CN113461135A - Method for rapidly degrading azo dye orange II - Google Patents

Method for rapidly degrading azo dye orange II Download PDF

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CN113461135A
CN113461135A CN202110796297.7A CN202110796297A CN113461135A CN 113461135 A CN113461135 A CN 113461135A CN 202110796297 A CN202110796297 A CN 202110796297A CN 113461135 A CN113461135 A CN 113461135A
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solution
orange
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ultrasonic
persulfate
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李海波
何丁缘
徐银
李玉华
何文杰
钟锋
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Hubei University
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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
    • C02F1/725—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
    • C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
    • C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
    • 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
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • 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
    • 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
    • C02F2101/38—Organic compounds containing nitrogen
    • 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
    • C02F2101/40—Organic compounds containing sulfur
    • 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
    • C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a method for rapidly degrading azo dye orange II, which comprises the following steps: (1) weighing golden orange II powder, dissolving the golden orange II powder in deionized water to prepare a golden orange II solution with the concentration of 10mg/L, wherein the golden orange II solution is a target pollutant; (2) putting a beaker filled with 200mL of target pollutant into an ultrasonic machine, setting the frequency and the ultrasonic time of the ultrasonic machine, starting the ultrasonic machine, and adding potassium hydrogen persulfate into the pollutant to ensure that the concentration of persulfate in the solution is 1-3 mmol/L; (3) ascorbic acid and raw ore are added immediately after 30 seconds, so that the ascorbic acid concentration in the solution is 0.15-0.35mmol/L and the raw ore content is 1-3 g/L. The concentration of the persulfate in the solution was 2 mmol/L. The ascorbic acid concentration in the solution was 0.25 mmol/L. The crude ore content in the solution was 2 g/L. The concentration of the golden orange II contained in the target pollutant is 10 mg/L. The ultrasonic frequency is 40KHz, and the ultrasonic time is 60 min. Can quickly and effectively degrade the golden orange II solution.

Description

Method for rapidly degrading azo dye orange II
Technical Field
The invention relates to the technical field of water pollution control, in particular to a method for rapidly degrading azo dye orange II.
Background
With the continuous development of modern chemical industry, the number and types of chemically synthesized organic matters entering water bodies through various ways are increased rapidly, and serious pollution is caused to the water environment. In water treatment engineering, wastewater containing such substances is generally difficult to treat by biological methods, and conventional physical and chemical methods are difficult to meet the requirements of purification treatment technically and economically. With the progress of research, it has been found that such problems can be solved by using advanced oxidation techniques.
In the existing various advanced oxidation technology types, persulfate (S) is used2O8 2-，HSO5 -) The underlying advanced oxidation technology is receiving increasing attention. In general, persulfates can be activated by a variety of methods including ultrasonic, thermal, ultraviolet, basic, transition metal, etc., which decompose to produce SO4·-Is a strong oxidant, the oxidation-reduction potential is 2.5-3.1eV, and various organic pollutants (chlorophenol, trichlorobiphenyl, polycyclic aromatic hydrocarbon, methylene blue, methyl orange and the like) can be degraded. Furthermore, SO4·-Can react with water or hydroxyl to generate hydroxyl radical OH which is another strong oxidant and can oxidize or even mineralize various organic pollutants.
The advantages of the persulfate advanced oxidation technology are roughly divided into four points as follows: 1. the water solubility is good, and the existence time in water is long; SO4·-The service life is long, and mass transfer is facilitated; 3. is slightly influenced by pH and is suitable for a natural buffer system; 4. the final product is sulfuric acid, and no secondary pollution is caused.
According to related research, ascorbic acid is used as a common antioxidant and natural environment-friendly reducing agent for water solubilityThe vitamin can induce the activation of persulfate, and can promote the decomposition of H2O2 in Fenton system (forming. OH) or the decomposition of persulfate in Fe (III)/persulfate system (forming SO 4) by accelerating the Fe (III)/Fe (II) cycle·-) And the problems that the oxidation of Fe (II) into Fe (III) is difficult to regenerate and the persulfate reaction is limited by pH are overcome.
At present, a plurality of azo dyes processing technologies exist, but the azo dyes processing technologies have certain disadvantages correspondingly, such as the adsorption method generally has the disadvantages of large adsorbent dosage, low adsorption effect, poor regeneration capability and the like; biological methods generally have the defects of being easily influenced by external factors and the like; the membrane separation method generally has the defects of narrow application range and the like; the electrochemical method has the defects of high treatment cost and the like; the photocatalytic oxidation method has the defects of reducing the application range and the like due to the need of extra light.
The invention patent with application number 201910375175.3 discloses a method for degrading a gold orange II dye by using wood chip biochar activated persulfate prepared by high-temperature pyrolysis and application thereof, and discloses that the degradation rate of the gold orange II dye by using the method is 96% in 180 minutes, and the degradation rate of the gold orange II dye in the method is shown in figure 1.
A paper of bismuth ferrite visible light catalysis peroxymonosulfate for removing gold orange II published in chemical research and application 2019,31(05) discloses a more popular heterogeneous catalysis technology in recent years, for example, a heterogeneous catalyst bismuth ferrite is used for carrying out visible light catalysis peroxymonosulfate treatment on gold orange II dye wastewater, authors design the degradation efficiency of the system on gold orange II with different concentrations, and finally obtain a curve that when the initial concentration of the gold orange II is 10mg/L, the removal rate reaches 99.58% in 70 minutes, the concentration of PMS is 0.3mmol/L, the dosage of bismuth ferrite is 0.2g, and the removal effect changes along with time under the conditions of different initial concentrations of gold orange II solutions is shown in a graph 2.
The experiment is based on a mechanism of activating persulfate by ascorbic acid, raw ore is added to improve Fe (II) and increase reaction sites, the raw ore is from raw ore used for ironmaking in a certain yellow stone enterprise, an ultrasonic machine is of a Xinzhi SB-120DT type, the raw ore is used as a reaction catalyst, a cavitation phenomenon is generated in an ultrasonic environment, the capacity of degrading dye wastewater is enhanced by cooperating with the persulfate activated by the ascorbic acid, and the accelerated activation and oxidation process is not reported yet.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a solution to the above problem.
The technical scheme for solving the technical problems is as follows: a method for rapidly degrading azo dye orange II comprises the following steps:
(1) weighing golden orange II powder, dissolving the golden orange II powder in deionized water to prepare a golden orange II solution with the concentration of 10mg/L, wherein the golden orange II solution is a target pollutant;
(2) sleeving and fixing a beaker filled with 200mL of the target pollutant with a foam plate, putting the beaker into an ultrasonic machine, adding deionized water into the ultrasonic machine to enable the liquid level of the deionized water in the ultrasonic machine to be equal to that of the beaker, keeping the ultrasonic set frequency and ultrasonic time, starting the ultrasonic machine, and adding potassium hydrogen persulfate into the pollutant to enable the concentration of persulfate in the solution to be 1-3 mmol/L;
(3) ascorbic acid and raw ore are added immediately after 30 seconds, so that the ascorbic acid concentration in the solution is 0.15-0.35mmol/L and the raw ore content is 1-3 g/L.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the concentration of the persulfate in the solution was 2 mmol/L.
Further, the ascorbic acid concentration in the solution was 0.25 mmol/L.
Further, the crude ore content in the solution was 2 g/L.
Furthermore, the concentration of the aurantium II contained in the target pollutant is 10 mg/L.
Furthermore, the ultrasonic frequency is 40KHz, and the ultrasonic time is 60 min.
Has the advantages that: the invention improves the problem that Fe (II) is oxidized into Fe (III) and is difficult to regenerate and the reaction is limited by pH by adding the ascorbic acid to induce the persulfate, on the basis, the raw ore is added to increase the reactive active sites, Fe (II) and generate free radicals through ultrasonic enhancement to achieve the purpose of accelerating the decoloration of the golden orange II dye, and the experimental result proves that the system can almost degrade 200ml of golden orange II solution with the concentration of 10mg/L in 45 minutes at the fastest speed, the degradation rate is greatly accelerated compared with an ascorbic acid and persulfate system, and the resource recycling can be realized by utilizing the raw ore treatment of a steel plant, and the economic cost is low. A method for rapidly degrading golden orange II by utilizing crude ore catalysis in cooperation with ascorbic acid activated persulfate under an ultrasonic condition is proved to have better feasibility through a series of experimental data, has quicker and more stable removal rate for golden orange II dye, realizes the treatment of wastes with processes of wastes by utilizing the crude ore of an iron and steel plant as a catalyst for reaction, and has certain economic applicability.
Drawings
FIG. 1 is a graph showing the degradation rate of a gold orange II dye in the invention patent application No. 201910375175.3, namely a method for degrading the gold orange II dye by using wood chip biochar activated persulfate prepared by high-temperature pyrolysis and application thereof;
FIG. 2 is a graph of the removal effect of bismuth ferrite visible light catalyzed peroxymonosulfate for removing gold orange II according to the initial concentration conditions of different gold orange II solutions published in chemical research and application 2019,31(05) as shown in FIG. 2;
FIG. 3 is a graph of the degradation rate of different systems on golden orange II;
FIG. 4 is a graph showing the degradation rate of golden orange II at different ore loadings;
FIG. 5 is a graph showing the degradation rate of golden orange II at different PMS dosages;
FIG. 6 is a graph of the degradation rate of golden orange II at different AA dosages;
FIG. 7 is a graph showing the degradation rate of orange II in the highest degradation rate condition.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
A method for rapidly degrading azo dye orange II comprises the following steps:
(1) weighing golden orange II powder, dissolving the golden orange II powder in deionized water to prepare a golden orange II solution with the concentration of 10mg/L, wherein the golden orange II solution is a target pollutant for reaction degradation;
(2) sleeving and fixing a beaker filled with 200mL of the target pollutant with a foam plate, putting the beaker into an ultrasonic machine, adding deionized water into the ultrasonic machine to enable the liquid level of the deionized water in the ultrasonic machine to be equal to that of the beaker, setting the frequency and the ultrasonic time of the ultrasonic machine, starting the ultrasonic machine, and adding potassium hydrogen persulfate into the pollutant to enable the concentration of persulfate in the solution to be 1-3 mmol/L;
(3) ascorbic acid and raw ore are added immediately after 30 seconds, so that the ascorbic acid concentration in the solution is 0.15-0.35mmol/L and the raw ore content is 1-3 g/L.
Preferably, the ultrasonic frequency is 40 KHz.
The molecular formula of the golden orange II is C16H11N2NaO4S, the molecular formula of the potassium hydrogen persulfate is K5H3S4O18, the molecular formula of the ascorbic acid is C6H8O6, the grades of all reagents are analytically pure, and the experimental water is deionized water.
The analysis results of the iron phase of the raw ore comprehensive sample (crushed ore discharge) are as follows:
magnetic iron: 24.47%, iron carbonate: 0.87%, brown iron: 3.15%, iron sulfide: 1.74%, insoluble iron silicate: 0.35%, total iron: 30.58 percent.
The experimental ultrasonic instrument is an SB-120DT ultrasonic cleaning machine manufactured by Ningbo Xinzhi Biotechnology GmbH, and the frequency of use is 40 KHz.
The rotor stirrer is an Ingxing 79-1 type constant-temperature heating magnetic stirrer, and the rotating speed of the rotor is 1000 revolutions per minute during experiments.
The UV-visible spectrophotometer used was Shimadzu UV-1800, and the absorbance was determined at a wavelength of 485nm by full scanning of 10mg/L orange II.
Example 1
Dissolving a certain amount of weighed golden orange II in deionized water to prepare a dye solution with a certain concentration, wherein a 50mg/L golden orange II stock solution is prepared in an experiment, and 200ml of a 10mg/L golden orange II solution is obtained in a beaker as a target pollutant through dilution in each experiment. 0.4403g of ascorbic acid is weighed into a 50ml brown volumetric flask, the volume is constant, the concentration of the ascorbic acid solution is 0.25mmol/L, the ascorbic acid solution is placed in a refrigerator for cold storage before use, and the raw ore and the potassium hydrogen persulfate are currently called. The following golden orange II is abbreviated as AO7, the concentration is 10mg/L, persulfate is abbreviated as PMS, ascorbic acid is abbreviated as AA, and the reaction time is 60 min.
The method comprises the steps of sleeving and fixing a beaker filled with 200mL of the target pollutant with a foam plate, placing the beaker into an ultrasonic machine, adding deionized water into the ultrasonic machine to enable the liquid level of the deionized water in the ultrasonic machine to be level with the liquid level of the beaker, starting the ultrasonic machine, wherein the frequency of the ultrasonic machine is 40KHz, changing reaction modes respectively, selecting any 1-3 combinations of raw ores, PMS and AA, inspecting the degradation rate of AO7 in the target pollutant, and replacing the deionized water in the ultrasonic machine after each group of tests is completed so as to avoid different reaction temperatures caused by the temperature rise of the deionized water in the ultrasonic machine due to the work of the ultrasonic machine. Through UV-visible spectrophotometer, samples were taken at 0, 10, 20, 30, 45, 60 minutes and their absorbance at 485nm was measured through 0.45umMCE aqueous membrane, and the results of comparing the degradation rates of different systems to golden orange II are shown in Table 1:
TABLE 1 Effect of different systems on the degradation rate of AO7
Figure BDA0003162934290000061
Figure BDA0003162934290000071
The degradation trend of different systems on golden orange II is shown in figure 1, and the conclusion is that: according to experimental data analysis, the rapid degradation of AO7 can be realized by using the catalysis of raw ore and the activation of persulfate by ascorbic acid under the ultrasonic condition, and the method comprises the following steps: 1g/L, PMS: 2mmol/L, AA: under the condition of 0.25mmol/L, the degradation rate of AO7 in 45 minutes reaches 95%, and the degradation rate of AO7 in 60 minutes reaches 99%.
Example 2
In order to explore the optimal condition for rapidly degrading golden orange II by using crude ore catalysis in cooperation with ascorbic acid activated persulfate under the ultrasonic condition, PMS: 2mmol/L, AA: under the condition of 0.25mmol/L, the influence of different ore feeding amounts on the AO7 degradation rate is examined, and the comparison results are shown in a table 2:
TABLE 2 Effect of different loadings on the degradation rate of AO7
Figure BDA0003162934290000072
And (4) conclusion: when the raw ore content is 2g/L, namely 0.4g, the concentration of PMS solution is 2mmol/L, and the concentration of AA solution is 0.25mmol/L, the system has the fastest degradation rate to AO7, and the removal rate of 99% is reached in 45 minutes.
Example 3
In order to explore the optimal conditions for rapidly degrading golden orange II by using crude ore catalysis in cooperation with ascorbic acid activated persulfate under the ultrasonic condition, the crude ore: 2g/L, AA: 0.25mmol/L, and the influence of PMS added with different concentrations on the AO7 degradation rate is examined, and the comparison results are shown in Table 3:
TABLE 3 Effect of PMS addition at different concentrations on AO7 degradation rate
Figure BDA0003162934290000081
And (4) conclusion: PMS with different concentrations is added, when the content of the obtained raw ore is 2g/L, the concentration of PMS solution is 2mmol/L, and AA is 0.25mmol/L, the system has the fastest degradation rate to AO7 with the concentration of 10 mg/L.
Example 4
In order to explore the optimal conditions for rapidly degrading golden orange II by using crude ore catalysis in cooperation with ascorbic acid activated persulfate under the ultrasonic condition, the crude ore: 2g/L, PMS: 2mmol/L, the influence of AA with different concentrations on the degradation rate of AO7 is examined, and the comparison result is shown in Table 3:
TABLE 4 Effect of different concentrations of AA on the degradation rate of AO7
Figure BDA0003162934290000082
Figure BDA0003162934290000091
And (4) conclusion: in the degradation data results of AO7 under different AA adding amounts, when the original ore content is 2g/L, PMS is 2mmol/L and AA is 0.25mmol/L, the system has the fastest degradation rate to AO7 of 10 mg/L.
Example 5
To verify whether the effect obtained by the system is accidental when the raw ore content is 2g/L, PMS is 2mmol/L and the AA addition amount is 0.25mmol/L, the experiment under the condition is repeated, and the results are as follows:
TABLE 5 results of 2 experiments in parallel according to the optimal reaction conditions
Figure BDA0003162934290000092
And (4) conclusion: the reaction conditions of 2g/L raw ore content, 2mmol/L PMS and 0.25mmol/L AA are repeated, and the comparison with other experimental data proves that the highest degradation rate of AO7 is achieved under the conditions, and the degradation rate of repeated experiments reaches 98% in 45 min.
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 (6)

1. A method for rapidly degrading azo dye orange II is characterized by comprising the following steps:
(1) weighing golden orange II powder, dissolving the golden orange II powder in deionized water to prepare a golden orange II solution with the concentration of 10mg/L, wherein the golden orange II solution is a target pollutant;
(2) sleeving and fixing a beaker filled with 200mL of the target pollutant with a foam plate, putting the beaker into an ultrasonic machine, adding deionized water into the ultrasonic machine to enable the liquid level of the deionized water in the ultrasonic machine to be equal to that of the beaker, setting the frequency and the ultrasonic time of the ultrasonic machine, starting the ultrasonic machine, and adding potassium hydrogen persulfate into the pollutant to enable the concentration of persulfate in the solution to be 1-3 mmol/L;
(3) ascorbic acid and raw ore are added immediately after 30 seconds, so that the ascorbic acid concentration in the solution is 0.15-0.35mmol/L and the raw ore content is 1-3 g/L.
2. The method for rapidly degrading azo dye, namely, gold orange II, according to claim 1, wherein the concentration of persulfate in the solution is 2 mmol/L.
3. The method for rapidly degrading azo dye golden orange II according to claim 1, wherein the concentration of ascorbic acid in the solution is 0.25 mmol/L.
4. The method for rapidly degrading azo dye, namely, gold orange II according to claim 1, wherein the raw ore content in the solution is 2 g/L.
5. The method for rapidly degrading azo dye aurantium II according to claim 1, wherein the concentration of aurantium II in the target pollutant is 10 mg/L.
6. The method for rapidly degrading azo dye golden orange II according to claim 1, wherein the ultrasonic frequency is 40KHz, and the ultrasonic frequency is 60 min.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101973622A (en) * 2010-10-19 2011-02-16 哈尔滨工业大学 Method for accelerating monopersulfate and persulfate to produce free sulfate radicals
CN107381766A (en) * 2017-07-31 2017-11-24 华中师范大学 A kind of method that natural organic molecule promotes persulfate activation repairing organic material contaminated soil and underground water
CN109052618A (en) * 2018-09-12 2018-12-21 北京农学院 Activate persulfate, the method for degradation of contaminant, application
CN110563116A (en) * 2019-09-09 2019-12-13 安徽科技学院 Method for degrading azo dye gold orange II solution by catalyzing persulfate through aluminum alloy pickling waste liquid
CN111908582A (en) * 2019-05-07 2020-11-10 南开大学 Method for degrading orange II dye by using wood chip biochar activated persulfate prepared by high-temperature pyrolysis and application

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101973622A (en) * 2010-10-19 2011-02-16 哈尔滨工业大学 Method for accelerating monopersulfate and persulfate to produce free sulfate radicals
CN107381766A (en) * 2017-07-31 2017-11-24 华中师范大学 A kind of method that natural organic molecule promotes persulfate activation repairing organic material contaminated soil and underground water
CN109052618A (en) * 2018-09-12 2018-12-21 北京农学院 Activate persulfate, the method for degradation of contaminant, application
CN111908582A (en) * 2019-05-07 2020-11-10 南开大学 Method for degrading orange II dye by using wood chip biochar activated persulfate prepared by high-temperature pyrolysis and application
CN110563116A (en) * 2019-09-09 2019-12-13 安徽科技学院 Method for degrading azo dye gold orange II solution by catalyzing persulfate through aluminum alloy pickling waste liquid

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Application publication date: 20211001