CN108455718A - A kind of biodegrading process of organic pollution - Google Patents
A kind of biodegrading process of organic pollution Download PDFInfo
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- CN108455718A CN108455718A CN201810205620.7A CN201810205620A CN108455718A CN 108455718 A CN108455718 A CN 108455718A CN 201810205620 A CN201810205620 A CN 201810205620A CN 108455718 A CN108455718 A CN 108455718A
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- China
- Prior art keywords
- organic pollution
- water
- biodegrading process
- nickel oxide
- nickel
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses a kind of to activate persulfate to generate the method that potentiometric titrations are used for organic pollution fast degradation using nickel oxide, be related to it is a kind of processing organic wastewater with difficult degradation thereby in terms of application, the catalyst, it is made by hydrothermal synthesis method, then the catalyst of preparation is put into the waste water containing organic pollution, persulfate is added again, and the reaction system all shows very excellent mineralization ability and stability in pH ranges 3~10.Method for preparing catalyst of the present invention is simple and practicable；The reaction system is cheap, and property is stablized, and industrial applications are conducive to.
Description
Technical field
The present invention relates to a kind of biodegrading process of organic pollution, belong to field of water treatment technology application.
Background technology
In recent years, with economic and industry fast development, the ecological environment in China is by serious harm.Various dyes
The use of material, herbicide, antibiotic and disinfectant etc. causes a large amount of poisonous and harmful and Recalcitrant chemicals to enter environment body
System so that water body is stained significantly, to cause serious damage, the mankind to the balance of human health and the entire ecosystem
The Faced In Sustainable Development of society stern challenge.
Traditional sewage disposal technology, such as bioanalysis, chemical electrolysis method, Physical are difficult to reach the requirement of processing,
Only this pollutant, just because of this, high-level oxidation technology could be thoroughly removed using the oxidant with stronger oxidability
Because it has the ability of organic pollution permineralization, meanwhile, strong, the applied widely and reaction speed with oxidability
The advantages that fast, becomes one of the effective ways of organic wastewater with difficult degradation thereby improvement.
In high-level oxidation technology, Fenton technologies are stablized, are simple, having application advantage relatively, get the attention.
Traditional Fenton-like system, core are to generate strong oxidizer OH (E based on ferrous catalyzing hydrogen peroxide0=1.8~2.7V) it removes
Organic pollution.However, there are still a series of shortcomings, such as catalytic effect to be influenced by pH for traditional Fenton-like system, it is right
H2O2Utilization rate it is low, and water outlet in often contain a large amount of Fe2+Iron containing sludge is easily generated, secondary pollution etc. is caused.It compares
In OH, SO4 2-As a kind of strong oxidizer, there is higher oxidation-reduction potential (E0=2.6V), broader pH is applicable in model
Enclose makes it be increasingly becoming a kind of high-level oxidation technology of novel great development prospect with longer survival service life, these advantages.
Currently, single persulfate (PMS) and persulfate (PS) are to generate SO4 2-Common oxidant, conventional activation PMS and PS
Generate SO4 2-Method include mainly ultraviolet light, thermal energy, microwave method and transition metal ion catalyst etc..However, physics
Method energy consumption is high, causes cost excessively high, limits its promotion and application significantly；In contrast, the catalyst such as transition metal ions are lived
Change can quickly carry out under room temperature, normal pressure, and need not add additional energy, be increasingly becoming the hot spot of research.At present
Studies have shown that most of transition metal ion catalyst, which can only be catalyzed PMS, generates SO4 2-, wherein Co2+It is best activation PMS
Catalyst, the system is high to the mineralization rate of organic matter, oxidability is strong, reaction speed is fast, and not carbonate suspension and villaumite
Deng influence.But Co2+Strong carcinogenesis limits the extensive use of the system, and PMS is compared to PS, price phase
To higher, and stability is poor, and therefore, developing the novel catalyst for capableing of effective activation PS becomes the research of researcher
Hot spot.
Invention content
It is only applicable to narrow pH ranges about traditional Fenton-like system for what is be previously mentioned in background above technology, it is common
Fenton-like, such as Co2+/ PMS, due to Co2+Toxicity is high, PMS higher prices and chemical stability is relatively poor limits it
The defects of popularization and application, the purpose of the present invention is be to have synthesized a kind of less toxic, efficient, stable and cheap nickel oxide to urge
Agent efficiently can generate SO by fast activating PS within the scope of very wide in range pH4 -, realize and organic contamination difficult to degrade gone
It removes.
The present invention is achieved by the following technical solutions：
The present invention provides a kind of biodegrading process of organic pollution comprising following steps：
Prepare nickel oxide powder；
The nickel oxide powder is put into the solution containing organic pollution, and puts into persulfate, stirring carries out
Degradation reaction realizes the mineralising to the organic pollution；
Wherein, the preparation method of the nickel oxide powder is：
Water soluble nickel salt and urea are dissolved in the mixed solution of water and ethylene glycol, after mixing, water is carried out at 120 DEG C
Thermal response obtains nickel hydroxide；
The nickel hydroxide is annealed, nickel oxide powder is obtained.
Preferably, the water soluble nickel salt and the molar ratio of urea are 1:4, the temperature of the annealing is 350~
550℃。
Preferably, in the mixed solution of the water and ethylene glycol, the volume ratio of water and ethylene glycol is 1:1.
Preferably, a concentration of 0.06mol/L of the water soluble nickel salt in the mixed solution of water and ethylene glycol,
Concentration 0.25mol/L of the urea in water and ethylene glycol mixed solution.
Preferably, a concentration of 0~50mg/L of the organic pollution.
Preferably, the organic pollution includes at least one of phenol, bisphenol-A and tetracycline.
Preferably, the dosage of the nickel oxide powder is 0.5~1.0g/L.
Preferably, the dosage of the persulfate is 0.5~2.0g/L.
Preferably, the pH value of the degradation reaction is 3~10.
Preferably, the water soluble nickel salt is nickel nitrate.
Meaning of the present invention is, overcomes traditional Fenton-like system and is only applicable to narrow pH ranges and common
Fenton-like, such as Co2+/ PMS, due to Co2+Toxicity is high, PMS higher prices and chemical stability is relatively poor limits it
The defects of popularization and application, the present invention use nickel hydroxide as precursor, anneal at high temperature, it is made to be transformed into chemical property more
Stable nickel oxide is used for catalytic activation PS oxidants, generates SO4 -Degradation for organic pollution.Meanwhile passing through sintering
The nickel oxide of preparation, stable structure, acid resistance enhance, and in reaction process, can effectively reduce the loss of Ni metals, and then keep
The stability of catalyst.The mechanism of action of such Fenton catalyst system and catalyzing-NiO/PS is as follows：
Ni(II)+S2O8 2-→Ni(III)+SO4 2-+·SO4 - (1)
Ni(III)+S2O8 2-→Ni(II)+·S2O8 - (2)
·S2O8 -+SO4 2-→·SO4 -+S2O8 2- (3)。
Compared with prior art, the present invention has following advantageous effect：
1, the nickel oxide that the present invention uses, property is more stablized after sintering, while still in store flaky nanometer structure, has
Conducive to catalyst combined with pollutant and PS, while Ni numbers of dropouts are extremely low, will not cause secondary pollution；
2, preparation method is simple for the nickel oxide that the present invention uses, and is easy to implement；
3, the nickel oxide that the present invention uses while constantly activation PS, is particularly easy to realize Ni in catalytic process
(II) cycle of/Ni (III), ensure that the recycling of catalyst；
4, the oxidant that the present invention uses is PS, and relative to PMS, price is cheaper, and property is more stablized, and is more advantageous to
Industrial applications；
5, the NiO/PS systems that the present invention uses all show very excellent performance in pH ranging from 3~10, wherein
In acid condition, efficient catalytic effect is still shown；
6, the NiO/PS systems that the present invention uses have very high degradation efficiency, remineralization efficacy to hardly degraded organic substance
Obviously.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the XRD characterization schematic diagram of the nickel oxide used in the embodiment of the present invention 1；
Fig. 2 is that the TEM of the nickel oxide used in the embodiment of the present invention 1 characterizes schematic diagram；
Fig. 3 is NiO/PS systems in the embodiment of the present invention 1,2 and 3 to bisphenol-A degradation schematic diagram；
Fig. 4 is NiO/PS systems in the embodiment of the present invention 1,2 and 3 to bisphenol-A mineralization ability schematic diagram；
Fig. 5 is that the TEM after the NiO reactions used in the embodiment of the present invention 1 characterizes schematic diagram.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
1, the preparation of nickel oxide：
(1) by Ni (NO3)2·6H2O and urea are dissolved in the mixed solution of water and ethylene glycol, one timing of magnetic agitation
Between make its be uniformly mixed.
(2) above-mentioned solution is transferred in water heating kettle, puts and keep 4h at 120 DEG C in an oven, waits for that reaction kettle is cooled to room
Wen Hou, by obtained product water and ethyl alcohol, alternately washing centrifuges three times, then by being dried in vacuo and grinding obtained hydroxide
Nickel.
(3) nickel hydroxide obtained is annealed in Muffle furnace high temperature, nickel oxide powder is finally made.
Ni (NO described in step 13)2·6H2The molar ratio of O and urea is 1:3.
The volume ratio of water described in step 1 and ethylene glycol is 1:0.5.
Ni (NO described in step 13)2·6H2A concentration of 0.04mol/Ls and urea of the O in water and ethylene glycol mixed solution
Concentration 0.20mol/L in water and ethylene glycol mixed solution.
The annealing temperature in Muffle furnace of nickel hydroxide described in step 1 is 450 DEG C, annealing time 5h.
Catalyst 60 DEG C of dry 4h in vacuum drying chamber obtained described in step 1.
Nickel oxide described in step 1, as shown in Figure 1, Jade spectrogram (No.47- of its peak XRD with standard oxidation nickel
1049) completely corresponding, show that catalyst has good crystal property.As seen in Figure 2, porous receive is presented in nickel oxide
Rice laminated structure.
2, nickel oxide powder obtained is put into the solution of bisphenol-A, meanwhile, a certain amount of PS is put into, in certain pH
Under the conditions of, it is stirred to react certain time, realizes the mineralising to organic pollution.
A concentration of 50mg/L of bisphenol-A described in step 2.
The dosage of catalyst described in step 2 is 0.5g/L.
The additive amount of PS described in step 2 is 0.5g/L.
PH described in step 2 is 10, and different pH are adjusted by hydrochloric acid and sodium hydroxide solution.
After being stirred to react 20min described in step 2, pollutant is completely degraded (as shown in Figure 3).
Pollutant can almost be completely removed described in step 2, mineralization rate reaches 87% or more (as shown in Figure 4).
3, the catalyst after reacting is centrifuged, after alternately being washed three times with water and ethyl alcohol, vacuum drying, with this time
Receive the degradation that nickel oxide is re-used for organic pollution.
Catalyst 60 DEG C of dry 4h in vacuum drying chamber obtained described in step 3.
Catalyst system and catalyzing described in step 3 recycles contaminant degradation four times, can still reach 100% removal efficiency.
Catalyst described in step 3, after reaction four times, flaky nanometer structure is still presented in pattern, shows catalyst
It is with good stability (as shown in Figure 5).
Embodiment 2
1, the preparation of nickel oxide：
(1) by Ni (NO3)2·6H2O and urea are dissolved in the mixed solution of water and ethylene glycol, one timing of magnetic agitation
Between make its be uniformly mixed.
(2) above-mentioned solution is transferred in water heating kettle, puts and keep 4h at 120 DEG C in an oven, waits for that reaction kettle is cooled to room
Wen Hou, by obtained product water and ethyl alcohol, alternately washing centrifuges three times, then by being dried in vacuo and grinding obtained hydroxide
Nickel.
(3) nickel hydroxide obtained is annealed in Muffle furnace high temperature, finally obtained sheet nickel oxide powder.
Ni (NO described in step 13)2·6H2The molar ratio of O and urea is 1:3.
The volume ratio of water described in step 1 and ethylene glycol is 1:0.5.
Ni (NO described in step 13)2·6H2A concentration of 0.04mol/Ls and urea of the O in water and ethylene glycol mixed solution
Concentration 0.20mol/L in water and ethylene glycol mixed solution.
The annealing temperature in Muffle furnace of nickel hydroxide described in step 1 is 350 DEG C, annealing time 6h.
Catalyst 60 DEG C of dry 5h in vacuum drying chamber obtained described in step 1.
2, nickel oxide powder obtained is put into the solution of bisphenol-A, meanwhile, a certain amount of PS is put into, in certain pH
Under the conditions of, it is stirred to react certain time, realizes the mineralising to organic pollution.
A concentration of 50mg/L of bisphenol-A described in step 2.
The dosage of catalyst described in step 2 is 0.5g/L.
The additive amount of PS described in step 2 is 1g/L.
PH described in step 2 is 7, and different pH are adjusted by hydrochloric acid and sodium hydroxide solution.
After being stirred to react 30min described in step 2, pollutant is completely degraded (as shown in Figure 3).
Pollutant can almost be completely removed described in step 2, mineralization rate reaches 85% or more (as shown in Figure 4).
3, the catalyst after reacting is centrifuged, after alternately being washed three times with water and ethyl alcohol, vacuum drying, with this time
Receive the degradation that nickel oxide is re-used for organic pollution.
Catalyst 60 DEG C of dry 5h in vacuum drying chamber obtained described in step 3.
Catalyst system and catalyzing described in step 3 recycles contaminant degradation four times, can still reach 100% removal efficiency.
Embodiment 3
1, the preparation of nickel oxide：
(1) by Ni (NO3)2·6H2O and urea are dissolved in the mixed solution of water and ethylene glycol, one timing of magnetic agitation
Between make its be uniformly mixed.
(2) above-mentioned solution is transferred in water heating kettle, puts and keep 4h at 120 DEG C in an oven, waits for that reaction kettle is cooled to room
Wen Hou, by obtained product water and ethyl alcohol, alternately washing centrifuges three times, then by being dried in vacuo and grinding obtained hydroxide
Nickel.
(3) nickel hydroxide obtained is annealed in Muffle furnace high temperature, nickel oxide powder is finally made.
Ni (NO described in step 13)2·6H2The molar ratio of O and urea is 1:5.
The volume ratio of water described in step 1 and ethylene glycol is 1:1.5.
Ni (NO described in step 13)2·6H2A concentration of 0.08mol/Ls and urea of the O in water and ethylene glycol mixed solution
Concentration 0.30mol/L in water and ethylene glycol mixed solution.
The annealing temperature in Muffle furnace of nickel hydroxide described in step 1 is 550 DEG C, annealing time 4h.
Catalyst 60 DEG C of dry 6h in vacuum drying chamber obtained described in step 1.
2, nickel oxide powder obtained is put into the solution of bisphenol-A, meanwhile, a certain amount of PS is put into, in certain pH
Under the conditions of, it is stirred to react certain time, realizes the mineralising to organic pollution.
A concentration of 50mg/L of bisphenol-A described in step 2.
The dosage of catalyst described in step 2 is 0.5g/L.
The additive amount of PS described in step 2 is 2g/L.
PH described in step 2 is 3, and different pH are adjusted by hydrochloric acid and sodium hydroxide solution.
After being stirred to react 50min described in step 2, pollutant is completely degraded (as shown in Figure 3).
Pollutant can almost be completely removed described in step 2, mineralization rate reaches 80% or more (as shown in Figure 4).
3, the catalyst after reacting is centrifuged, after alternately being washed three times with water and ethyl alcohol, vacuum drying, with this time
Receive the degradation that nickel oxide is re-used for organic pollution.
Catalyst 60 DEG C of dry 6h in vacuum drying chamber obtained described in step 3.
Catalyst system and catalyzing described in step 3 recycles contaminant degradation four times, can still reach 100% removal efficiency.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (10)
1. a kind of biodegrading process of organic pollution, which is characterized in that include the following steps：
Prepare nickel oxide powder；
The nickel oxide powder is put into the solution containing organic pollution, and puts into persulfate, stirring is degraded
The mineralising to the organic pollution is realized in reaction；
Wherein, the preparation method of the nickel oxide powder is：
Water soluble nickel salt and urea are dissolved in the mixed solution of water and ethylene glycol, after mixing, it is anti-that hydro-thermal is carried out at 120 DEG C
It answers, obtains nickel hydroxide；
The nickel hydroxide is annealed, nickel oxide powder is obtained.
2. the biodegrading process of organic pollution as described in claim 1, which is characterized in that the water soluble nickel salt and urea
Molar ratio is 1:4, the temperature of the annealing is 350~550 DEG C.
3. the biodegrading process of organic pollution as described in claim 1, which is characterized in that the mixing of the water and ethylene glycol is molten
In liquid, the volume ratio of water and ethylene glycol is 1:(0.5~1.5).
4. the biodegrading process of organic pollution as described in claim 1, which is characterized in that the water soluble nickel salt is in water and second
A concentration of 0.04~0.08mol/L in the mixed solution of glycol, concentration 0.20 of the urea in water and ethylene glycol mixed solution
~0.30mol/L.
5. the biodegrading process of organic pollution as described in claim 1, which is characterized in that the organic pollution it is a concentration of
0~50mg/L.
6. the biodegrading process of the organic pollution as described in claim 1 or 5, which is characterized in that the organic pollution includes
At least one of phenol, bisphenol-A and tetracycline.
7. the biodegrading process of organic pollution as described in claim 1, which is characterized in that the dosage of the nickel oxide powder
For 0.5~1.0g/L.
8. the biodegrading process of organic pollution as described in claim 1, which is characterized in that the dosage of the persulfate is
0.5~2.0g/L.
9. the biodegrading process of organic pollution as described in claim 1, which is characterized in that the pH value of the degradation reaction is 3
~10.
10. the biodegrading process of organic pollution as described in claim 1, which is characterized in that the water soluble nickel salt is nitric acid
Nickel.
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Cited By (5)
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|---|---|---|---|---|
| CN109012720A (en) * | 2018-10-24 | 2018-12-18 | 天津理工大学 | A kind of preparation method and application of the catalyst for phenol wastewater of degrading |
| CN111468067A (en) * | 2020-04-27 | 2020-07-31 | 吉林化工学院 | Preparation and application of metal oxide NiO |
| CN112403471A (en) * | 2020-11-30 | 2021-02-26 | 华东师范大学 | Preparation method and application of hydrangea-shaped nickel oxide microsphere catalyst |
| CN112871174A (en) * | 2021-02-04 | 2021-06-01 | 华东师范大学 | Preparation method and application of hexagonal flaky nano nickel oxide catalyst |
| CN112973696A (en) * | 2021-02-05 | 2021-06-18 | 合肥工业大学 | Preparation method and application of Ni @ NiO heterojunction two-dimensional sheet-shaped nanomaterial |
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Cited By (7)
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|---|---|---|---|---|
| CN109012720A (en) * | 2018-10-24 | 2018-12-18 | 天津理工大学 | A kind of preparation method and application of the catalyst for phenol wastewater of degrading |
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| CN112403471A (en) * | 2020-11-30 | 2021-02-26 | 华东师范大学 | Preparation method and application of hydrangea-shaped nickel oxide microsphere catalyst |
| CN112871174A (en) * | 2021-02-04 | 2021-06-01 | 华东师范大学 | Preparation method and application of hexagonal flaky nano nickel oxide catalyst |
| CN112973696A (en) * | 2021-02-05 | 2021-06-18 | 合肥工业大学 | Preparation method and application of Ni @ NiO heterojunction two-dimensional sheet-shaped nanomaterial |
| CN112973696B (en) * | 2021-02-05 | 2022-04-01 | 合肥工业大学 | Preparation method and application of Ni @ NiO heterojunction two-dimensional sheet-shaped nanomaterial |
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Application publication date: 20180828 |