CN109179585B - Method for degrading methyl violet wastewater - Google Patents

Method for degrading methyl violet wastewater Download PDF

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CN109179585B
CN109179585B CN201811082438.3A CN201811082438A CN109179585B CN 109179585 B CN109179585 B CN 109179585B CN 201811082438 A CN201811082438 A CN 201811082438A CN 109179585 B CN109179585 B CN 109179585B
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methyl violet
wastewater
electrode
filtering
oxidation
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CN109179585A (en
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王莉
王俊波
潘华
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Zhejiang Shuren 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
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage 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
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • 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
    • C02F2001/007—Processes including a sedimentation step
    • 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
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
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Abstract

The invention discloses a method for degrading methyl violet wastewater, which comprises the steps of firstly, settling sand on a methyl violet wastewater grid, then heating the methyl violet wastewater to 10-60 ℃, adjusting the pH to 2-7, filtering after 1 hour, electrolyzing the filtrate obtained by filtering, adopting one of platinum sheet, iron, copper, gold, ruthenium, palladium, graphite, lead and BDD electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, electrochemically oxidizing the solution for two minutes under the condition that the oxidation voltage is 1.0-1.5V, adding a proper amount of free radical capture agent, and carrying out electropolymerization reaction on the free radical capture agent and an electrolysis product to generate precipitate; the clear liquid was obtained by filtration. Compared with other methods for degrading methyl violet, the method can combine small molecular fragments generated by electrochemical oxidation of methyl violet with a radical trapping agent to generate a series of precipitates, and generate a polymer through electropolymerization on an electrode, thereby greatly reducing degradation time, electrolysis energy consumption and COD value in wastewater.

Description

Method for degrading methyl violet wastewater
Technical Field
The invention belongs to the field of environmental protection, and particularly relates to a method for degrading methyl violet wastewater.
Background
Methyl violet of formula C23H31ClN2O3And the molecular weight is 479.029. Is a bright peach red artificially synthesized basic dye, and is widely used for the paper making industry and the printing and dyeing industry, such as the dyeing of printing paper, wax paper, feather products, wheat straws, leather and the like. Methyl violet has strong fluorescence in solution, good stability, high wastewater chromaticity and poor biodegradability, and the biological accumulation in land and aquatic ecosystems has influence on the environment and human health. Therefore, treatment of methyl violet wastewater is urgent.
Currently, the studied methods for degrading methyl violet include an adsorption method, a chemical oxidation method, a Fenton method, an electrochemical oxidation method, a photocatalytic method and the like. The adsorbent is adopted to adsorb methyl violet, complex pretreatment is required, and the decolorization rate is relatively low; the chemical oxidation method adopts an oxidant to oxidize methyl violet, so that secondary pollution is easily caused; the electrochemical oxidation method is fast and simple, but is difficult to be widely applied due to high energy consumption and large power consumption. The Fenton method and the photocatalytic method utilize generated hydroxyl radicals to oxidize methyl violet, wherein the research on photocatalytic degradation of methyl violet is the most, the method has the advantages of thorough degradation, low speed, long degradation time, complex degradation process, difficult control of reaction conditions, high energy consumption, difficulty in meeting the production requirements of industrial enterprises, poor COD removal efficiency in solution and difficulty in large-scale application in actual wastewater treatment.
The aniline derivatives are monomers capable of initiating polymerization reaction by an electrochemical method, aniline free radicals are easily generated on electrodes, attack dye molecules methyl violet to generate organic molecules with larger molecular weight, the water-soluble capacity of the aniline derivatives is greatly reduced along with the increase of the molecular weight, and then the aniline derivatives are precipitated from water, and redundant aniline derivatives can be mutually polymerized to generate polyaniline to be precipitated from the water, so that the water quality can be rapidly purified, and pollutants in the water can be removed.
Disclosure of Invention
The invention aims to provide a method for degrading methyl violet wastewater, aiming at the defects of the prior art.
The purpose of the invention is realized by the following technical scheme: a method for degrading methyl violet wastewater comprises the following steps:
(1) settling sand on the methyl violet wastewater grid;
(2) heating the methyl violet wastewater treated in the step (1) to 10-60 ℃, adjusting the pH to 2-7, and filtering after 1 hour to obtain a filtrate;
(3) taking the filtrate treated in the step (2) as an electrolyte, adopting one of platinum, iron, copper, gold, ruthenium, palladium, graphite, lead and BDD electrodes as an oxidation working electrode, adopting a saturated calomel electrode as a reference electrode, adopting a graphite electrode as a counter electrode, oxidizing for two minutes under the condition that the oxidation voltage is 1.0-1.5V, adding a free radical trapping agent, and combining broken micromolecular free radicals generated by electrolysis with the free radical trapping agent to generate flocculent precipitates; and filtering the oxidized electrolyte by using a filter membrane to obtain clear liquid.
Further, in the step 3, the free radical scavenger is selected from aniline, benzylamine and phenylethylamine, and the addition amount of the free radical scavenger is 0.2-2 ml/L of wastewater.
The invention has the beneficial effects that: the invention adopts an electrolytic method to degrade methyl violet, generates molecular fragments, partially precipitates, and partially reacts with substances such as aniline and the like added into electrolyte to generate polyaniline-like compounds, thereby reducing the COD value of the wastewater in a short time. Compared with a photocatalysis or high-voltage method, the method greatly reduces the degradation time and the electrolysis energy consumption. Is suitable for the early-stage rapid pretreatment of large-scale industrial wastewater.
Detailed Description
The invention uses methyl violet waste water (C is 100mg dm)-3) After the precipitation through a grating, the pH value of the solution is adjusted, and the precipitate is filtered to remove Fe (OH) generated in the solution2、Fe(OH)3After the metal hydroxide is precipitated, electrochemically oxidizing the methyl violet wastewater in an electrolytic cell, and adding substances such as free radical trapping agent aniline and the like until a precipitate is generated; the precipitate was filtered. The methyl violet is easy to generate electropolymerization reaction at the anode to generate polymer precipitate similar to aniline, greatly reduces the COD value of the solution, and obviously reduces the electric energy and time consumed by degradation. The COD value of the microbiological method similar to the process is about 60-400mg dm-3While the lowest COD value of the solution is only 14mg dm by adopting the electropolymerization method to degrade the methyl violet wastewater-3Left and right.
The invention degrades methyl violet in wastewater through the following two ways:
route 1: electropolymerization
Figure BDA0001802299930000021
Route 2: polymerizing small molecular fragment and aniline
Figure BDA0001802299930000022
Figure BDA0001802299930000031
Specifically, the method for degrading methyl violet wastewater comprises the following steps:
(1) settling sand on the methyl violet wastewater grid;
(2) heating the methyl violet wastewater treated in the step (1) to 10-60 ℃, adjusting the pH to 2-7, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Plasma forms a precipitate in the environment, filtering is carried out, and the filtrate obtained by filtering is subjected to next treatment;
(3) taking the filtrate treated in the step (2) as an electrolyte, adopting one of a platinum sheet, iron, copper, gold, ruthenium, palladium, graphite, lead and BDD electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, oxidizing for two minutes under the condition that the oxidation voltage is 1.0-1.5V, adding substances such as free radical trapping agent aniline and the like, and carrying out electro-polymerization reaction on the methyl violet wastewater to generate a precipitate; and filtering the electrolyte after the oxidation reaction by using a filter membrane to obtain clear liquid.
Example 1
(1) Methyl violet (C100 mg dm)-3) Settling sand by using a waste water grid;
(2) heating the methyl violet wastewater treated in the step (1) to 15 ℃, adjusting the pH to 5, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Forming precipitate, filtering, and treating the filtrate;
(3) and (3) taking the filtrate treated in the step (2) as an electrolyte, adopting a platinum electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 0.2 ml/L aniline solution into the filtrate, oxidizing for two minutes under the condition that the oxidation voltage is 1.3V, and carrying out electropolymerization reaction on the methyl violet wastewater to generate a precipitate. Filtering the oxidized electrolyte with a filter membrane to obtain a clear solution;
the clear liquid obtained by the degradation in this example showed a COD of 15mg dm-3。
Example 2
(1) Methyl violet (C100 mg dm)-3) Settling sand by using a waste water grid;
(2) heating the methyl violet wastewater treated in the step (1) to 15 ℃, adjusting the pH to 7, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Forming a precipitate, filtering off, and filteringThe obtained filtrate is processed in the next step;
(3) and (3) taking the filtrate treated in the step (2) as an electrolyte, adopting a gold electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 0.4 ml/L aniline solution into the filtrate, oxidizing for two minutes under the condition that the oxidation voltage is 1.1V, and carrying out electropolymerization reaction on the methyl violet wastewater to generate a precipitate. Filtering the oxidized electrolyte with a filter membrane to obtain clear liquid;
the clear liquid obtained by the degradation in this example showed a COD of 50mg dm-3。
Example 3
(1) Methyl violet (C100 mg dm)-3) Settling sand by a water grid;
(2) heating the methyl violet wastewater treated in the step (1) to 25 ℃, adjusting the pH to 6, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Forming precipitate, filtering, and treating the filtrate;
(3) taking the filtrate treated in the step (2) as an electrolyte, a graphite electrode as an oxidation electrode, a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 0.4 ml/L of phenylmethylamine solution into the wastewater, oxidizing the wastewater for two minutes under the condition that the oxidation voltage is 1.2V, carrying out electropolymerization reaction on the methyl violet wastewater, and filtering the oxidized electrolyte by a filter membrane to obtain a clear solution;
the clear liquid obtained by the degradation in this example showed a COD of 45mg dm-3。
Example 4
(1) Settling sand on a methyl violet (C is 100mg/L) wastewater grid;
(2) heating the methyl violet wastewater treated in the step (1) to 30 ℃, adjusting the pH to 2, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Forming precipitate, filtering, and treating the filtrate;
(3) and (3) taking the filtrate treated in the step (2) as an electrolyte, adopting a ruthenium electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 0.5 ml/L of phenethylamine solution into the filtrate, oxidizing the filtrate for two minutes under the condition that the oxidation voltage is 1.2V, and carrying out electropolymerization reaction on the methyl violet wastewater to generate a precipitate. Filtering the precipitation filter membrane to obtain clear liquid;
the clear liquid obtained by the degradation in this example showed a COD of 45mg dm-3。
Example 5
(1) Methyl violet (C100 mg dm)-3) Settling sand by using a waste water grid;
(2) heating the methyl violet wastewater treated in the step (1) to 30 ℃, adjusting the pH to 4, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Precipitating, filtering, and performing next treatment on the filtrate obtained by filtering;
(3) taking the filtrate treated in the step (2) as an electrolyte, adopting a palladium electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 0.5 ml/L of phenylethylamine solution into the wastewater, oxidizing the wastewater for two minutes under the condition that the oxidation voltage is 1.1V, carrying out electropolymerization reaction on the methyl violet wastewater, and filtering an oxidized electrolyte filter membrane to obtain a clear liquid;
the clear liquid obtained by the degradation in this example showed a COD of 41mg dm-3。
Example 6
(1) Settling sand on a methyl violet (C is 100mg/L) wastewater grid;
(2) heating the methyl violet wastewater treated in the step (1) to 30 ℃, adjusting the pH to 2, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Precipitating, filtering, and performing next treatment on the filtrate obtained by filtering;
(3) and (3) taking the filtrate treated in the step (2) as an electrolyte, adopting a BDD electrode as an oxidation electrode and a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 0.6 ml/L of phenylmethylamine solution into the filtrate, oxidizing the mixture for two minutes under the condition that the oxidation voltage is 1.1V, and carrying out electropolymerization reaction on the methyl violet wastewater to generate a precipitate. Filtering the oxidized electrolyte with a filter membrane to obtain clear liquid;
degradation by this exampleThen, a clear liquid was obtained, and COD was measured to be 49 mg. dm-3。
Example 7
(1) Settling sand on a methyl violet (C is 100mg/L) wastewater grid;
(2) heating the methyl violet wastewater treated in the step (1) to 35 ℃, adjusting the pH to 3, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Precipitating, filtering, and performing next treatment on the filtrate obtained by filtering;
(3) and (3) taking the filtrate treated in the step (2) as an electrolyte, adopting a lead electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 0.3 ml/L of phenethylamine solution into the filtrate, oxidizing the filtrate for two minutes under the condition that the oxidation voltage is 1.1V, and carrying out electropolymerization reaction on the methyl violet wastewater to generate a precipitate. Filtering the oxidized electrolyte with a filter membrane to obtain clear liquid;
the clear liquid obtained by the degradation in this example showed a COD of 28mg dm-3。
Example 8
(1) Settling sand on a methyl violet (C is 100mg/L) wastewater grid;
(2) heating the methyl violet wastewater treated in the step (1) to 40 ℃, adjusting the pH to 3, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Precipitating, filtering, and performing next treatment on the filtrate obtained by filtering;
(3) and (3) taking the filtrate treated in the step (2) as an electrolyte, adopting a copper electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 1 ml/L aniline solution into the filtrate, oxidizing for two minutes under the condition that the oxidation voltage is 1.3V, and carrying out electropolymerization reaction on the methyl violet wastewater to generate a precipitate. Filtering the oxidized electrolyte with a filter membrane to obtain clear liquid;
the clear liquid obtained by the degradation in this example showed a COD of 15mg dm-3。
Example 9
(1) Settling sand on a methyl violet (C is 100mg/L) wastewater grid;
(2) will step withHeating the methyl violet wastewater treated in the step (1) to 30 ℃, adjusting the pH to 6, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Precipitating, filtering, and performing next treatment on the filtrate obtained by filtering;
(3) and (3) taking the filtrate treated in the step (2) as an electrolyte, adopting an iron electrode as an oxidation electrode, adopting a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 0.2 ml/L of phenylmethylamine solution into the filtrate, oxidizing the phenylmethylamine solution for two minutes under the condition that the oxidation voltage is 1.2V, and carrying out electropolymerization reaction on the methyl violet wastewater to generate a precipitate. Filtering the oxidized electrolyte with a filter membrane to obtain clear liquid;
the clear liquid obtained by the degradation in this example showed a COD of 20mg dm-3。
Example 10
(1) Methyl violet (C100 mg dm)-3) Settling sand by using a waste water grid;
(2) heating the methyl violet wastewater treated in the step (1) to 25 ℃, adjusting the pH to 2, and filtering after 1 hour; fe in wastewater2+、Fe3+，Ca2+Precipitating, filtering, and performing next treatment on the filtrate obtained by filtering;
(3) and (3) taking the filtrate treated in the step (2) as an electrolyte, adopting a BDD electrode as an oxidation electrode and a saturated calomel electrode as a reference electrode, then simultaneously dropwise adding 2 ml/L aniline solution into the filtrate, oxidizing for two minutes under the condition that the oxidation voltage is 1.2V, and carrying out electropolymerization reaction on the methyl violet wastewater to generate a precipitate. Filtering the oxidized electrolyte with a filter membrane to obtain clear liquid;
the clear liquid obtained by the degradation in this example showed a COD of 48mg dm-3。
The above-described embodiments are intended to illustrate rather than to limit the invention, and any modifications and variations of the present invention are within the spirit of the invention and the scope of the appended claims.

Claims (2)

1. A method for degrading methyl violet wastewater is characterized by comprising the following steps:
(1) settling sand on the methyl violet wastewater grid;
(2) heating the methyl violet wastewater treated in the step (1) to 10-60 ℃, adjusting the pH to 2-7, and filtering after 1 hour to obtain a filtrate;
(3) taking the filtrate treated in the step (2) as an electrolyte, adopting one of platinum, iron, copper, gold, ruthenium, palladium, graphite, lead and BDD electrodes as an oxidation working electrode, taking a saturated calomel electrode as a reference electrode, taking a graphite electrode as a counter electrode, oxidizing for 2 minutes under the condition that the oxidation voltage is 1.0-1.5V, adding a free radical trapping agent, and combining broken micromolecular free radicals generated by electrolysis with the free radical trapping agent to generate flocculent precipitates; filtering the oxidized electrolyte by using a filter membrane to obtain clear liquid; the free radical trapping agent is one of aniline, benzylamine and phenylethylamine.
2. The method for degrading methyl violet wastewater according to claim 1, wherein in the step (3), the addition amount of the free radical scavenger is 0.2-2 ml/L wastewater.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102249376A (en) * 2011-05-20 2011-11-23 北京化工大学 Method for realizing recycling of aniline waste water and zero release through electropolymerization

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102249376A (en) * 2011-05-20 2011-11-23 北京化工大学 Method for realizing recycling of aniline waste water and zero release through electropolymerization

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
电化学聚合;廖川平;《化学通报》;化学通报;20000218;第37-41页 *
聚结晶紫修饰玻碳电极检测叶酸;杜学萍等;《河南大学学报（自然科学版）》;河南大学学报（自然科学版）;20141130;第659-662页 *

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