CN107720925A - Utilize the method for sodium sulfite activation persulfate degraded methyl orange azo dye wastewater - Google Patents
Utilize the method for sodium sulfite activation persulfate degraded methyl orange azo dye wastewater Download PDFInfo
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- CN107720925A CN107720925A CN201710827726.6A CN201710827726A CN107720925A CN 107720925 A CN107720925 A CN 107720925A CN 201710827726 A CN201710827726 A CN 201710827726A CN 107720925 A CN107720925 A CN 107720925A
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- methyl orange
- activation
- azo dye
- sodium sulfite
- dye wastewater
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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
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Organic Chemistry (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention provides a kind of method using sodium sulfite activation persulfate degraded methyl orange azo dye wastewater, compared with prior art, sodium sulfite (Na of the invention2SO3) activation persulfate (Na2S2O8) constitute the active specy (potentiometric titrations that a kind of redox system produces strong oxidizing property：SO4 ‑With inferior sulfate radical free radical：SO3 ‑), handle methyl orange azo dye wastewater, the results showed that the conjugated system that strong oxidizing property free radical energy rapid damage methyl orange azo double bond is formed, there is preferable decolored degradation effect.Compared to conventional activation technology, processing cost is low, and reaction system is gentle, and reaction product is nontoxic sulfate ion, non-secondary pollution, and activation energy is relatively low.The invention is advantageous to the transformation and upgrade of waste water from dyestuff pollution reducing facility, also has potential commercial application value to poisonous and hazardous industrial organic waste water.
Description
Technical field
The invention belongs to field of waste water treatment, and in particular to one kind utilizes sodium sulfite activation persulfate degraded methyl orange
The method of azo dye wastewater.
Background technology
In recent years, the potentiometric titrations (SO for producing strong oxidizing property is activated based on persulfate4 ·—) advanced oxidation skill
Art receives significant attention.Advanced oxidation based on sulphuric acid free radical oneself be widely used in repairing the underground water and soil that are contaminated
Earth, also obtaining certain research with the effect in sewage and drinking water treatment recently.This be based primarily upon it is following some：(1) sulphur
The oxidability of acid free radical is strong, its E=2.6V, has non-selectivity, continuation and reaction rate to Organic substance in water oxidation
It hurry up；(2) sulphuric acid free radical and its oxidation product SO4 2-Do not influence subsequent biological treatment；(3) persulfate is easily stored, water-soluble
Good, environment-friendly, safety and stability is easily controllable, and price is low good commercial promise.
Persulfate activating technology is quickly grown, and common activating technology has thermal activation, transition metal ions activate, be ultraviolet
Line activation, alkali activation, ultrasonic activation etc..Recently some new activating technologies are continued to bring out out, including with Fe0, iron content
Ore (iron composite material), activated carbon (carbon composite) include the new material of modified synthesis based on above-mentioned material and contained
The novel activated technology of the organic matter activation persulfate of quinone structure.
Dyeing is the discharge rich and influential family of industrial wastewater, is mainly derived from dye and dye intermediate production industry, waste water
In organic component mostly using aromatic hydrocarbons and heterocyclic compound as parent, and with colour developing group and polar group.In waste water also
Contain more raw material and byproduct, such as aniline, phenols and inorganic salts.Other DYE PRODUCTION is wide in variety, and towards anti-light
Solution, anti-oxidant, antibiooxidation direction are developed.To realize national energy-saving emission reduction requirement, dyeing waste water discharge standard is significantly
Lifting, qualified discharge is difficult to using traditional materialization, biochemical process route.
Numerous studies, such as advanced oxidation processes have been carried out to the advanced treating of dyestuff both at home and abroad, have mainly there is Fenton, e-
Fenton, electro-catalysis, photocatalysis, photoelectrocatalysis；Physico-chemical process, mainly there are absorption, ion exchange, ultrafiltration, UF membrane, coagulation etc..
Bioanalysis mainly has biological reinforced etc..
The unification of removal effect, financial cost, ecological benefits is still relatively inaccessible to from the point of view of domestic treatment effect.Therefore,
Explore inexpensive, efficient techniques of Dyeing Wastewater Treatment and try out it is imperative.
Methyl orange (MO) is a kind of soluble azo dyes, chromophoric group-N=N- (azo double bond), in waste water from dyestuff
With certain representativeness, it is not easy to be degraded by some conventional methods, so being more easy to cause serious problem of environmental pollution.
The content of the invention
It is an object of the invention to provide utilize sodium sulfite activation persulfate degraded methyl orange azo dye wastewater
Method, with sodium sulfite (Na2SO3) activation persulfate (Na2S2O8) constitute a kind of redox system generation strong oxidizing property
Active specy (potentiometric titrations：SO4 -With inferior sulfate radical free radical：SO3 -), handle methyl orange azo dye wastewater.
The method using sodium sulfite activation persulfate degraded methyl orange azo dye wastewater of the offer of the present invention, bag
Include following steps：
Na is added into methyl orange azo dye wastewater2SO3And Na2S2O8, then add NaOH or H2SO4Adjust reactant
It is initial pH to 2-11, heats, you can.
Preferably, reaction system initial pH to 3-11 is adjusted.
Described heat is specially to handle 60min at 25-60 DEG C.
Na2SO3And Na2S2O8Mol ratio be 0.5-1:1.
Na2S2O8Concentration is 5-25mM in waste water.
Compared with prior art, sodium sulfite (Na of the invention2SO3) activation persulfate (Na2S2O8) constitute one kind
Redox system produces the active specy (potentiometric titrations of strong oxidizing property：SO4 -With inferior sulfate radical free radical：
SO3 -), handle methyl orange azo dye wastewater, the results showed that strong oxidizing property free radical energy rapid damage methyl orange azo double bond
The conjugated system of formation, there is preferable decolored degradation effect.Compared to conventional activation technology, processing cost is low, and reaction system is gentle,
Reaction product is nontoxic sulfate ion, non-secondary pollution, and activation energy is relatively low.The invention is advantageous to waste water from dyestuff pollution
The transformation and upgrade for the treatment of facility, also there is potential commercial application value to poisonous and hazardous industrial organic waste water.
Brief description of the drawings
Fig. 1 is that the activation efficiency of different disposal method contrasts；
Fig. 2 contrasts for ultraviolet scanning spectrum figure；
Fig. 3 contrasts for infrared spectrogram；
Fig. 4 mechanism of degradation figures；
Influences of Fig. 5 different mol ratios M to MO degradation rates；
Different initial influences of the pH to MO degradation rates of Fig. 6；
Fig. 7 differences S2O8 2-To the influence of MO degradation processes under concentration；
Fig. 8 is influence of the different initial concentrations to MO degradation rates；
Fig. 9 is influence of the different temperatures to MO degradation rates.
Embodiment
Embodiment 1
Using the method for sodium sulfite activation persulfate degraded methyl orange azo dye wastewater, comprise the following steps：
0.1g methyl orange MO powder is weighed respectively, and constant volume places 24h, MO concentration is 100mg/ in 1000mL volumetric flasks
L, it is diluted to MO concentration 60mg/L；Add Na2SO3And Na2S2O8(Na2SO3And Na2S2O8Mol ratio 0.5:1, Na2S2O8Concentration is
15mM), reaction system initial pH to 11 is adjusted with 0.1M NaOH solution, 60min is handled at 40 DEG C, with 0.45um filter membrane mistakes
It is measured after filter, methyl orange degradation rate 96.79%.
Water sample MO degradation rates and sign are using UV detector (T6, Beijing spectrum analysis are general) measure before and after reaction.It is red
Outer sign uses Fourier transformation infrared spectrometer (IRPrestige-21, Japanese Shimadzu), and its analysis condition is：Negate after answering
The supernatant 20mL of centrifugation is put into small beaker, then takes 0.2g KBr dissolution of crystals that beaker then is placed in into vacuum and done in wherein
Dry case is dried in vacuo 24 hours, the organic molecule in reaction system is adsorbed in KBr molecular surfaces, after sample drying after tabletting
Carry out infrared analysis.
Embodiment 2
Contrast SO3 2-Activate S2O8 2-, single S2O8 2-With single SO3 2-Degraded of three kinds of systems to MO.MO initial concentrations C0=
10mg/L, n (SO3 2-) and n (S2O8 2-) dosage is 10mM, initial pH value 3.0, temperature is room temperature, as a result such as Fig. 1 institutes
Show.As seen from the figure, under same experiment condition, from the point of view of MO degradation rates, SO3 2-To S2O8 2-There is obvious activation effect.Preceding
In 30min, SO3 2-/S2O8 2-The methyl orange degradation rate η of activation systemMOThan single S2O8 2-Want high by 35.26%；Dropped in 60min
Solution rate is close to 88.55%, and single S2O8 2-Degradation efficiency just reach 67.52 in 60min, both ηMODiffer nearly 21.03%.
And single SO3 2-System MO degradation rates are very low, and 60min is less than 5.93%.
MO degradation rates and molecule structure change are further analyzed, to MO raw waters, SO3 2-/S2O8 2-With single S2O8 2-Carry out UV
Analyzed with FT-IR scanning optical spectrums, as a result respectively as shown in Fig. 2 and Fig. 3.As can be seen that former MO MO molecules near 473nm are even
π-the π of N structure*Strong absworption peak caused by transition, because of the π-π of phenyl ring conjugated system at 270 and 312nm*Cause 2 it is weaker
Absworption peak；In single S2O8 2-Under oxidation system, peak heights of the MO at 473 substantially reduces, and illustrates the conjugation hair in MO structures
Color system has destroyed, and the absworption peak at 270 nm is not apparent from declining；And in SO3 2-/S2O8 2-Under system effect, MO is whole
Absworption peak in oxidizing process at 473nm, 270 and 310nm is almost wholly absent, and azo bond absworption peak is substantially than benzene
Ring conjugated system declines fast.Equally from the point of view of infrared results, raw water MO is in 1460cm-1It is nearby the stretching vibration of azo bond
Peak, 1518cm-1It is nearby the C=C vibration absorption peaks on phenyl ring skeleton, 1118cm-1It is the connection of N atoms and phenyl ring C-N that position, which speculates,
Characteristic absorption peak, 1365cm-1It is-SO3 -Symmetric and unsymmetric vibration peak, and pass through SO3 2-/S2O8 2-From the point of view of system result,
1460cm-1Place's azo absorption of vibrations is almost wholly absent compared with raw water sample, 1518cm-1Locate the absworption peak and 1365cm of phenyl ring-1
Locate the obvious intensity decreases of characteristic peak.
It can be seen that SO3 2-Activate S2O8 2-During generate more active species (strong oxidizing property potentiometric titrations
SO4 ·—With inferior sulfate radical free radical SO3 ·-), its activating mechanism can be described by with formula (1).
S2O8 2-+SO3 2-→SO4 2-+SO4 ·-+SO3 ·- (1)
Due to SO4 ·-With very strong oxidation activity and higher electron affinity energy, head advances the higher idol of cloud density
Nitrogen groups, its single electron transfer change induction of lone pair electrons on azo to single electron, and what is formed is active containing four single electrons
Transition state combined rapidly with four protons, so as to form two amino, destroy MO azo structures, cause MO by SO4 ·-Drop
Solution, is converted into other products, MB concentration also decreases in solution.Its initial breakdown reaction mechanism is as shown in Figure 4.
Embodiment 3
Experimentation controls influences of the different mol ratio M to MO degradation rates, different initial pH to drop MO with embodiment 1
The influence of solution rate, different S2O8 2-Influence to degradation process of influence of the concentration to MO degradation rates, different initial MO concentration, difference
Influence of the treatment temperature to degradation process.
MO degradation rate part table 1 below under the conditions of differential responses：
Table 1
Fig. 5 is as reaction system MO initial concentrations CMO=60mg/L, temperature are room temperature, initial pH=3.0, are investigated respectively not
With mol ratio M=n (SO3 2-)：n(S2O8 2-) it is 5mM：5mM、2.5mM：5mM and 5mM：Change is degraded to MO in the range of 7.5mM
The influence of rate.As can be seen that in reaction 300min, work as SO3 2-Initial concentration from 0.25mM bring up to 0.5mM when, MO degradation rates are bright
It is aobvious to rise, increase to 74.6% from 20.3%.And fix n (SO3 2-) it is 5mM；With S2O8 2-Concentration further improves, MO drops
Solution rate has almost no change.This shows appropriate SO3 2-S can be promoted2O8 2-Activation, strengthen the degraded to MO, work as S2O8 2-It is excessive
When can to MO degrade play inhibitory action on the contrary.
Fig. 6 is n (SO3 2-)=n (S2O8 2-)=5.0mM, initial concentration CMOUnder the conditions of=60mg/L, under condition of different pH
The variation tendency of MO degradation rates.As a result show, as pH=2.0, its degradation rate is minimum, and reaction 300min is only reached
65.54%；And when pH scopes are 3.0-9.0, with the increase of initial pH value, MO clearance is in slightly downward trend,
When pH value is 3.0 degrade clearance be 87.63%, when pH value be 4.0 when, degraded clearance be 84.89%, compared with pH be 3.0 when
It is low.But the degraded clearance of methyl orange has also respectively reached 84.06%, 81.71% when pH value is 6.0,9.0.And pH value is
When 11.0, methyl orange degradation clearance be 84.82%, with pH be 4.0 when it is suitable, also illustrate that SO3 2-/S2O8 2-Activation system
It is wider to initial pH accommodation.
Fig. 7 is initial pH=3.0, MO initial concentrations CMO=60mg/L, fixed n (SO3 2-)/n(S2O8 2-)=1.0, it is different
S2O8 2-To the influence of MO degradation processes under concentration.As can be seen that in the S of investigation2O8 2-In concentration range, work as S2O8 2-Concentration is
During 5.0mM, after reacting 300min, MO degradation rates reach 53.9% from 0%.With S excessively2O8 2-Initial concentration increases from 5.0mM-
25.0mM, MO degradation rate also accordingly increase, and from 0to 84.7%, this also illustrates with S2O8 2-Increase, the activity of oxidisability
The increase that species are responded.Work as S2O8 2-Incrementss be 25mM preferably when, clearance is highest 95.6%.
Fig. 8 is initial pH=3.0, n (SO3 2-)=n (S2O8 2-Different initial MO concentration (10- 60mg/L) under)=5.0mM
Influence to degradation process.As seen from the figure, as the rise of MO concentration, its degradation rate are on a declining curve.When concentration is from 10mg/L
When rising to 60mg/L, it is known that its clearance of degrading of its reaction rate constant should successively decrease in gradient, from 2.4649E-4min-1Drop
As little as 1.8212E-4min-1.Because due to during the course of the reaction, because the SO added3 2-And S2O8 2-Amount it is identical, and MO
The increase of concentration, cause to produce competition between pollutant, degraded will thoroughly not increase intermediate species, and so also consume system
In caused SO4 ·-, cause the reduction of reaction rate.
Fig. 9 is that reaction temperature changes to 318k, initial pH=3.0, n (SO by 298K3 2-)=n (S2O8 2-)=5.0mM, MO
Initial concentration CMO=60mg/L, investigate affecting laws of the temperature to MO degradation efficiencies.As temperature raises, the reaction of oxidation system
Speed increases, and MO removal efficiency is also accordingly improved.With reference to Arrhenius formula (formula 7), experiment condition is tried to achieve in analysis
Under reaction activity Ea(kJ/mol)=44.9 kJ/mol.
Claims (5)
1. utilize the method for sodium sulfite activation persulfate degraded methyl orange azo dye wastewater, it is characterised in that the side
Method comprises the following steps：
Na is added into methyl orange azo dye wastewater2SO3And Na2S2O8, then add NaOH or H2SO4At the beginning of adjusting reaction system
Beginning pH to 2-11, heat, you can.
2. according to the method for claim 1, it is characterised in that regulation reaction system initial pH to 3-11.
3. method according to claim 1 or 2, it is characterised in that the heating is specially to be handled at 25-60 DEG C
60min。
4. method according to claim 1 or 2, it is characterised in that Na2SO3And Na2S2O8Mol ratio be 0.5-1:1.
5. according to the method described in claim any one of 1-4, it is characterised in that Na2S2O8Concentration is 5-25mM in waste water.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111441184A (en) * | 2020-05-08 | 2020-07-24 | 南通大学 | Dyeing textile washing method free of auxiliary agent, capable of removing foot water and floating color |
| CN112624298A (en) * | 2020-12-29 | 2021-04-09 | 四川大学 | Advanced treatment process and system for sewage |
| CN112897781A (en) * | 2021-03-08 | 2021-06-04 | 沈阳大学 | Method for degrading azo dye by synergy of ultrasonic-ultraviolet-semidry desulfurization ash |
| CN113501562A (en) * | 2021-08-03 | 2021-10-15 | 吉林建筑大学 | Photodegradant of carbamazepine, method and device for degrading carbamazepine |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111441184A (en) * | 2020-05-08 | 2020-07-24 | 南通大学 | Dyeing textile washing method free of auxiliary agent, capable of removing foot water and floating color |
| CN111441184B (en) * | 2020-05-08 | 2021-12-24 | 南通大学 | Dyeing textile washing method free of auxiliary agent, capable of removing foot water and floating color |
| CN112624298A (en) * | 2020-12-29 | 2021-04-09 | 四川大学 | Advanced treatment process and system for sewage |
| CN112624298B (en) * | 2020-12-29 | 2022-02-18 | 四川大学 | Advanced treatment process and system for sewage |
| CN112897781A (en) * | 2021-03-08 | 2021-06-04 | 沈阳大学 | Method for degrading azo dye by synergy of ultrasonic-ultraviolet-semidry desulfurization ash |
| CN113501562A (en) * | 2021-08-03 | 2021-10-15 | 吉林建筑大学 | Photodegradant of carbamazepine, method and device for degrading carbamazepine |
| US20230053646A1 (en) * | 2021-08-03 | 2023-02-23 | Jilin Jianzhu University | Photodedgradant for carbamazepine, method and apparatus for degrading carbamazepine |
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