应用前景。
The present invention discloses a method for catalytically degrading pollutants, comprising adding a trivalent bismuth salt aqueous solution to a buffered salt solution and a water mixture containing phenolic pollutants, generating bismuth hydroxide in situ in the mixture, and then utilizing the bismuth hydroxide to catalyze ferrate to degrade the water pollutants. The present invention solves the problem of how to efficiently catalyze Fe(VI) and organic pollutants in water after generating bismuth hydroxide in situ. Due to the characteristic that Bi(III) itself is extremely easy to hydrolyze to generate hydroxide precipitates, the bismuth hydroxide precipitates generated in situ in water are easy to recycle and process, will not cause secondary pollution, and can be recycled multiple times. In combination with ferrate, it can effectively achieve efficient removal of multiple phenols in water. Its application in Fe(VI) catalytic reaction efficiency enhancement has excellent application prospects.
Description
Technical Field
The invention relates to a method for degrading phenolic pollutants, in particular to a method for degrading phenolic pollutants by catalyzing ferrate through in-situ generation of bismuth hydroxide.
Background
Ferrate (Fe (VI)) is used as a strong oxidant and has the characteristics of strong selectivity, high efficiency, no toxic or harmful byproducts and the like. The method can be applied to the aspects of efficient oxidation, sterilization, disinfection, adsorption flocculation and the like in the water supply treatment, and particularly has excellent treatment capacity in the water body medicine and personal care product removal. However, fe (VI) is unstable in water and can be rapidly self-decomposed, and the preparation cost is high, and the process condition is complex, so that the application of ferrate is limited.
To solve the above problems, researchers have improved the oxidizing ability of the oxidation system by forming a catalyst in situ in the oxidation system. In the prior art described in journal literature (Synergistic effect of aqueous removal of fluoroquinolones by acombined use of peroxymonosulfate and ferrate(VI),Chemosphere2017,177,144-148.Accelerated Oxidation of Organic Contaminants by Ferrate(VI):The Overlooked Role of Reducing Additives,Environ.Sci.Technol.2018,52(19).Oxidation of manganese(II)with ferrate:Stoichiometry,kinetics,products and impact of organic carbon,Chemosphere2016,159,457-464.Insights into the role of in-situ and ex-situ hydrogen peroxide for enhanced ferrate(VI)towards oxidation of organic contaminants,Water Res.2021,203,117548.Efficient activation of ferrate(VI)by colloid manganese dioxide:Comprehensive elucidation of the surface-promoted mechanism,Water Res.2022,215,118243.), the synergy means for Fe (VI) have been concentrated on the combination with reducing anions such as Persulfate (PMS), thiosulfate (S 2O3 2-), sulfite (SO 3 2-), cu (II), and Fe (III). However, the method has the defects of secondary pollution of the introduced water body, difficult recovery and treatment and the like. Therefore, other efficient and recyclable catalysts are being sought for the widening of the field of application of Fe (VI).
Bismuth-based catalysts (such as bismuth oxyhalide, bismuth-based oxyacid salts and the like) are widely applied in the field of photocatalysis, and no related research has been carried out on positive trivalent bismuth ions (Bi (III)) to remove organic pollutants in water bodies.
Disclosure of Invention
The invention aims to provide a method for catalyzing and degrading pollutants, which is used for solving the problems of secondary pollution, difficult recovery and the like existing in the conventional ferrate synergistic means by utilizing bismuth hydroxide generated in situ in polluted water to carry out synergistic effect on a ferrate oxidative degradation system.
Bismuth hydroxide generated in situ in water body is used as a pollutant degradation catalyst, and Fe (VI) is efficiently catalyzed to degrade organic pollutants in the water body based on the bismuth hydroxide generated in situ.
The method for catalytic degradation of pollutants comprises the steps of generating bismuth hydroxide in situ in a water body containing pollutants, and utilizing the bismuth hydroxide to catalyze ferrate to degrade the water body pollutants.
The bismuth hydroxide precipitate generated in situ is applied to catalyzing Fe (VI) degradation pollutants of ferrate by utilizing the characteristic that Bi (III) is extremely easy to hydrolyze to generate hydroxide precipitate.
Preferably, the method for generating bismuth hydroxide in situ comprises the step of adding a trivalent bismuth salt water solution into a water body containing pollutants to generate bismuth hydroxide precipitate in situ.
Preferably, the trivalent bismuth salt comprises at least one of bismuth nitrate, bismuth sulfate and bismuth chloride, and the pH value of the water body containing the pollutants ranges from 3 to 10. The trivalent bismuth salt can be a pure substance or a bismuth salt hydrate. The proper pH value is more favorable for the trivalent bismuth salt to quickly and uniformly form flocculent bismuth hydroxide precipitate in water, bismuth hydroxide particles in the flocculent precipitate are finer and uniform, and the contact surface area with the water body is larger, so that the flocculent bismuth hydroxide precipitate is more favorable for serving as a catalyst.
Preferably, the trivalent bismuth salt aqueous solution is prepared by dissolving trivalent bismuth salt in nitric acid aqueous solution, and the pH value of the water body containing pollutants is adjusted by adding buffer salt solution. The buffer salt solution can ensure that the pH value of the water body is always in the optimal reaction pH value range, and prevent the generation of bismuth hydroxide precipitation from being influenced by great fluctuation of the pH value in the reaction process.
Preferably, the buffer salt solution is one of boric acid buffer solution, citric acid buffer solution or phosphoric acid buffer solution, and the concentration of the nitric acid aqueous solution is 0.5-1.5M. The trivalent bismuth salt is dissolved in water with the help of dilute nitric acid to prepare the trivalent bismuth salt aqueous solution.
Preferably, the aqueous solution of trivalent bismuth salt is added to the body of water containing the contaminant to a final Bi 3+ concentration of 0.1-10mM.
Preferably, the water contaminant is a phenolic contaminant including at least one of 2-hydroxybenzophenone, benzophenone-1, benzophenone-3, benzophenone-4, benzophenone-7, benzophenone-8, bisphenol S, bisphenol a, 2, 4-difluorophenol, 2,4, 6-trichlorophenol, 2,3,4, 6-tetrachlorophenol, 4-chlorophenol, phenol. The invention can be used for degrading phenolic pollutants, but the Fe (VI) -Bi 3+ oxidation system can have similar reactivity for other micro pollutants except phenolic substances in water.
Preferably, the in-situ generation of bismuth hydroxide catalyzes the degradation of water pollutants by ferrate, which specifically comprises the following steps:
(1) Mixing the buffer salt solution with a water body containing pollutants, and adjusting the pH value to 3-10;
(2) Adding the trivalent bismuth salt aqueous solution into the mixed solution in the step (1) to generate bismuth hydroxide precipitate in situ;
(3) After bismuth hydroxide precipitates are generated, ferrate stock solution is added for reaction, and water pollutants can be degraded.
The concentration of ferrate in the ferrate stock solution in the catalytic degradation step is 10-120mM, the final concentration of ferrate is 10-300 mu M, the molar ratio of ferrate to pollutants is 2.5-30:1, and the solvent of the ferrate stock solution is potassium-boron aqueous solution prepared by dissolving sodium tetraborate and dipotassium hydrogen phosphate in water.
Compared with the prior art, the method has the advantages that the bismuth hydroxide catalyst system adopted by the method is generated in situ, the preparation method is simple, the catalyst generation time is short, the catalytic degradation efficiency is high, and the efficient degradation of various phenolic pollutants can be realized in 5 min. The bismuth hydroxide precipitate generated in situ in the water body is easy to recycle and can be recycled for a plurality of times, the degradation rate can still reach more than 95% after 5 times of recycling, the bismuth hydroxide precipitate has excellent catalytic performance, and the bismuth hydroxide precipitate can be matched with ferrate to effectively realize the efficient removal of various phenols in the water body.
Drawings
FIG. 1 is a scanning electron microscope image of in situ generated bismuth hydroxide;
FIG. 2 is a schematic representation of the kinetics of 2-HBP degradation;
FIG. 3 is a schematic representation of the degradation kinetics of the Fe (VI) -Bi 3+ system for various phenols;
FIG. 4 is a statistical graph of the effect of recycling bismuth hydroxide as a catalyst;
FIG. 5 is a schematic diagram of a catalytic mechanism of Fe (VI) -Bi 3+ system;
FIG. 6 is an XRD spectrum of the catalyst before/after catalytic degradation reaction;
FIG. 7 is an XPS spectrum of a catalyst before/after catalytic degradation;
FIG. 8 is a graph showing the open circuit potential contrast of different reaction systems;
FIG. 9 is a graph showing the instantaneous current change of different reaction systems.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
EXAMPLE 1 method for degrading 2-hydroxybenzophenone (2-HBP) by Fe (VI) -Bi 3+ system is as follows:
(1) Weighing a proper amount of 2-HBP solid, dissolving in a 100mL volumetric flask, preparing a 2.0mM2-HBP stock solution by ultrasonic auxiliary dissolution, storing at a low temperature of 4 ℃ in a dark place, and simulating a water body sample containing phenolic pollutants by using the 2-HBP stock solution.
(2) 0.2312G of potassium ferrate solid was weighed and dissolved in 4.0mL of potassium boron solution prepared from sodium tetraborate and dipotassium hydrogen phosphate in water to give a 40mM ferrate stock solution, wherein the concentration of sodium tetraborate in the potassium boron solution was 1mM, and the concentration of dipotassium hydrogen phosphate was 5mM.
(3) 6.0634G of bismuth nitrate pentahydrate (Bi (NO 3)3·9H2 O) was dissolved in 12.5mL of 1M molar nitric acid aqueous solution, the volume was fixed to 25mL of 0.5M bismuth nitrate aqueous solution prepared by using 0.1M dilute nitric acid aqueous solution, and 100. Mu.L of 8M NaOH solution was previously added to 30mL of borax/boric acid buffer solution having a pH of 8.0 and a concentration of 20mM, so that the pH value of the reaction system after adding bismuth nitrate aqueous solution was the desired optimal reaction pH value, namely, pH value was 8.0.
(4) To 30mL of a boric acid buffer salt system (pH 8.0) was added 150. Mu.L of a 2-HBP stock solution, and 300. Mu.L of Bi (NO 3)3 aqueous solution having a concentration of 0.5M was added under magnetic stirring to give a Bi 3+ final concentration of 5mM in the mixed solution;
(5) After the formation of a white flocculent precipitate was observed (about 10s during the precipitation), 75. Mu.L of a 20mM stock solution of ferrate was added to start the reaction and the reaction was timed, with a molar ratio of ferrate to 2-HBP of 5:1 and a final concentration of ferrate of 50. Mu.M. And measuring the concentration change of the 2-HBP in the system by adopting high performance liquid chromatography and calculating the degradation rate of the 2-HBP. The morphology of bismuth hydroxide precipitate is shown in figure 1.
Results As shown in FIG. 2, FIG. 2 is a schematic diagram showing the degradation kinetics of ferrate to 2-HBP under in situ bismuth hydroxide catalysis, and it can be seen that the in situ generated Bi (OH) 3 precipitate is not substantially adsorbed to the reaction substrate (e.g., 5mM Bi 3+ group), and the removal rate of 2-HBP is improved by 36% (from 35% to 71%) at a final concentration of 5mM Bi (NO 3)3 addition).
Example 2 the remainder were the same as in example 1 except that:
The concentration of ferrate stock was 10mM, the molar ratio of ferrate to 2-HBP was 2.5:1, and the final concentration of ferrate was 25. Mu.M. Bismuth nitrate is replaced by bismuth sulfate, bismuth sulfate is dissolved in 0.5M nitric acid aqueous solution, borax/boric acid buffer solution is replaced by citric acid buffer solution, the optimal reaction pH value is kept to be 3.0, and the Bi 3+ in the mixed solution is kept to be 10mM.
Example 3 the remainder were the same as in example 1 except that:
the concentration of ferrate stock was 120mM, the molar ratio of ferrate to 2-HBP was 30:1, and the final concentration of ferrate was 300. Mu.M. Bismuth nitrate is replaced by bismuth chloride, the bismuth chloride is dissolved in 1.5M nitric acid aqueous solution, borax/boric acid buffer solution is replaced by phosphate buffer solution, the optimal reaction pH value is kept to be pH7.4, and the Bi 3+ in the mixed solution is 0.1mM.
Example 4 degradation experiments were performed by replacing 2-HBP with other phenolic contaminants according to the same method as in example 1, and the results are shown in FIG. 3, and under similar reaction conditions, the method provided by the invention has better removal performance for benzophenone-1, benzophenone-3, benzophenone-4, benzophenone-7, benzophenone-8, bisphenol S, bisphenol A, 2, 4-difluorophenol, 2,4, 6-trichlorophenol, 2,3,4, 6-tetrachlorophenol, 4-chlorophenol and phenol, and has higher universality for phenolic contaminants in water bodies. In FIG. 3, (a) shows the degradation kinetics of benzophenone-1, (b) shows the degradation kinetics of benzophenone-3, (c) shows the degradation kinetics of benzophenone-4, (d) shows the degradation kinetics of benzophenone-7, (e) shows the degradation kinetics of benzophenone-8, (f) shows the degradation kinetics of bisphenol A, (g) shows the degradation kinetics of bisphenol S, (h) shows the degradation kinetics of 2, 4-difluorophenol, (i) shows the degradation kinetics of 2,3,4, 6-tetrachlorophenol, (j) shows the degradation kinetics of 2,4, 6-trichlorophenol, (k) shows the degradation kinetics of 4-chlorophenol, and (l) shows the degradation kinetics of 2-hydroxybenzophenone.
Example 5 recycling experiments with bismuth hydroxide as catalyst:
After the catalyst precipitate after the reaction of the example 1 is centrifuged, the catalyst precipitate is washed once by using methanol solution and deionized water respectively, the washed catalyst precipitate is transferred to borate buffer solution, 2-HBP stock solution and ferrate stock solution are added in sequence, and then the second reaction is started repeatedly. Multiple cycles of reaction steps and so on.
As shown in FIG. 4, the degradation rate of the catalyst is 6 times in turn from left to right, and the recycling experiment of bismuth hydroxide as the catalyst proves that the catalyst still has excellent catalytic performance after 5 times of recycling, and the degradation rate of the phenolic pollutants can still reach more than 95%.
In the Fe (VI) -Bi 3+ degradation reaction system, the catalytic mechanism of bismuth hydroxide is that ferrate can oxidize bismuth hydroxide containing trivalent bismuth ions into sodium bismuthate containing pentavalent bismuth ions, so that the sodium bismuthate containing pentavalent bismuth ions and phenolic pollutants undergo oxidation-reduction reaction and are reduced into bismuth hydroxide containing trivalent bismuth ions again (as shown in figure 5).
To demonstrate the catalytic mechanism of degradation of phenolic contaminants in the above examples, the applicant conducted the following experiments:
Characteristic peaks of sodium bismuthate can be found according to XRD spectra (X-ray diffraction, XRD) of the material after the catalytic degradation reaction and correspond to JCPD standard spectra (No. 85-1130) (shown in figure 6);
XPS (X-ray photoelectron spectroscopy, XPS) characterization results show that the binding energy peak position of the material shifts by 0.14eV after the reaction (as shown in figure 7), and the generation of high-valence bismuth is further proved by [S.Hofmann,Auger-and X-Ray Photoelectron Spectroscopy in Materials Science,Springer,New York 2013,p.487.], consistent with the increase of Bi ion binding energy with the increase of valence state in the literature report.
According to the electrochemical experiment result, as shown in fig. 8, the open-circuit potential in the catalytic system is obviously enhanced, which indicates that the oxidation capability in the catalytic system is enhanced, in addition, a GOP experiment system is constructed, the instantaneous current in the catalytic system and the non-catalytic system is compared, and the result in fig. 9 indicates that the instantaneous current intensity in the catalytic system is increased, which indicates that the single electron transfer process in the catalyst experiment group is enhanced.
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| CN116139849A (en) * | 2023-02-06 | 2023-05-23 | 河海大学 | Method for degrading organic pollutants by photocatalytic production of high-valence iron species |
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| US4062772A (en) * | 1976-04-01 | 1977-12-13 | Phillips Petroleum Company | Polluted water purification |
| US20030143030A1 (en) * | 2002-01-30 | 2003-07-31 | Richard Greenberg | Method of treating contaminants in an in situ environment |
| RU2595343C2 (en) * | 2014-12-16 | 2016-08-27 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Дальневосточный государственный университет путей сообщения" (ДВГУПС) | Method of producing photocatalyst based on bismuthate alkali-earth metal and method of purifying water from organic contaminants using photocatalyst |
| CN107531533A (en) * | 2015-03-16 | 2018-01-02 | 水科技有限公司 | The method and apparatus for handling water |
| CN109731605B (en) * | 2019-02-28 | 2021-11-09 | 哈尔滨工业大学 | Metal composite in-situ nitrogen-doped carbon microsphere catalyst and application thereof |
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| CN116139849A (en) * | 2023-02-06 | 2023-05-23 | 河海大学 | Method for degrading organic pollutants by photocatalytic production of high-valence iron species |
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| 氢氧化铋的制备及性能研究;赵青燕等;《化学研究与应用》;20160131;第28卷(第1期);第83-88页 * |
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