CN112067563A - Method for activating hydrogen peroxide to oxidize As (III) by using cobalt bicarbonate complex and detection method - Google Patents

Method for activating hydrogen peroxide to oxidize As (III) by using cobalt bicarbonate complex and detection method Download PDF

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CN112067563A
CN112067563A CN202010955258.2A CN202010955258A CN112067563A CN 112067563 A CN112067563 A CN 112067563A CN 202010955258 A CN202010955258 A CN 202010955258A CN 112067563 A CN112067563 A CN 112067563A
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iii
hydrogen peroxide
mixture
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bicarbonate complex
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刘勇
吴佳璇
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Tianjin University of Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • 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
    • 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
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • 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
    • C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
    • 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
    • C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
    • G—PHYSICS
    • G01—MEASURING; TESTING
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • 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
    • C02F2101/103—Arsenic compounds

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Abstract

A method for activating oxidation of As (III) by hydrogen peroxide by a cobalt bicarbonate complex, comprising the steps of: step 1: preparation of NaHCO3A stock solution; step 2: configuration of CoCl2A stock solution; and step 3: adding NaHCO to As (III) -containing material3A stock solution; and 4, step 4: adding distilled water to the mixture of step 3; and 5: adding hydrochloric acid and/or NaOH solution into the mixture obtained in the step 4 to adjust the pH value; step 6: mixing the obtained product in the step 5Placing the compound in a constant temperature environment; and 7: adding CoCl to the mixture of step 6 in sequence2Stock solution and 30% H2O2And carrying out constant-temperature reaction to complete oxidation.

Description

Method for activating hydrogen peroxide to oxidize As (III) by using cobalt bicarbonate complex and detection method
Technical Field
The invention belongs to the technical field of water treatment, is suitable for treating trivalent arsenic in wastewater or underground water, and particularly relates to a method for activating hydrogen peroxide by a cobalt bicarbonate complex to oxidize As (III) and a detection method.
Background
The existing treatment method of high-arsenic underground water mainly comprises the following steps: adsorption, ion exchange and membrane separation.
(1) Adsorption process
The adsorption method uses iron-aluminum oxide, modified zeolite, activated carbon, resin, and various natural minerals, and uses the high specific surface area characteristics of these insoluble materials to fix arsenic on the surface of the adsorbent by physical adsorption, chemical adsorption, and other mechanisms, thereby removing arsenic.
(2) Ion exchange process
The ion exchange method has the advantages of simple operation, good removal effect and the like, and the method uses the anion exchange resin to realize the high-efficiency removal of arsenic. Because the ion exchange column has the defects of high cost, complex manufacturing process, complex regeneration and the like, the ion exchange column is more suitable for treating wastewater with high recovery value, low arsenic content and small treatment capacity.
(3) Membrane separation process
Membrane separation methods utilize the selective permeability of the membrane itself to separate different ions or molecules. The specific processes of the membrane separation method can be classified into microfiltration, ultrafiltration, nanofiltration and reverse osmosis, wherein the processes commonly used in high-arsenic groundwater treatment are nanofiltration and reverse osmosis. The method has the advantages of no secondary pollution, low cost, high investment and complex management.
Disclosure of Invention
In the high-arsenic underground water treatment process, As (III) is usually pre-oxidized by using oxidants such As ozone, potassium permanganate, chlorine dioxide, hypochlorous acid, a fenton reagent, hydrogen peroxide, manganese dioxide and the like, and in a weakly alkaline underground water environment, partial methods such As the fenton reagent and the like have low treatment efficiency. And CoIIThe BAP system can still maintain higher oxidation activity under the weak alkaline condition. However, to date, CoIIThe BAP system oxidizes As (III) and its mechanism has not been disclosed.
Based on the technical problems, the invention provides a method for oxidizing As (III) by hydrogen peroxide activated by a cobalt bicarbonate complex in order to realize efficient oxidation of As (III) in an alkaline environment. The adopted specific technical scheme is as follows:
a method for activating oxidation of As (III) by hydrogen peroxide by a cobalt bicarbonate complex, comprising the steps of:
step 1: preparation of NaHCO3A stock solution;
step 2: configuration of CoCl2A stock solution;
and step 3: adding NaHCO to As (III) -containing material3A stock solution;
and 4, step 4: adding distilled water to the mixture of step 3;
and 5: adding hydrochloric acid or NaOH solution into the mixture obtained in the step 4 to adjust the pH value;
step 6: putting the mixture obtained in the step 5 into a constant temperature environment;
and 7: adding CoCl to the mixture of step 6 in sequence2Stock solution and 30% H2O2And reacting in a constant temperature environment to complete the oxidation of As (III).
Further, NaHCO as described in step 13The stock solution had a concentration of 2M.
Further, CoCl as described in step 22The stock solution concentration was 10 mM.
Further, the material containing As (III) in the step 3 is in a solution state.
Further, step 3 said As (III) material is mixed with NaHCO3The volume ratio of the stock solution is 1: 15.
further, the volume ratio of the mixture in the step 4 to the distilled water is 3: 1.
further, the pH value is adjusted to 6-11 in the step 5.
Further, the constant temperature environment in step 6 and step 7 is a constant temperature water bath oscillator.
Further, the reaction time in the constant temperature environment in the step 6 is 20-30 minutes.
Further, CoCl as described in step 72The stock solution was added in an amount of 30% H to 1 ‰ of the volume of the mixture2O2Is added in an amount of 2% by volume of the mixture.
The method can effectively oxidize As (III) into As (V), and in order to efficiently test As (III) of the method, the following detection method is specially designed:
in the detection method, a molybdate color development method is adopted for the As (V) analysis method. The reagents used included: firstly, ascorbic acid solution; ammonium molybdate solution; ③ antimony potassium tartrate solution; sulfuric acid solution; 11% hydrochloric acid solution.
Firstly, preparing a color developing agent: according to the weight ratio of ammonium molybdate: sulfuric acid: antimony potassium tartrate: ascorbic acid 6: 5: 1: 2, mixing the ammonium molybdate and the sulfuric acid, and mixing the antimony potassium tartrate and the ascorbic acid in two beakers according to the ratio, and quickly pouring the mixed solution of the ammonium molybdate and the sulfuric acid into the mixed solution of the antimony potassium tartrate and the ascorbic acid after the ammonium molybdate and the sulfuric acid are uniformly mixed to finally obtain a light yellow green clear solution, wherein the solution is the color developing agent.
Secondly, the samples treated by the method of the invention are sampled, and H is added2O2After that, 0.5mL of the sample was taken when the reaction proceeded for 1, 5, 10, 20, 30, 60 and 120 minutes, and each sample was analyzed for As (V) content rapidly to reduce the effect of the reaction continuing on the experimental results.
Finally, the detection method comprises the following steps: 0.5mL of the sample was diluted 10-fold by adding to 4.5mL of water; adding 0.5mL of 11% hydrochloric acid into the diluted sample, shaking and shaking uniformly; then, quickly adding 0.5mL of prepared color developing agent into the sample, shaking up the mixture by shaking, and standing the mixture for 1 hour; measuring absorbance of the sample at a wavelength λ 880nm using a spectrophotometer; the as (v) concentration in the sample was calculated from the concentration-absorbance standard curve.
Control experiments were designed according to the above detection method, as shown in FIG. 1, in HCO alone3 -,H2O2,Co2+The degradation effect of either or both substances is other than that of HCO3-+H2O2All others are not ideal, and HCO3-+H2O2Although the degradation efficiency is high, the degradation speed is slow, and in HCO3 -+H2O2+Co2+In the system, the degradation efficiency and rate are high.
As for the influence of pH, as shown in fig. 2, the optimum reaction condition was selected to be pH 8.5, because the degradation efficiency reached 90% or more, the reaction rate was the fastest and the degradation rate reached 97% at pH 8 (6 to 11), and the degradation rate reached 97% even at pH 8.5, which is the initial pH of the reaction.
As for the effect of Co ion concentration, as shown in FIG. 3, the reaction rate gradually increased with the increase of Co ion concentration (0.05mM-0.4mM), the degradation rate was almost unchanged, and 0.2mM was selected as the optimum reaction concentration for economic reasons.
With respect to H2O2Influence of concentration, as in FIG. 4, with H2O2The reaction rate gradually increased with increasing concentration (1mM-15mM), and the degradation rate increased from 87% to 97%, and for economic reasons we chose 10mM as the reaction concentration.
With respect to HCO3 -Effect of concentration, as shown in FIG. 5, with HCO3 -As the concentration (0.05mM-0.4mM) was increased, the reaction rate was gradually increased and the degradation rate was almost unchanged, and for economic reasons, we selected 0.2mM as the reaction concentration.
For the consideration of economic benefit and degradation effect, the optimal parameter scheme of the method is as follows: pH 8.5, Co2+＝0.2mM,H2O2＝10mM,HCO3 -＝0.2mM。
The method has the advantages that: in high-arsenic groundwater, As (iii) is usually pre-oxidized by using oxidants such As ozone, potassium permanganate, chlorine dioxide, hypochlorous acid, fenton reagent, hydrogen peroxide, manganese dioxide and the like, and in alkalescent groundwater environment, partial methods such As fenton reagent and the like have lower treatment efficiency, while the Mn (manganese) provided by the invention is low in treatment efficiencyIIThe BAP system can still keep higher oxidation activity under the alkalescent condition, the conversion rate of arsenic by methods such as Fenton reagent and the like can only reach about sixty percent and the time consumption is basically more than one hour, but the method can completely convert the arsenic within 10 minutes and has extremely high economic value and practicability.
Drawings
FIG. 1 is an analysis chart of a control experiment of the present invention
FIG. 2 is a graph showing the effect of pH on the method of the present invention
FIG. 3 is a diagram showing the effect of Co ion concentration on the method of the present invention
FIG. 4 shows a process H according to the invention2O2Analysis chart of influence of concentration on effect of method
FIG. 5 shows HCO in the process of the invention3 -Analysis chart of influence of concentration on effect of method
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the following detailed description of the invention is further explained, but not limiting the protection scope of the invention.
First, a 250mL Erlenmeyer flask was taken and the volume of the flask was adjusted according to 1: 15 of NaHCO3Stock and As (iii) stock, the solution volume was increased to 198mL using distilled water, and the erlenmeyer flask solution pH was subsequently adjusted to the experimental pH using 0.1M hydrochloric acid and 0.1M NaOH. Placing the conical flask into a constant-temperature water bath oscillator to preheat for 30 minutes, and then sequentially adding CoCl with the volume of 1 per mill of the existing solution into the conical flask2Stock and existing solution 2% by volume 30% H2O2And starting the constant-temperature water bath oscillator to vibrate. From the addition of H2O2Immediately thereafter, the timer was started. When the reaction proceeded for 1, 5, 10, 20, 30, 60, 90 and 120 minutes, 0.5mL of sample was taken from the flask using a pipette and analyzed for As (V) content rapidly to reduce the effect of the reaction proceeding on the experimental results. 0.5mL of the sample was diluted 10-fold with 4.5mL of water, and 0.5mL of 11% hydrochloric acid was added to the diluted sample, followed by shaking. Then, 0.5mL of the prepared color developing agent is rapidly added into the sample, shaken up and kept stand for 1 h. The absorbance of the sample was measured using a spectrophotometer at a wavelength λ 880 nm.
The results of sampling at different times show that the arsenic conversion is already as high as 90% at 1 minute and that complete conversion of arsenic is achieved at 5 minutes, indicating that the process according to the invention has a very fast reaction rate.
The method for activating the oxidation of As (III) by hydrogen peroxide with a cobalt bicarbonate complex according to the invention has been described by way of specific examples. The technical personnel can use the content of the invention to change the process flow or the process parameters and other links appropriately to realize other corresponding purposes, and the related changes do not depart from the content of the invention, and any modification, equivalent replacement, improvement and the like made within the spirit and the principle of the invention are all included in the protection scope of the invention.

Claims (10)

1. A method for activating oxidation of As (III) by hydrogen peroxide by a cobalt bicarbonate complex, comprising the steps of:
step 1: preparation of NaHCO3A stock solution;
step 2: configuration of CoCl2A stock solution;
and step 3: adding NaHCO to As (III) -containing material3A stock solution;
and 4, step 4: adding distilled water to the mixture of step 3;
and 5: adding hydrochloric acid or NaOH solution into the mixture obtained in the step 4 to adjust the pH value;
step 6: putting the mixture obtained in the step 5 into a constant temperature environment;
and 7: adding CoCl to the mixture of step 6 in sequence2Stock solution and 30% H2O2And reacting in a constant temperature environment to complete the oxidation of As (III).
2. The method for activating oxidation of As (III) by hydrogen peroxide with cobalt bicarbonate complex As claimed in claim 1, wherein said NaHCO is used in step 13The stock solution had a concentration of 2M.
3. The method for activating oxidation of As (III) by hydrogen peroxide through cobalt bicarbonate complex As claimed in claim 1, wherein the CoCl in step 2 is2The stock solution concentration was 10 mM.
4. According to claimThe method for oxidizing As (III) by hydrogen peroxide through a cobalt bicarbonate complex As claimed in claim 1, wherein the As (III) -containing material in step 3 is in a solution state, and the As (III) -containing material is mixed with NaHCO3The volume ratio of the stock solution is 1: 15.
5. the method for activating oxidation of As (III) by hydrogen peroxide through cobalt bicarbonate complex As claimed in claim 4, wherein the volume ratio of the mixture in step 4 to distilled water is 3: 1.
6. the method for activating oxidation of As (III) by hydrogen peroxide through a cobalt bicarbonate complex As claimed in claim 1, wherein the pH in step 5 is adjusted to 6-11.
7. The method for activating oxidation of As (III) by hydrogen peroxide through a cobalt bicarbonate complex As claimed in claim 1, wherein the constant temperature environment in step 6 and step 7 is a constant temperature water bath oscillator.
8. The method for activating oxidation of As (III) by hydrogen peroxide through cobalt bicarbonate complex As claimed in claim 1, wherein the reaction time in step 6 is 20-30 minutes at constant temperature.
9. The method of claim 4, wherein the CoCl in step 7 is used As a catalyst for oxidizing As (III) with hydrogen peroxide via a cobalt bicarbonate complex2The stock solution was added in an amount of 30% H to 1 ‰ of the volume of the mixture2O2Is added in an amount of 2% by volume of the mixture.
10. A method of measuring the conversion of As (iii) material in a method according to any of claims 1 to 9, comprising the steps of:
step 1: according to the weight ratio of ammonium molybdate: sulfuric acid: antimony potassium tartrate: ascorbic acid 6: 5: 1: 2, preparing a color developing agent according to the volume ratio of the solution;
step 2: sampling 0.5mL of the sample treated by the method of claims 1-9;
and step 3: adding 4.5mL of water to the 0.5mL of sample obtained in the step 2 for dilution;
and 4, step 4: adding 0.5mL of 11% hydrochloric acid into the diluted sample, shaking and shaking uniformly;
and 5: adding 0.5mL of the color developing agent prepared in the step 1 into the sample treated in the step 4, shaking up the mixture by shaking, and standing the mixture for 1 hour;
step 6: the absorbance of the sample treated in step 5 was measured at a wavelength λ 880nm using a spectrophotometer, and the as (v) concentration in the sample was calculated from the concentration-absorbance standard curve.
CN202010955258.2A 2020-09-11 2020-09-11 Method for activating hydrogen peroxide to oxidize As (III) by using cobalt bicarbonate complex and detection method Pending CN112067563A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1675525A (en) * 2002-08-21 2005-09-28 纽约市哥伦比亚大学托管会 An arsenic meter
CN101788495A (en) * 2010-01-29 2010-07-28 白银有色集团股份有限公司 Method for measuring arsenic by iodine solution absorption method
CN107449744A (en) * 2017-07-14 2017-12-08 纤化（上海）生物化工股份有限公司 The analysis method of activity of catalase in a kind of detection textile printing and dyeing industry
CN111175270A (en) * 2020-02-11 2020-05-19 道道全粮油股份有限公司 Method for detecting trace arsenic in vegetable oil by extraction and dry ashing atomic fluorescence

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1675525A (en) * 2002-08-21 2005-09-28 纽约市哥伦比亚大学托管会 An arsenic meter
CN101788495A (en) * 2010-01-29 2010-07-28 白银有色集团股份有限公司 Method for measuring arsenic by iodine solution absorption method
CN107449744A (en) * 2017-07-14 2017-12-08 纤化（上海）生物化工股份有限公司 The analysis method of activity of catalase in a kind of detection textile printing and dyeing industry
CN111175270A (en) * 2020-02-11 2020-05-19 道道全粮油股份有限公司 Method for detecting trace arsenic in vegetable oil by extraction and dry ashing atomic fluorescence

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ZI-HE MENG ET AL.: "Formation and Oxidation Reactivity of MnO2+(HCO3−)n in the MnII(HCO3−)−H2O2 System", INORGANIC CHEMISTRY, vol. 59, no. 5, pages 3172 - 3180 *
何健;: "三价砷的检测", 当代化工, no. 05 *

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