CN110697869A - Low-ferrous-dosage composite Fenton reagent and method for degrading organic pollutants by using same - Google Patents
Low-ferrous-dosage composite Fenton reagent and method for degrading organic pollutants by using same Download PDFInfo
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
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- C02F2101/32—Hydrocarbons, e.g. oil
- C02F2101/327—Polyaromatic Hydrocarbons [PAH's]
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- C02F2101/36—Organic compounds containing halogen
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The invention discloses a low-ferrous-dosage composite Fenton reagent and a method for degrading organic pollutants by using the same, wherein the composite Fenton reagent consists of a low-dosage ferrous solution, biochar prepared by high-temperature pyrolysis and a hydrogen peroxide aqueous solution, and the dosage of the biochar is 1-9 g.L‑1The dosage of the ferrous solution is 0.05-0.9 mg.L calculated by Fe‑1With H2O2The dosage of the hydrogen peroxide aqueous solution is 2-15 mmol.L‑1. The method for degrading organic pollutants based on the reagent has obvious effect on treating organic wastewater containing chlorinated organic compounds, antibiotics, aromatic compounds and the like. In the reagents and methods of the inventionThe dosage of the ferrous iron used is far lower than that of the conventional Fenton system, so that the concentration of residual iron in water can be effectively reduced, and the generation of iron sludge is reduced or even avoided.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a low-ferrous-dosage composite Fenton reagent and a method for degrading organic pollutants by using the same.
Background
The problem of water environment pollution becomes an important restriction factor for the urbanization process and the development of industrial and agricultural production. Some organic pollutants which are difficult to be biodegraded such as chlorinated organic compounds,Antibiotics, aromatic compounds and the like are gradually accumulated after entering the water body, and further harm plants, microorganisms and human health. Advanced oxidation technologies, represented by Fenton (Fenton) oxidation technology, can convert these contaminants into small acids that are more readily biodegradable, and even completely mineralize to carbon dioxide (CO)2) And water (H)2O), and the like. Ferrous salt and hydrogen peroxide (H) are utilized in Fenton oxidation technology2O2) The combined series of reactions generate hydroxyl radicals (. OH) with strong oxidizing property (standard redox potential of 2.8V), and can degrade organic pollutants through dechlorination, hydroxylation, ring opening, chain scission and other reactions. Compared with other advanced oxidation technologies, the Fenton oxidation technology has the advantages of high oxidation efficiency, high reaction speed, no selectivity, low cost and the like, so that the Fenton oxidation technology becomes an important method for treating refractory organic pollutants.
One of the keys to the Fenton (or Fenton-like) oxidation technology is the continuous generation of OH (reaction (1)) to ensure the gradual conversion of contaminants of relatively large molecular mass to CO2And H2O and other small molecular compounds. Ferric ion (Fe) generated by reaction (1)3+) To ferrous ion (Fe)2+) The conversion rate of (2) is relatively slow, and the dosage of the iron salt used in the Fenton reagent is usually 1 mmol.L to increase the degradation rate of the pollutants-1(56 mg. L in terms of Fe dose)-1) The above. The dosage is far higher than 10 mg.L specified in GB/T31962-2015 water quality standard for discharging sewage into urban sewer-1And (4) limiting values. Therefore, in the case of organic wastewater treatment using fenton oxidation, it is generally necessary to adjust pH after the reaction and precipitate and remove excessive ferric (fe (iii)) or ferrous (fe (ii)) in the wastewater, thereby causing the generation of a large amount of iron sludge. To reduce sludge production, there have been studies (Chemosphere,58(2005)1409-1414.DOI 10.1016/j. Chemosphere.2004.09.091) that attempted to control the ferrous salt concentration to 10 mg.L-1However, the composition is effective only on contaminants easily oxidized such as azo dyes and the like in the absence of other auxiliary agents, and 10 mg.L-1The dosage of the composition still far exceeds 0.3 mg.L specified in GB5749-2006 sanitary Standard for Drinking Water-1And (4) limiting values. Therefore, to reduce the Fenton oxidation technologyThe subsequent treatment process of the technology reduces the treatment cost of pollutants, and controls the content of ferric salt in sewage at the same time, so that a novel Fenton oxidation system with low ferrous dosage needs to be developed.
Fe2++H2O2→Fe3++OH-+·OH (1)
Biochar is a carbon-containing solid obtained by pyrolysis treatment of biomass under oxygen-limited conditions. The biochar has wide raw material source and low production cost, and has wide prospect in the fields of pollution control, soil remediation, carbon sequestration, emission reduction and the like. The biochar prepared by pyrolysis at high temperature (650-850 ℃) has high graphitization degree and stable property, and is an ideal catalyst carrier and adsorbent. Recent researches show that the biochar has stronger electron transport capacity and can promote the conversion of Fe (III) to Fe (II) in a Fenton-like reaction system (ACSAppl. Mater. Interf.9(2017)17115-17124.DOI:10.1021/acsami.7b03310), but the dosage of Fe in the system is 0.4 mmol.L-1(22.4 mg. L. in terms of Fe dose)-1). Meanwhile, the inventor also finds that the quinone-hydroquinone group on the biochar has stronger capability of stabilizing free radicals and can improve H2O2Efficiency of decomposition to OH. Therefore, by utilizing the catalysis promoting functions of the biochar and combining with the Fenton reagent, the organic pollutants can be removed by oxidation under the condition of low iron dosage.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a composite Fenton reagent with low ferrous dosage and a method for degrading organic pollutants by using the composite Fenton reagent, wherein the ferrous dosage used in the reagent and the method is far lower than that of a conventional Fenton system, the residual iron concentration in water can be effectively reduced, and the generation of iron sludge is reduced or even avoided.
In order to achieve the purpose, the invention adopts the following technical scheme:
a low ferrous dosage composite Fenton reagent is prepared from low dosageThe carbon-containing biological carbon comprises a ferrous solution, biological carbon prepared by high-temperature pyrolysis and a hydrogen peroxide aqueous solution, wherein the dosage of the biological carbon is 1-9 g.L-1The dosage of the ferrous solution is 0.05-0.9 mg.L calculated by Fe-1With H2O2The dosage of the hydrogen peroxide aqueous solution is 2-15 mmol.L-1。
The ferrous solution is ferrous sulfate or ferrous chloride water solution.
The dosage of the ferrous solution is 0.1-0.35 mg.L-1。
The biochar is a solid obtained by pyrolyzing biomass rich in lignin, cellulose and hemicellulose at 650-850 ℃ for 1-6 hours.
The biochar is obtained by soaking a pyrolyzed solid in water for 24 hours and then drying in vacuum, and the catalytic performance of the biochar can be improved by soaking and drying.
The raw materials of the biochar are wood chips, rice straws, wheat straws or corn straws.
The method for degrading organic pollutants by using the low-ferrous-dosage composite Fenton reagent comprises the following steps of: sequentially adding a biochar solution and a ferrous solution into wastewater containing organic pollutants, adjusting the pH to 3-4, stirring and mixing for 5-30 min, adding a hydrogen peroxide aqueous solution, and reacting for 120-360 min; wherein the dosage of the biochar is 1-9 g.L-1The dosage of the ferrous solution is 0.05-0.9 mg.L calculated by Fe-1With H2O2The dosage of the hydrogen peroxide aqueous solution is 2-15 mmol.L-1。
The organic contaminants are organic contaminants such as chlorinated organic compounds, antibiotics, aromatic compounds, and the like, which are hardly degraded by microorganisms.
Compared with the prior Fenton oxidation technology, the technical scheme provided by the invention has the following advantages and characteristics:
(1) the biochar obtained by high-temperature pyrolysis has a developed pore structure, and can promote the enrichment of organic pollutants in the wastewater to a solid-liquid phase reaction interface, so that the Fenton oxidation reaction of the pollutants is accelerated.
(2) Raw material obtained by high-temperature pyrolysisThe charcoal has strong electron transfer and free radical stabilizing ability, and can promote the conversion of Fe (III) to Fe (II) and increase H2O2Efficiency of decomposition to OH.
(3) The dosage of the used ferrous iron is far lower than that of the conventional Fenton oxidation system, so that the content of free iron in water can be obviously reduced, and the generation and subsequent treatment of iron sludge are reduced or even avoided.
(4) The composite Fenton reagent is suitable for the oxidative degradation of organic pollutants such as chlorinated organic compounds, antibiotics and aromatic compounds which are difficult to biodegrade, and can be used for the advanced treatment of wastewater containing the organic pollutants; can also be combined with wastewater treatment technologies such as biodegradation and the like for the early-stage treatment of wastewater containing organic pollutants; and the organic pollutant can be further enhanced by combining with auxiliary means such as illumination, electrochemistry, ultrasonic waves and the like.
Detailed Description
The invention is further described below with reference to specific embodiments:
examples 1 to 8:
the composite Fenton reagent consists of a low-dose ferrous solution, biochar prepared by high-temperature pyrolysis and an aqueous hydrogen peroxide solution, and different compositions of the composite Fenton reagent are specifically shown in Table 1.
TABLE 1 composition of the complex Fenton reagent
Example 9
According to the composition of the composite Fenton's reagent given in example 1, 1g of biochar and 2mL of Fe content 50 mg.L were sequentially added-1Adding the ferrous sulfate aqueous solution into 1L of wastewater containing 50mg of chlorobenzene, and adding the ferrous sulfate aqueous solution into the wastewater at a concentration of 1.0 mol.L-1Adjusting the pH value of the sulfuric acid solution to 3, stirring and mixing for 20min, and adding the sulfuric acid solution with the concentration of 1 mol.L-1The reaction was started with 2mL of aqueous hydrogen peroxide solution and allowed to react for 360 min. The content of the residual chlorobenzene in the wastewater after the sampling analysis reaction is 3.3 mg.L-1The chlorobenzene removal rate was calculated to be 93%. Sampling and analyzing chloride ions in wastewater after reactionThe content is 14.3 mg.L-1Corresponding to 90% of the dechlorination amount of the chlorobenzene after being completely degraded. It is shown that chlorobenzene is degraded rather than adsorbed in the composite Fenton reaction system. The content of free total iron in the wastewater after sampling analysis reaction is 0.09 mg.L-1Is lower than the limit value (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water for iron content in Water-1)。
Example 10
According to the composition of the composite Fenton reagent given in example 2, 5g of biochar and 6mL of Fe content 50 mg.L are sequentially added-1Adding the ferrous sulfate aqueous solution into 1L of wastewater containing 100mg of chlorobenzene, and adding the ferrous sulfate aqueous solution into the wastewater with the concentration of 1.0 mol.L-1Adjusting the pH value of the sulfuric acid solution to 3, stirring and mixing for 20min, and adding the sulfuric acid solution with the concentration of 1 mol.L-1The reaction was started with 5mL of aqueous hydrogen peroxide solution and allowed to react for 240 min. The content of the residual chlorobenzene in the wastewater after the sampling analysis reaction is 2.6 mg.L-1The chlorobenzene removal rate was calculated to be 97%. The content of chloride ions in the wastewater after the sampling analysis reaction is 29.2 mg.L-1This corresponds to 92% of the dechlorinated content of chlorobenzene after its complete degradation. It is shown that chlorobenzene is degraded rather than adsorbed in the composite Fenton reaction system. The content of free total iron in the wastewater after sampling analysis reaction is 0.25 mg.L-1Is lower than the limit value (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water for iron content in Water-1)。
Example 11
According to the composition of the composite Fenton reagent given in example 3, 9g of biochar and 6mL of Fe content 100 mg.L are sequentially added-1Adding the ferrous sulfate aqueous solution into 1L of wastewater containing 150mg of chlorobenzene, and adding the ferrous sulfate aqueous solution into the wastewater with the concentration of 1.0 mol.L-1Adjusting pH to 3.5, stirring and mixing for 15min, adding 1 mol. L-1The reaction was started with 10mL of aqueous hydrogen peroxide solution and allowed to react for 180 min. The content of the residual chlorobenzene in the wastewater after the sampling analysis reaction is 2.0 mg.L-1The chlorobenzene removal rate was calculated to be 99%. The content of chloride ions in the wastewater after sampling analysis reaction is 45.0 mg.L-1Corresponding to 95% of the dechlorination amount after the chlorobenzene is completely degraded. The compound Fenton reaction bodyIn this system, chlorobenzene is degraded rather than adsorbed. The content of free total iron in the wastewater after sampling analysis reaction is 0.53 mg.L-1Higher than the limit value (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water for iron content in Water-1) But far below 10 mg.L specified in GB/T31962-2015 water quality Standard for wastewater discharge into urban sewer-1And (4) limiting values.
Example 12
According to the composition of the composite Fenton's reagent given in example 4, 2g of biochar and 4mL of Fe content 50 mg.L were sequentially added-11L of the ferrous chloride aqueous solution of 70 mg.L of Chemical Oxygen Demand (COD)-1The antibiotic wastewater of (1.0 mol. L) is added-1Adjusting the pH value of the sulfuric acid solution to 3, stirring and mixing for 30min, and adding the sulfuric acid solution with the concentration of 1 mol.L-1The reaction was started with 5mL of aqueous hydrogen peroxide solution and allowed to react for 240 min. The COD content in the wastewater after the sampling analysis reaction is 15 mg.L-1The allowable discharge concentration (50 mg. L) is lower than the first class A standard in GB18918-2002 discharge Standard of pollutants for municipal wastewater treatment plants-1) And calculating to obtain the COD removal rate of the antibiotic wastewater to be 78%. The content of free total iron in the wastewater after sampling analysis reaction is 0.17 mg.L-1Is lower than the limit value (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water for iron content in Water-1)。
Example 13
According to the composition of the composite Fenton reagent given in example 5, 6g of biochar and 9mL of Fe content 100 mg.L are sequentially added-11L of the ferrous chloride aqueous solution of (1) Chemical Oxygen Demand (COD) of 220 mg. L is added-1The antibiotic wastewater of (1.0 mol. L) is added-1Adjusting the pH value of the sulfuric acid solution to be 4, stirring and mixing for 25min, and adding the sulfuric acid solution with the concentration of 1 mol.L-1The reaction was started with 15mL of aqueous hydrogen peroxide solution and allowed to react for 120 min. The COD content in the wastewater after sampling analysis reaction is 31 mg.L-1The allowable discharge concentration (50 mg. L) is lower than the first class A standard in GB18918-2002 discharge Standard of pollutants for municipal wastewater treatment plants-1) And calculating to obtain the COD removal rate of the antibiotic wastewater to be 86%. Sampling and analyzing free total in waste water after reactionThe iron content is 0.79 mg.L-1Higher than the limit value (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water for iron content in Water-1) But far below 10 mg.L specified in GB/T31962-2015 water quality Standard for wastewater discharge into urban sewer-1And (4) limiting values.
Example 14
According to the composition of the composite Fenton reagent given in example 6, 8g of biochar and 7mL of Fe with the content of 50 mg.L are sequentially added-1Adding 1L of ferrous chloride aqueous solution with Chemical Oxygen Demand (COD) of 150 mg.L-1The antibiotic wastewater of (1.0 mol. L) is added-1Adjusting the pH value of the sulfuric acid solution to 3, stirring and mixing for 15min, and adding the sulfuric acid solution with the concentration of 1 mol.L-1The reaction was started with 6mL of aqueous hydrogen peroxide solution and allowed to react for 360 min. The COD content in the wastewater after sampling analysis reaction is 28 mg.L-1The allowable discharge concentration (50 mg. L) is lower than the first class A standard in GB18918-2002 discharge Standard of pollutants for municipal wastewater treatment plants-1) And calculating to obtain the COD removal rate of the antibiotic wastewater to be 81%. The content of free total iron in the wastewater after sampling analysis reaction is 0.30 mg.L-1Meets the limit value requirement (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water on the iron content in Water-1)。
Example 15
According to the composition of the composite Fenton's reagent given in example 7, 5g of biochar and 1mL of Fe content 50 mg.L were sequentially added-1Adding 1L of water solution of ferrous sulfate containing 75 mg.L of hydroquinone-1The wastewater of (2) is added to a concentration of 1.0 mol. L-1Adjusting the pH value of the sulfuric acid solution to 3, stirring and mixing for 10min, and adding the sulfuric acid solution with the concentration of 1 mol.L-1The reaction was started with 2mL of aqueous hydrogen peroxide solution and allowed to react for 360 min. The content of the hydroquinone remained in the wastewater after the sampling analysis reaction is 8.9 mg.L-1The calculated hydroquinone removal rate was 88%. The content of free total iron in the wastewater after sampling analysis reaction is 0.05 mg.L-1Is lower than the limit value (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water for iron content in Water-1)。
Example 16
According to the composition of the composite Fenton's reagent given in example 8, 5g of biochar and 4mL of Fe content 100 mg.L were sequentially added-1Adding 1L of water solution of ferrous sulfate containing 75 mg.L of hydroquinone-1The wastewater of (2) is added to a concentration of 1.0 mol. L-1Adjusting the pH value of the sulfuric acid solution to 3, stirring and mixing for 5min, and adding the sulfuric acid solution with the concentration of 1 mol.L-1The reaction was started with 6mL of aqueous hydrogen peroxide solution and allowed to react for 240 min. The content of hydroquinone remained in the wastewater after sampling analysis reaction is 0.5 mg.L-1The removal rate of hydroquinone was calculated to be 99%. The content of free total iron in the wastewater after sampling analysis reaction is 0.32 mg.L-1Higher than the limit value (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water for iron content in Water-1) But far below 10 mg.L specified in GB/T31962-2015 water quality Standard for wastewater discharge into urban sewer-1And (4) limiting values.
Examples 9 to 16 above illustrate that, when the amount of ferrous iron in the composite Fenton reagent is 0.1 to 0.35 mg.L-1The removal rate of organic pollutants in the wastewater is more than 90 percent, and the content of free total iron in the solution meets the limit requirement (0.3 mg. L) of GB5749-2006 sanitary Standard for Drinking Water on the content of iron in water-1)。
Comparative examples 1 to 2
To further illustrate the effect of the low ferrous dose in the composite fenton reagent, the two lowest ferrous dose reagent combinations of example 1 and example 7 were reacted for 360min without ferrous iron according to the methods described in example 9 and example 15, respectively, under otherwise identical conditions. The removal rate of chlorobenzene and hydroquinone in the wastewater after the sampling analysis reaction is only 45% and 38%, which are obviously lower than the removal rate (93% and 88%) in the example 9 and the example 15. The ferrous iron in the composite Fenton reagent is H2O2Decomposition to produce·OH in turn oxidatively degrades the main active component of organic pollutants.
Comparative examples 3 to 4
To further illustrate the effect of biochar in the complex fenton reagent, the reactions were performed under otherwise identical conditions in the two highest ferrous dose reagent combinations of example 3 and example 5, without adding biochar, according to the methods described in example 11 and example 13, respectively. The removal rate of COD in the wastewater after sampling and analyzing reaction is only 26% and 33%, which are obviously lower than the removal rate (99% and 86%) in the example 11 and the example 13. The biological carbon in the composite Fenton reagent is an important component for promoting the oxidative degradation of organic pollutants.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A low ferrous dose composite Fenton's reagent, characterized in that: the composite Fenton reagent is composed of a low-dose ferrous solution, biochar prepared by high-temperature pyrolysis and a hydrogen peroxide aqueous solution, wherein the using amount of the biochar is 1-9 g.L-1The dosage of the ferrous solution is 0.05-0.9 mg.L calculated by Fe-1With H2O2The dosage of the hydrogen peroxide aqueous solution is 2-15 mmol.L-1。
2. A low ferrous dose composite fenton reagent according to claim 1 wherein: the ferrous solution is ferrous sulfate or ferrous chloride water solution.
3. A low ferrous dose composite fenton reagent according to claim 1 wherein: the dosage of the ferrous solution is 0.1-0.35 mg.L-1。
4. A low ferrous dose composite fenton reagent according to claim 1 wherein: the biochar is a solid obtained by pyrolyzing biomass rich in lignin, cellulose and hemicellulose at 650-850 ℃ for 1-6 hours.
5. A low ferrous dose of composite Fenton's reagent according to claim 4 wherein: the biochar is obtained by soaking a solid after pyrolysis in water for 24 hours and then drying in vacuum.
6. A low ferrous dose of composite Fenton's reagent according to claim 5 wherein: the raw materials of the biochar are wood chips, rice straws, wheat straws or corn straws.
7. The method for degrading organic pollutants by using the low-ferrous-dosage composite Fenton's reagent according to any one of claims 1 to 6, wherein the method comprises the following steps: the method comprises the following steps: sequentially adding a biochar solution and a ferrous solution into wastewater containing organic pollutants, adjusting the pH to 3-4, stirring and mixing for 5-30 min, adding a hydrogen peroxide aqueous solution, and reacting for 120-360 min; wherein the dosage of the biochar is 1-9 g.L-1The dosage of the ferrous solution is 0.05-0.9 mg.L calculated by Fe-1With H2O2The dosage of the hydrogen peroxide aqueous solution is 2-15 mmol.L-1。
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| WO2021227361A1 (en) * | 2020-05-09 | 2021-11-18 | 中国石油大学(华东) | Combined treatment method for petroleum contaminated soil |
| CN113800618A (en) * | 2021-09-08 | 2021-12-17 | 华中科技大学 | Method for improving efficiency of Fenton system by accelerating ferrous ion regeneration of biochar |
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| WO2021227361A1 (en) * | 2020-05-09 | 2021-11-18 | 中国石油大学(华东) | Combined treatment method for petroleum contaminated soil |
| US11292038B2 (en) | 2020-05-09 | 2022-04-05 | China University Of Petroleum | Combined treatment method of petroleum-contaminated soil |
| CN113800618A (en) * | 2021-09-08 | 2021-12-17 | 华中科技大学 | Method for improving efficiency of Fenton system by accelerating ferrous ion regeneration of biochar |
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