CN108046407A - It is a kind of to use nano-CeO2/H2O2/O3The method of the acid used water difficult to degradate of system processing - Google Patents
It is a kind of to use nano-CeO2/H2O2/O3The method of the acid used water difficult to degradate of system processing Download PDFInfo
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- CN108046407A CN108046407A CN201711110906.9A CN201711110906A CN108046407A CN 108046407 A CN108046407 A CN 108046407A CN 201711110906 A CN201711110906 A CN 201711110906A CN 108046407 A CN108046407 A CN 108046407A
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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
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- 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
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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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- Environmental & Geological Engineering (AREA)
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- Treatment Of Water By Oxidation Or Reduction (AREA)
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Abstract
The invention discloses a kind of methods of heterocatalysis ozone hydrogen peroxide treatment of acidic wastewater.Using pyrolytic nitrate process synthetic catalyst.It is ceria with solid catalyst its ingredient used in X-ray diffraction analysis (XRD), x-ray photoelectron spectroscopy (XPS) analytical proof exists simultaneously Ce in the catalyst3+And Ce4+.The visible catalyst of scanning electron microscope (SEM) observation catalyst morphology is nanosphere aggregate.The catalyst synthesized with this method for the hardly degraded organic substance in heterocatalysis ozone hydrogen peroxide oxidation acid water (such as：Acetic acid) show good activity.Compared with prior art, the solid catalyst prepared by the present invention is prepared simple, and Catalyst Production is at low cost, and catalytic activity is high, has higher application value.
Description
(1) technical field
The present invention relates to field of waste water treatment more particularly to it is a kind of use nano-CeO2/H2O2/O3System processing is acid difficult
The method of degrading waste water.
Use nano-CeO2/H2O2/O3Recalcitrant chemicals in system efficient process acid waste water, specifically with receiving
Rice cerium oxide is as catalyst, the Recalcitrant chemicals in catalytic ozonation treatment of acidic wastewater.
(2) background technology
Since 21 century, with the development of industrialization and urbanization, environmental pollution situation is more and more severeer, industrial wastewater,
The problems such as city domestic sewage, rivers and lakes are polluted, causes great shadow to national economic development, ecological environment, human health
It rings.These waste water largely contain the recalcitrant pollutants such as polycyclic aromatic hydrocarbon, halogenated hydrocarbons, heterocycle compound, organic agricultural chemicals,
Traditional biological chemical method is difficult processing.High-level oxidation technology (advanced oxidation process, AOPs) is to show such as
The present handles organic used water difficult to degradate most one of method of application prospect.Including Fenton (H2O2/Fe2+), it is class Fenton, smelly
(ozone-based advanced oxidation process, are denoted as AOP-O to oxygen high-level oxidation technology below3), persulfuric acid
Salt high-level oxidation technology etc..
Ozone high grade oxidation technology has green, high rate, non-secondary pollution etc. a little, has in terms of sewage disposal well
Application prospect.Most of unsaturated and macromolecular fragrant type organic matters can directly and ozone reaction, but be usually associated with a large amount of
The generation of the by-products such as organic molecule acid, these by-products are difficult by ozone direct oxidation.Select suitable catalyst such as transition
Metal oxide CuO, MnO2、TiO2、Fe2O3The hydroxyl radical free radical (OH) of catalysis ozone generation more high oxidative is to grind at present
Study carefully the core content of ozone high grade oxidation.Ozone is easier to generation hydroxyl radical free radical in alkaline conditions, yet with organic acid
Generation, as the carry out solution of reaction often becomes acid so that degradation rate declines or even terminates.Ozone dioxygen water coincidence skill
Art so that ozone decomposes in acid condition and generates hydroxyl radical free radical.But efficiency is still relatively low.
Heterogeneous catalysis H in recent years2O2/O3System is one of hot spot of research.Titanium lewis acid, Titanium Sieve Molecular Sieve (TS-
1) and solid super-strong acid (SZF) be come this year we have found that the higher several catalyst of efficiency.On cerium oxide in this respect
Research be not yet reported that.This work is prepared for nano-cerium oxide, and finds that it is catalyzed H2O2/O3System is right in acid condition
The small molecule acid of difficult degradation has good removal effect.
(3) content of the invention
The shortcomings that it is an object of the invention to overcome existing ozone difficult degradation acid waste water, provides a kind of wastewater treatment side
Method, (pH≤5) energy efficient catalytic ozone generates hydroxyl radical free radical, and organic small point of difficult degradation of degrading to this method in acid condition
Sub- acid.It is expected to solve the intractable problem of ambient water process field acid waste water.
It is a kind of to use nano-CeO2/H2O2/O3The method of the acid used water difficult to degradate of system processing, comprises the following steps：
(1) nano-CeO is added in containing organic pollution, the acid waste water that pH is 1~52Solid catalyst and H2O2,
Stir evenly to obtain mixed liquor；The organic pollution for monocyclic and polycyclc aromatic compound, heterocyclic compound, aliphatic hydrocarbon and its
One or more mixing in derivative；The organic pollution, H2O2And nano-CeO2The mass ratio of solid catalyst is
1:0.5~4:0.2~3；
(2) ozone is passed through into mixed liquor and carries out degradation reaction, the waste water after being degraded.
H2O2/O3System is very low to the degradation rate of organic pollution in acid condition, nano-CeO2Addition carry significantly
High H2O2/O3System is in acid condition to the degradation rate of organic pollution.
The nano-CeO of the present invention2/H2O2/O3System has higher degrading activity to acid used water difficult to degradate；Described
Acid used water difficult to degradate is to contain other reluctant organic pollutions of ozone high grade oxidation technology, preferred fat hydrocarbon derivative
In small molecular organic acid waste water；The small molecular organic acid is preferably acetic acid.
Reluctant small molecular organic acid-acetic acid is employed in the embodiment of the present invention as organic pollution, in use
When stating method degradation acetic acid, the mechanism of action is acetic acid usually as the by-product during above-mentioned macromolecular organic pollutant degradation
Object occurs, and property is stablized, and under normal circumstances, the hydroxyl radical free radical of only superpower oxidisability can be oxidized decomposition.If in general,
Acetic acid can effectively be degraded, then it is believed that the larger molecular organics such as other organic pollutions, such as aliphatic, aromatic series also can quilt
Effective height is degraded.
In the waste water of the organic pollution for unknown concentration of degrading, the COD value of waste water need to be first surveyed, it can according to COD value of waste water
To estimate the quality of contained organic wastewater in waste water, so that it is determined that needing the H put into2O2And nano-CeO2The throwing of solid catalyst
Dosage.
Preferably, the nano-CeO2Solid catalyst is using six nitric hydrate Asia cerium oxide as precursor, using height
Warm the nano-cerium oxide of decomposition method synthesis.
It is further preferred that the nano-CeO2The preparation method of solid catalyst is：
(a) weigh cerium nitrate to be put into ceramic boat, be put into Muffle furnace, under air atmosphere, with 10 DEG C
min-1Heating rate be increased to 550 DEG C calcining 4h, obtain faint yellow solid；
(b) faint yellow solid in step (a) is fully ground up to the nano-CeO2Solid catalyst.
Preferably, in the mixed liquor of step (1), organic pollution, H2O2And nano-CeO2The mass ratio of solid catalyst
For 1:0.5~4:0.2~3；It is further preferred that organic pollution, H2O2And nano-CeO2The mass ratio of solid catalyst is
1:1~4:0.8~1.6；Most preferably, organic pollution, H2O2And nano-CeO2The mass ratio of solid catalyst is 1:2~4:
0.8。
Preferably, in step (2), the ozone is with O2/O3The form of mixed gas is passed through, mixed gas flow for 0.1~
0.6L·min-1, wherein ozone concentration is 1.4~39.2mgL-1。
Compared with prior art, wastewater treatment method of the invention has the following advantages：
(1) (pH≤5) can be incited somebody to action with efficient degradation acidity used water difficult to degradate, the utilization rate of ozone in acid condition
Organic pollution in acid waste water removes completely, avoids the secondary pollution of by-product；
(2)nano-CeO2Solid catalyst prepares simple, at low cost, the high catalytic efficiency of catalyst of synthesis, ozone utilization
Rate is high, and good degradation effect can be realized in less ozone dosage, and catalytic applications prospect is splendid.
(4) illustrate
Fig. 1 is the Experimental equipment of acetic acid in catalytic ozonation degradation water in embodiment；In figure, 1- oxygen bottles, 2-
Ozone generator, 3- flowmeters, 4- ozone reactors, 5- circulating cooling water outs, 6- feed inlets, 7- sample taps, 8- Xun Huans are cold
But water inlet, 71-Ozone Absorption device, 72-Ozone Absorption device, 8- sample taps, 9- discharge ports, 10.1,10.2- ozone are inhaled
Receiving apparatus.
Fig. 2 is nano-CeO2The XRD characterization figure of solid catalyst；
Fig. 3 is nano-CeO2The SEM phenograms of solid catalyst；
Fig. 4 is nano-CeO2The XPS phenograms of solid catalyst；
Fig. 5 is the contrast effect figure of different catalysts under the same terms.
Fig. 6 is CeO2It is catalyzed different system degradation acetic acid design sketch.
Fig. 7 is hydroxyl radical free radical yield comparison diagram in different systems.
(5) specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
Following embodiment carries out wastewater treatment using device shown in FIG. 1, which includes oxygen bottle 1, ozone is sent out
Raw device 2, flowmeter 3, ozone reactor 4, Ozone Absorption device 10.1,10.2, ozone breaker 11.It is the oxygen bottle 1, smelly
Oxygen Generator 2, flowmeter 3, ozone reactor 4, Ozone Absorption device 10.2, ozone breaker 11 are sequentially connected in series company by pipeline
It connects, the connecting line between the flowmeter 3 and ozone reactor 4 is equipped with two-way valve, and another access of two-way valve is connected with
Another Ozone Absorption device 10.1.The ozone reactor 4 is equipped with circulating cooling water inlet 8 and cooling water outlet 5, is connected with Xun Huan
Cooling water, the ozone reactor 4 are also equipped with feed inlet 6 and are equipped with sample tap 7, discharge port 9 in lower part at an upper portion thereof.It is described
Ozone Absorption device 10.1,10.2 uses most common form, two or more connected test tubes equipped with 2%KI solution
Or other containers.Ozone generator model CFS-1A, destructor model ODF-003, contact material is 316L stainless steels, smelly
Oxygen reactor is simple glass, and internal diameter 5cm, high 75cm, the sand core of ozone reactor bottom is step device of air, and connecting line is adopted
Use silicone tube.
Ozone reactor first is cleaned with secondary deionized water before reaction, with ozone pretreatment 5min, after emptying, use is secondary
Deionized water rinsing reactor is twice.Pending waste water solution deionized water configuration is placed in ozone reactor 4, to ozone
Reactor 4 puts into proper catalyst.During reaction, the oxygen flowed out from oxygen bottle 1 is given birth to as unstripped gas by ozone generator
Into ozone, O is obtained2/O3Mixed gas controls inlet gas ozone by adjusting discharge power and the gas flow of ozone generator
Concentration opens the two-way valve of connection ozone reactor, O2/O3Mixed gas enters in reactor to react with waste water, and degradation is useless
Water, the O after ozone reactor2/O3Mixed gas is left from reactor head, is broken by Ozone Absorption device 10.2, ozone
It is discharged into after bad device 11 in air.During reaction, analyzed at regular intervals from sample tap sampling, water sample nitrogen bubbling
3min terminates the oxidation reaction of ozone.
After reaction, the two-way valve of connection Ozone Absorption device 10.1 is opened, absorbs ozone tail gas with 2%KI solution.
nano-CeO2The preparation of solid catalyst：
(1) 5g cerium nitrates are weighed to be put into ceramic boat；
(2) sample weighed in step (1) is put into Muffle furnace, under air atmosphere, with 10 DEG C of min-1Heating
Rate is increased to 550 DEG C of calcining 4h, obtains faint yellow solid；
(3) faint yellow solid in step (2) is transferred to after being fully ground in agate mortar and stored, nano- is prepared
CeO2Solid catalyst, XRD characterization figure, SEM phenograms, XPS phenograms are as in Figure 2-4.In XRD diagram, marked by comparing
Quasi- CeO2The catalyst component that card illustrates to prepare is CeO2, nanometer pelletizing that the visible catalyst of SEM figures is 10-50nm
Polymers has higher specific surface area.X-ray photoelectron spectroscopic analysis (XPS) illustrate prepared CeO2Have in catalyst compared with
More Ce3+Presence, it is meant that catalyst has many Lacking oxygens, and catalytic activity is higher.
In following embodiment, the detection method of acetic acid concentration：PH value is measured with pH precision acidity meters；In solution acetate from
The concentration of son is surveyed using high performance liquid chromatography UltiMate 3000 (ThermoFisher Dionex Ultimate3000, USA)
It is fixed, separate column type number：C18 columns (250 × 4.6mm, particle size 5mm), leacheate are that the phosphate of 0.0134mol delays
The mixture of fliud flushing (pH=3) and methanol (950:50, V:V), flow velocity 1.20mLmin-1, ultraviolet detection wavelength is 210nm.
Embodiment 1
By the above-mentioned finished catalyst prepared for Catalytic Ozonation acetic acid waste water (acetic acid concentration 100mg/L,
Reaction solution volume is 250ml, remaining is water).The dosage of catalyst is 0.08g/L, and the dosage of hydrogen peroxide is 100mg/
L, then solution ph is transferred to 3.0 with sulfuric acid.Experiment is using half batch processing mode, in O2/O3Gaseous mixture flow velocity is 0.1L/min,
Ozone output carries out under the conditions of being 9.9mg/min, sampling detection when 30min is reacted in experiment.
Comparative example 1~4
As a comparison, under same experimental conditions, following 4 groups of contrast tests has been done, have been H respectively2O2/O3、CeO2/O3、
CeO2/H2O2/O2、CeO2/O2System is degraded with the acetic acid solution of concentration.
Acetic acid concentration (initial concentration 100mg/L) is as shown in table 1 when water sample handles 30min.
Table 1
Embodiment 2~4
The above-mentioned finished catalyst prepared is used to be catalyzed H2O2/O3Acetic acid of degrading waste water (acetic acid concentration 100mg/L,
H2O2Dosage is 100mg/L, and reaction solution volume is 250ml, remaining is water).The dosage of catalyst is 0.08g/L, and experiment is adopted
With half batch processing mode, in O2/O3Gaseous mixture flow velocity is 0.1L/min, and ozone output is carried out under the conditions of being 9.9mg/min, tested
Sampling detection when reacting 30min.
Solution ph is transferred to 1.0,5.0,7.0 by embodiment 2~4 respectively with sulfuric acid respectively, and other conditions are the same as embodiment 1.
Acetic acid concentration (initial concentration 100mg/L) is as shown in table 2 when water sample handles 30min.
Table 2
| Embodiment | Embodiment 2 | Embodiment 1 | Embodiment 3 | Embodiment 4 |
| Acetic acid concentration (mg/L) | 88.84 | 32.42 | 53.62 | 4.57 |
Embodiment 5~8
By the above-mentioned finished catalyst prepared for Catalytic Ozonation acetic acid waste water (acetic acid concentration 100mg/L,
H2O2Dosage is 100mg/L, and reaction solution volume is 250ml, remaining is water).Again respectively with sulphur acid for adjusting pH value to 3.0.Experiment
Using half batch processing mode,
In O2/O3Gaseous mixture flow velocity is 0.1L/min, and ozone output carries out under the conditions of being 9.9mg/min, experiment reaction
Detection is sampled during 30min.
The dosage of catalyst is respectively 0.02g/L, 0.04g/L, 0.16g/L, 0.32g/L in embodiment 5~8, other
Condition is the same as embodiment 1.
Acetic acid concentration (initial concentration 100mg/L) is as shown in table 3 when water sample handles 30min.
Table 3
Embodiment 9~12
By the above-mentioned finished catalyst prepared for Catalytic Ozonation acetic acid waste water (acetic acid concentration 100mg/L,
H2O2Dosage is 100mg/L, and reaction solution volume is 250ml, remaining is water).The dosage of catalyst is 0.08g/L, then uses sulphur
Acid for adjusting pH value is to 3.0.Experiment is using half batch processing mode, in O2/O3Gaseous mixture flow velocity carries out under conditions of being 0.1L/min,
Sampling detection during experiment reaction 30min.
The ozone output of embodiment 9~12 be 1.4mg/min, 4.5mg/min, 20.2mg/min, 39.2mg/min, other
Condition is the same as embodiment 1.
Acetic acid concentration (initial concentration 100mg/L) is as shown in table 4 when water sample handles 30min.
Table 4
Embodiment 13~15
By the above-mentioned finished catalyst prepared for Catalytic Ozonation acetic acid waste water (acetic acid concentration 100mg/L,
Reaction solution volume is 250ml, remaining is water).The dosage of catalyst is 0.08g/L, then is arrived respectively with sulphur acid for adjusting pH value
3.0.Experiment is using half batch processing mode, in O2/O3Gaseous mixture flow velocity is 0.1L/min, under the conditions of ozone output is 9.9mg/min
It carries out, sampling detection when 30min is reacted in experiment.
H in embodiment 13~152O2Dosage is respectively 50mg/L, 200mg/L, 400mg/L, the same embodiment of other conditions
1。
Acetic acid concentration (initial concentration 100mg/L) is as shown in table 5 when water sample handles 30min.
Table 5
Embodiment 16
By the above-mentioned finished catalyst prepared, for Catalytic Ozonation nitrobenzene waste water, (nitro phenenyl concentration is
100mg/L, reaction solution volume are 500ml, remaining is water).The dosage of catalyst is 0.08g/L, then is adjusted respectively with sulfuric acid
PH value is to 3.0.Experiment is using half batch processing mode, in O2/O3Gaseous mixture flow velocity is 0.1L/min, ozone output 9.9mg/min
Under the conditions of carry out, experiment reaction 5min, 10min, 20min, sampling detection nitro phenenyl concentration when 30min, 40min, and survey COD.
| Example 16 | 0min | 5min | 10min | 20min | 30min | 40min |
| Nitro phenenyl concentration (mg/L) | 100 | 50.92 | 25.25 | 0.4572 | 0 | 0 |
| COD(mg/L) | 190.1 | 151.6 | 84 | 54 | 48 | 32 |
Claims (8)
1. a kind of use nano-CeO2/H2O2/O3The method of the acid used water difficult to degradate of system processing, which is characterized in that including following
Step：
(1) nano-CeO is added in containing organic pollution, the acid waste water that pH is 1~52Solid catalyst and H2O2, stirring
It is uniform to obtain mixed liquor；The organic pollution is monocyclic or polycyclc aromatic compound, heterocyclic compound, aliphatic hydrocarbon and its derivative
One or more mixing in object；The organic pollution, H2O2And nano-CeO2The mass ratio of solid catalyst is 1:0.5
~4:0.2~3；
(2) ozone is passed through into mixed liquor and carries out degradation reaction, the waste water after being degraded.
2. according to claim 1 use nano-CeO2/H2O2/O3The method of the acid used water difficult to degradate of system processing, it is special
Sign is：The nano-CeO2Solid catalyst is using six nitric hydrate Asia cerium oxide as precursor, using high temperature thermal decomposition
The nano-cerium oxide of method synthesis.
3. according to claim 2 use nano-CeO2/H2O2/O3The method of the acid used water difficult to degradate of system processing, it is special
Sign is, the nano-CeO2The preparation method of solid catalyst is：(a) weigh cerium nitrate and be put into ceramic boat
In, it is put into Muffle furnace, under air atmosphere, with 10 DEG C of min-1Heating rate be increased to 550 DEG C calcining 4h, obtain yellowish
Color solid；
(b) faint yellow solid in step (a) is fully ground up to the nano-CeO2Solid catalyst.
4. use nano-CeO according to described in claim 12/H2O2/O3The method of system treatment of acidic wastewater, which is characterized in that
In the mixed liquor of step (1), the organic pollution, H2O2And nano-CeO2The mass ratio of solid catalyst is 1:1~4:0.8
~1.6.
5. use nano-CeO according to described in claim 12/H2O2/O3The method of system treatment of acidic wastewater, which is characterized in that
In step (2), the ozone is with O2/O3The form of mixed gas is passed through, and mixed gas flow is 0.1~0.6Lmin-1,
Middle ozone concentration is 1.4~39.2mgL-1。
6. use nano-CeO according to described in claim 12/H2O2/O3The method of the acid used water difficult to degradate of system processing, feature
It is：The organic pollution is fatty hydrocarbon derivative.
7. use nano-CeO according to described in claim 62/H2O2/O3The method of the acid used water difficult to degradate of system processing, feature
It is：The fat hydrocarbon derivative is small molecular organic acid.
8. use nano-CeO according to described in claim 72/H2O2/O3The method of the acid used water difficult to degradate of system processing, feature
It is：The small molecular organic acid is acetic acid.
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| CN110115994A (en) * | 2019-05-15 | 2019-08-13 | 杭州诚洁环保有限公司 | A kind of activated carbon supported CeO2-xCatalyst and its preparation method and application |
| CN111977776A (en) * | 2020-08-28 | 2020-11-24 | 吉林大学 | Catalytic ozonation-based pretreatment method for acidic wastewater containing difficultly-degradable water-soluble polymers |
| CN113307348A (en) * | 2020-02-27 | 2021-08-27 | 深圳市长隆科技有限公司 | Method for advanced treatment of methyl parathion wastewater |
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| CN111977776B (en) * | 2020-08-28 | 2023-01-24 | 吉林大学 | Catalytic ozonation-based pretreatment method for acidic wastewater containing difficultly-degradable water-soluble polymers |
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