CN105540985A - Method for degrading organic wastewater by hydroxylamine hydrochloride reinforced iron oxide activated persulfate - Google Patents
Method for degrading organic wastewater by hydroxylamine hydrochloride reinforced iron oxide activated persulfate Download PDFInfo
- Publication number
- CN105540985A CN105540985A CN201510984805.9A CN201510984805A CN105540985A CN 105540985 A CN105540985 A CN 105540985A CN 201510984805 A CN201510984805 A CN 201510984805A CN 105540985 A CN105540985 A CN 105540985A
- Authority
- CN
- China
- Prior art keywords
- ferriferous oxide
- waste water
- oxammonium hydrochloride
- iron oxide
- persulphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
-
- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- 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 method for degrading organic wastewater by hydroxylamine hydrochloride reinforced iron oxide activated persulfate, and belongs to the technical field of water treatment. The method comprises the following specific steps: mixing hydroxylamine hydrochloride with wastewater to be pretreated; regulating pH (potential of hydrogen) to weak acidity; adding iron oxide and persulfate, and stirring at room temperature until reaction is complete; separating and recovering the iron oxide by adopting an external magnetic field to obtain purified wastewater, wherein proportion of organic matter to hydroxylamine hydrochloride to the iron oxide to the persulfate in the wastewater is 1 mmol: (5 to 10 mmol): 5mg: (10 to 30 mmol). A sulfate radical anion with strong oxidizing property is generated by the hydroxylamine hydrochloride reinforced iron oxide activated persulfate, therefore organic pollutants in a water body are removed. By adopting the method disclosed by the invention to remove the organic pollutants in the water, a removal rate can reach 70 percent to 99 percent in 30 minutes. The method disclosed by the invention is simple to operate, high in efficiency and low in operating cost, and has a broad application prospect in the field of advanced wastewater treatment.
Description
Technical field
The invention belongs to water-treatment technology field, relate to the method for a kind of oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water.
Background technology
In environment, the process of organic wastewater with difficult degradation thereby is the difficult point in water technology always for a long time, and for waste water from dyestuff, its high pollution, difficult degradation, total emission volumn are large.At present, the treatment process that combines with biological process of industrial usual employing chemical method.But mostly complicated operation, treatment effect also time have pessimistic.
High-level oxidation technology, refers to and utilizes the reaction such as strong oxidizing property free radical and pollutent generation addition, replacement, scission of link, open loop, makes organism be converted into the small-molecule substance of easily degraded.High-level oxidation technology based on potentiometric titrations is the oxidative degradation new technology of rising in recent years.Under room temperature persulphate by light, heat, transition metal (as Fe
2+) etc. activation method produce potentiometric titrations and hydroxyl radical free radical oxidative degradation pollutent.
Fe
2+as the metal ion that occurring in nature the most extensively exists, in persulphate activation, application is general.But Fe
2+react with persulphate and be exceedingly fast, and SO4
-transformation period very short again
[5], thus limit [Fe
2+]/[persulphate] oxidation system is to the degraded of pollutent; On the other hand, in reaction process along with Fe
3+generation can produce a large amount of iron mud, the subsequent disposal of iron mud is also a great problem in water treatment.
Summary of the invention
The present invention is in order to solve existing [Fe
2+]/[persulphate] the too fast and restriction of oxidation system oxidizing reaction to the degradation rate of pollutent and the problem producing a large amount of pending iron mud, provide a kind of oxammonium hydrochloride to strengthen the method for ferriferous oxide activation persulphate degradation of organic waste water.
The present invention is by the following technical solutions:
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
(1) oxammonium hydrochloride is mixed with pretreated waste water;
(2) regulate reaction pH to slightly acidic;
(3) add ferriferous oxide and persulphate, stirred at ambient temperature reacts completely;
(4) waste water after being namely purified after adopting foreign field Separation and Recovery ferriferous oxide;
The ratio of useless Organic substance in water, oxammonium hydrochloride, ferriferous oxide, persulphate is 1mmol:5-10mmol:5mg:10-30mmol.
As preferably, persulphate is at least one in potassium hydrogen persulfate or hydrogen persulfate sodium.
As preferably, described ferriferous oxide is at least one in Z 250, ferric oxide or iron mud.
As preferably, the pH value of described reaction is 3-5.
As preferably, the concentration of organic waste water is 0.01-1mmol/L, and the reaction times is 30min-1h.
Principle of the present invention is as follows:
2Fe
3++2NH
2OH·HCl=2Fe
2++N
2↑+2H
2O+4H
++2Cl
-
Fe
2++HSO
5 -=Fe
3++SO
4 -·+OH
-
In the present invention, ferriferous oxide discharges Fe in the solution
2+and Fe
3+, wherein Fe
3+fe is reduced to by oxammonium hydrochloride
2+, Fe
2+activation persulphate produces potentiometric titrations, oxidative degradation organic pollutant.And Fe
2+be oxidized to Fe
3+the iron mud produced then by the mode Separation and Recovery of externally-applied magnetic field together with ferriferous oxide, can reuse as activator.
Compared with the existing technology, tool has the following advantages and beneficial effect in the present invention:
(1) the present invention makes ferrous ion in system can slow releasing because using ferriferous oxide as activator, thus ensures that oxidation system can continue the organic pollutant in efficient degradation water, substantially increases organic degradation rate.
(2) the present invention uses ferriferous oxide as activator, is easy to recycle and reuse, greatly reduces cost.
(3) issuable for oxidizing reaction iron mud and activator can reclaim by the present invention jointly, drop into oxidation system and are used, solve the process problem of iron mud.
(4) present invention process flow process is simple, and cost is low, and efficiency is high, environmental friendliness, is applicable to the water treatment of low pH organic waste water.
Accompanying drawing explanation
Fig. 1 is the time m-clearance graphic representation of embodiment 1 pair of wastewater through organic matter.
Fig. 2 is the uv-vis spectra variation diagram of wastewater through organic matter in embodiment 1 reaction process.
Fig. 3 be embodiment 1 activator reusable time m-clearance graphic representation.
Fig. 4 is the time m-clearance graphic representation of embodiment 4 pairs of wastewater through organic matter.
Embodiment
Below in conjunction with concrete case study on implementation, the present invention is described in further detail, but the scope of protection of present invention is not limited to following case study on implementation.
Embodiment 1
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
Will containing 0.1mmol/L orange G (1-phenylazo-beta naphthal-6,8-sodium disulfonate) simulated wastewater 1L be placed in reactor, add 0.5mmol oxammonium hydrochloride, regulate pH be 3, add 0.5g Z 250 and 1mmol potassium hydrogen persulfate more wherein, under room temperature, react 30min.
What represent in Fig. 1 is only add persulphate degradation of organic waste water and utilize the time m-clearance graphic representation of the oxammonium hydrochloride of embodiment 1, activator Z 250 and persulphate degradation of organic waste water.As seen from Figure 1, the clearance only adding persulfate oxidation is only about 10% when 30min, and the clearance of oxammonium hydrochloride strengthening ferriferous oxide activation persulfate oxidation can up to 99%.Show that the oxammonium hydrochloride strengthening ferriferous oxide that the present invention sets up activates the high efficiency that persulfate oxidation water treatment method can ensure persulfate oxidation.
Fig. 2 is the change of uv-vis spectra with the reaction times of orange G under oxammonium hydrochloride, activator Z 250 and persulphate system.As seen from Figure 2,2 charateristic avsorption bands are had in the molecular structure of orange G.Appear at the 330nm place of visible region 475nm and ultraviolet region respectively.π → π * transition of what ultraviolet region 327nm place was corresponding is naphthalene nucleus; And the peak value at 476nm place, visible region represents the conjugated system formed by azo bond in orange G structure, it is also the chromophoric group of orange G structure.In reaction 30min, orange G reduces rapidly at the charateristic avsorption band at this two place, illustrates that the chromophoric group of orange G and naphthalene ring are destroyed totally.As from the foregoing, oxammonium hydrochloride strengthening ferriferous oxide activation persulphate system can effectively be degraded orange G.
After adopting above method degraded 30min, reclaim Z 250 and carry out the above step of repetition as activator, reuse through 5 times, as seen from Figure 3, the activity of activator does not significantly reduce, and shows that the stability of activator is better, can repeatedly use.
Embodiment 2
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
The simulated wastewater (the starting point concentration 0.1mmol/L of orange G) 1L being contained orange G is placed in reactor, adds 0.5mmol oxammonium hydrochloride, regulates pH to be 3, then adds 0.5g iron mud and 1mmol potassium hydrogen persulfate wherein, under room temperature, react 30min.
As seen from Figure 4, oxammonium hydrochloride strengthening ferriferous oxide activation persulphate system rate of oxidation is far away higher than only ferriferous oxide activation persulphate system.Ferriferous oxide activation persulfate oxidation degraded orange G degradation rate when 30min is only about 37%, and the present invention just can reach more than 99% when 10min after utilizing oxammonium hydrochloride to strengthen.
Embodiment 3
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
The simulated wastewater (the starting point concentration 0.1mmol/L of orange G) 1L being contained orange G is placed in reactor, adds 0.5mmol oxammonium hydrochloride, regulates pH to be 3, then adds 0.5g ferric oxide and 1mmol potassium hydrogen persulfate wherein, under room temperature, react 30min.Record the clearance of orange G of the present invention when 30min and can reach 71%.
Embodiment 4
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
The simulated wastewater (the starting point concentration 0.1mmol/L of orange G) 1L being contained orange G is placed in reactor, add 0.5mmol oxammonium hydrochloride, pH is regulated to be 3, add 0.5g ferriferous oxide (Z 250+iron mud more wherein, mass ratio is 1:1) and 1mmol potassium hydrogen persulfate, under room temperature, react 30min.Record the clearance of orange G of the present invention when 30min and can reach 99%.
Embodiment 5
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
1L is contained benzoic simulated wastewater (the starting point concentration 0.1mmol/L of orange G) and be placed in reactor, add 1mmol oxammonium hydrochloride, regulate pH to be 3, then add 0.5g Z 250 and 2mmol hydrogen persulfate sodium wherein, under room temperature, react 30min.Record the clearance of phenylformic acid of the present invention when 30min and can reach 70%.
Embodiment 6
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
1L is contained benzoic simulated wastewater (the starting point concentration 0.1mmol/L of orange G) and be placed in reactor, add 1mmol oxammonium hydrochloride, regulate pH to be 3, then add 0.5g iron mud and 2mmol hydrogen persulfate sodium wherein, under room temperature, react 30min.Record the clearance of phenylformic acid of the present invention when 30min and can reach 90%.
Embodiment 7
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
The simulated wastewater (the starting point concentration 0.1mmol/L of orange G) 1L being contained polychlorobiphenyl is placed in reactor, adds 1mmol oxammonium hydrochloride, regulates pH to be 5, then adds 0.5g Z 250 and 2mmol potassium hydrogen persulfate wherein, under room temperature, react 30min.Record the clearance of polychlorobiphenyl of the present invention when 30min and can reach 81%.
Embodiment 8
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
The simulated wastewater (the starting point concentration 0.1mmol/L of orange G) 1L being contained orange G is placed in reactor, adds 1mmol oxammonium hydrochloride, regulates pH to be 5, then adds 0.5g iron mud and 2mmol potassium hydrogen persulfate wherein, under room temperature, react 30min.Record the clearance of orange G of the present invention when 30min and can reach 99%.
Embodiment 9
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
The simulated wastewater (the starting point concentration 1mmol/L of orange G) 1L being contained orange G is placed in reactor, adds 8mmol oxammonium hydrochloride, regulates pH to be 4, then adds 5g iron mud and 30mmol potassium hydrogen persulfate wherein, under room temperature, react 60min.Record the clearance of orange G of the present invention when 60min and can reach 99%.
Embodiment 10
A method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
The simulated wastewater (the starting point concentration 0.01mmol/L of orange G) 1L being contained orange G is placed in reactor, adds 0.1mmol oxammonium hydrochloride, regulates pH to be 5, then adds 0.05g iron mud and 0.3mmol potassium hydrogen persulfate wherein, under room temperature, react 30min.Record the clearance of orange G of the present invention when 30min and can reach 99%.
Claims (5)
1. a method for oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water, comprises the following steps:
(1) oxammonium hydrochloride is mixed with pretreated waste water;
(2) regulate reaction pH to slightly acidic;
(3) add ferriferous oxide and persulphate, stirred at ambient temperature reacts completely;
(4) waste water after being namely purified after adopting foreign field Separation and Recovery ferriferous oxide;
The ratio of useless Organic substance in water, oxammonium hydrochloride, ferriferous oxide, persulphate is 1mmol:5-10mmol:5mg:10-30mmol.
2. the method for a kind of oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water according to claim 1, is characterized in that, persulphate is at least one in potassium hydrogen persulfate or hydrogen persulfate sodium.
3. the method for a kind of oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water according to claim 1, it is characterized in that, described ferriferous oxide is at least one in Z 250, ferric oxide or iron mud.
4. the method for a kind of oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water according to claim 1, it is characterized in that, the pH value of described reaction is 3-5.
5. the method for a kind of oxammonium hydrochloride strengthening ferriferous oxide activation persulphate degradation of organic waste water according to claim 1, it is characterized in that, the concentration of organic waste water is 0.01-1mmol/L, and the reaction times is 30min-1h.
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|---|---|---|---|
| CN201510984805.9A CN105540985A (en) | 2015-12-25 | 2015-12-25 | Method for degrading organic wastewater by hydroxylamine hydrochloride reinforced iron oxide activated persulfate |
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| CN201510984805.9A CN105540985A (en) | 2015-12-25 | 2015-12-25 | Method for degrading organic wastewater by hydroxylamine hydrochloride reinforced iron oxide activated persulfate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217901A (en) * | 2016-12-14 | 2018-06-29 | 江苏联化科技有限公司 | A kind of method of azanol and/or hydroxylamine salt in degrading waste water |
| CN110422922A (en) * | 2019-06-19 | 2019-11-08 | 中国地质大学（武汉） | A method of iron/persulfate is strengthened based on cysteine and removes organic contamination |
| CN111847623A (en) * | 2020-06-23 | 2020-10-30 | 东华大学 | Method for composite treatment of PVA-containing printing and dyeing wastewater based on two free radicals |
| CN112090415A (en) * | 2020-08-28 | 2020-12-18 | 北京建筑大学 | Hollow microsphere CoSXEnhanced Fe3+Method for degrading methylene blue by PMS system |
| CN112142279A (en) * | 2020-05-20 | 2020-12-29 | 华能大庆热电有限公司 | Thermal power plant calcium carbonate sludge regeneration treatment agent and process |
| CN112759060A (en) * | 2020-12-23 | 2021-05-07 | 浙江工业大学 | Hydroxylamine hydrochloride heterogeneous Fenton-like system and application thereof |
| CN113213611A (en) * | 2021-03-31 | 2021-08-06 | 河南科技大学 | Method for degrading dye wastewater by directly activating persulfate through hydroxylamine hydrochloride |
| CN114133017A (en) * | 2021-11-26 | 2022-03-04 | 武汉理工大学 | Method for catalytically treating organic pollutants in wastewater by using copper tailings |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217901A (en) * | 2016-12-14 | 2018-06-29 | 江苏联化科技有限公司 | A kind of method of azanol and/or hydroxylamine salt in degrading waste water |
| CN110422922A (en) * | 2019-06-19 | 2019-11-08 | 中国地质大学（武汉） | A method of iron/persulfate is strengthened based on cysteine and removes organic contamination |
| CN112142279A (en) * | 2020-05-20 | 2020-12-29 | 华能大庆热电有限公司 | Thermal power plant calcium carbonate sludge regeneration treatment agent and process |
| CN111847623A (en) * | 2020-06-23 | 2020-10-30 | 东华大学 | Method for composite treatment of PVA-containing printing and dyeing wastewater based on two free radicals |
| CN112090415A (en) * | 2020-08-28 | 2020-12-18 | 北京建筑大学 | Hollow microsphere CoSXEnhanced Fe3+Method for degrading methylene blue by PMS system |
| CN112090415B (en) * | 2020-08-28 | 2022-12-02 | 北京建筑大学 | Hollow microsphere CoS X Enhanced Fe 3+ Method for degrading methylene blue by PMS system |
| CN112759060A (en) * | 2020-12-23 | 2021-05-07 | 浙江工业大学 | Hydroxylamine hydrochloride heterogeneous Fenton-like system and application thereof |
| CN113213611A (en) * | 2021-03-31 | 2021-08-06 | 河南科技大学 | Method for degrading dye wastewater by directly activating persulfate through hydroxylamine hydrochloride |
| CN114133017A (en) * | 2021-11-26 | 2022-03-04 | 武汉理工大学 | Method for catalytically treating organic pollutants in wastewater by using copper tailings |
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