CN106745650A - A kind of method of organic dyestuff in utilization ferriferrous oxide nano cage activation sodium peroxydisulfate degradation water - Google Patents
A kind of method of organic dyestuff in utilization ferriferrous oxide nano cage activation sodium peroxydisulfate degradation water Download PDFInfo
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- CN106745650A CN106745650A CN201611144384.XA CN201611144384A CN106745650A CN 106745650 A CN106745650 A CN 106745650A CN 201611144384 A CN201611144384 A CN 201611144384A CN 106745650 A CN106745650 A CN 106745650A
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- water
- nanocages
- organic dyestuff
- solution
- rhodamine
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- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 title claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002091 nanocage Substances 0.000 title claims abstract description 56
- 239000000975 dye Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000015556 catabolic process Effects 0.000 title claims abstract description 17
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 17
- 230000004913 activation Effects 0.000 title abstract description 8
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 38
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 230000010355 oscillation Effects 0.000 claims abstract description 7
- 238000011084 recovery Methods 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 31
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 12
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 9
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 238000003918 potentiometric titration Methods 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002105 nanoparticle Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 238000004043 dyeing Methods 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000007210 heterogeneous catalysis Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- -1 hydroxyl radical free radical Chemical class 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000005408 paramagnetism Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/61—
-
- 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
-
- 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
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
Abstract
The invention discloses the method using organic dyestuff in ferriferrous oxide nano cage activation sodium peroxydisulfate degradation water, realized especially by following steps：Prepare Fe3O4Nanocages；By obtained Fe3O4In nanocages solution of the input containing rhodamine B, then sodium peroxydisulfate is put into, react 30 ~ 120 min, bath temperature is set as 20 ~ 60 DEG C, and frequency of oscillation is 60 ~ 180 times/min；Reacted Fe3O4Nanocages are collected by externally-applied magnetic field, are dried at 75 DEG C after alternately cleaning three times with water and ethanol, and Fe is reclaimed with this3O4Nanocages, the Fe of recovery3O4Nanocages can be re-used for the degraded of rhodamine B.Fe provided by the present invention3O4Nanocages possess hollow meso-hole structure, with huge specific surface area, can be fully contacted with sodium peroxydisulfate, generate the degradation rate that sufficient amount of potentiometric titrations improve organic dyestuff in water.
Description
Technical field
The invention belongs to water-treatment technology field, and in particular to one kind is using ferriferrous oxide nano cage activation sodium peroxydisulfate
There is engine dyeing in the method for processing waste water from dyestuff, more particularly to a kind of activation sodium peroxydisulfate degradation water using ferriferrous oxide nano cage
The method of material.
Background technology
With expanding economy, problem of environmental pollution becomes the huge challenge for being faced at present.In recent years, dyestuff
It is widely used in industry such as weaving, printing and dyeing, process hides, papermaking, produced waste water is substantial amounts of to be entered in water environment.Due to
The features such as its colourity is high big with toxicity, greatly threatens the stabilization of the ecosystem, and stable chemical constitution causes tradition in addition
Sewage treatmentmethod be difficult to completely remove it, therefore explore it is a kind of it is effective treatment dyeing waste water method to environmental protection
It is significant.Rhodamine B（Rhodamine B, RhB）A kind of typical artificial synthesized organic dyestuff, in the industry by
Largely use, the concentration that rhodamine B is detected in dyeing waste water can generally be more than 100 mg/L.The rhodamine of such high concentration
If B fails effectively to be processed and enter natural water body, the harm to the ecosystem and health will be huge.Luo Dan
The high chroma characteristic of bright B can influence the translucency of water body, suppress the photosynthesis of aquatic ecosystem, reduce the dissolving in water body
Oxygen, damages to aquatic ecosystem.Additionally, rhodamine B is a kind of carcinogen, it is impossible to which effectively removing it will prestige
Coerce the physical and mental health of the mankind.
Heterogeneous catalysis persulfate technology is, using solid material as catalyst, to activate persulfate and obtain Strong oxdiative
The potentiometric titrations of activity（SO4 -.）Organic pollution in removal water body.Compared to traditional hydroxyl radical free radical（.OH）It is high
Level oxidation technology, heterogeneous catalysis persulfate technology has more development potentiality, is mainly shown as：（1）Potentiometric titrations
（SO4 -.）There is stronger oxidability, longer half-life period compared to hydroxyl radical free radical；（2）Sodium peroxydisulfate dissolubility is good, energy
It is enough fully to be contacted with target contaminant and catalyst, improve the utilization ratio of oxidant；（3）Heterogeneous catalysis persulfate skill
The secondary pollution that art is produced is few, and catalyst is easily recycled.
Fe-series catalyst contains the catalyst of heavy metal element compared to other as a kind of green catalyst, in catalysis
Secondary pollution can't be brought in persulfate degradable organic pollutant to water body.Fe3O4As one kind of Fe-series catalyst, no
But environmentally friendly catalyst, and there is the characteristic of superparamagnetism because of it, it is easy to recycle, so as to reduce run into
This.Therefore Fe3O4Had a good application prospect in organic wastewater with difficult degradation thereby is processed.Traditional Fe3O4Nano particle specific surface area
It is relatively low, be easy in water to reunite, had a strong impact on the performance of catalytic performance.
The content of the invention
The invention provides the side of organic dyestuff in a kind of utilization ferriferrous oxide nano cage activation sodium peroxydisulfate degradation water
Method, the Fe that the present invention is developed3O4Nanocages possess hollow meso-hole structure, and resulting huge specific surface area can
It is fully contacted with sodium peroxydisulfate, generates sufficient amount of potentiometric titrations.Additionally, Fe3O4Nanocages possess good superparamagnetic
Property, can be recycled and reused using externally-applied magnetic field.
One kind utilizes Fe3O4The method of organic dyestuff, specifically grasps according to the following steps in nanocages activation sodium peroxydisulfate treatment water
Make：
First, Fe3O4The preparation of nanocages：
（1）By FeCl3·6H2O, NaOH and triethanolamine are dissolved in the mixed solution of ethylene glycol and water, and stirring obtains Huang
Color clear solution A；
（2）By FeCl2·4H2O, NaOH and triethanolamine are dissolved in the mixed solution of ethylene glycol and water, and stirring obtains green
Color clear solution M；
（3）By step（1）Solution A and step（2）Solution M stirring mixing, obtain colloidal solution C；
（4）By step（3）The colloidal solution C for obtaining heats 20 h at being placed in 100 DEG C, obtains black precipitate；
（5）Step（4）After the black precipitate for obtaining is cooled to room temperature, with alternately cleaning three times of water and ethanol, collected with magnet
After be placed in 75 DEG C at dry, the black powder obtained after being fully ground is Fe3O4Nanocages；
2nd, by obtained Fe3O4In nanocages solution of the input containing rhodamine B, 30 min are vibrated in water bath with thermostatic control, to reach suction
Attached balance；
3rd, by the solution in sodium peroxydisulfate input step 2,30 ~ 120 min are reacted, bath temperature is set as 20 ~ 60 DEG C,
Frequency of oscillation is 60 ~ 180 times/min；
4th, reacted Fe3O4Nanocages are collected by externally-applied magnetic field, after alternately cleaning three times with water and ethanol at 75 DEG C
Dry, Fe is reclaimed with this3O4Nanocages, the Fe of recovery3O4Nanocages can be re-used for the degraded of rhodamine B.
Preferably, step（1）Described in ethylene glycol and water volume ratio be 3:1.
Preferably, step（1）Described in FeCl3·6H2The mol ratio of O, NaOH and triethanolamine is about：0.6:
6:1。
Preferably, step（1）Described in FeCl3·6H2Concentration of the O in water and alcohol mixeding liquid is about 0.12
mol/L。
Preferably, step（2）Described in ethylene glycol and water ratio be 3:1.
Preferably, step（2）Described in FeCl2·4H2The mol ratio of O, NaOH and triethanolamine is about 0.4:6:
1。
Preferably, step（2）Described in FeCl2·4H2Concentration of the O in water and ethylene glycol mixture is about 0.08
mol/L。
Preferably, rhodamine B solution concentration described in step 2 is 1 ~ 100 mg/L.
Preferably, Fe described in step 23O4The dosage of nanocages is 0.1 ~ 1 g/L.
Preferably, the sodium peroxydisulfate described in step 3 is about 5 ~ 100 with the mol ratio of rhodamine B:1:1.
Meaning of the present invention is, traditional Fe3O4Nano particle specific surface area is relatively low, be easy to reunion, serious shadow in water
The performance of catalytic performance is rung.The Fe that the present invention is used3O4Nanocages are 20 h to be heated at 100 DEG C and is obtained using coprecipitation
To a kind of nano material for possessing cage structure.The Fe that the present invention is developed3O4Nanocages possess hollow meso-hole structure, thus
The huge specific surface area for producing can be fully contacted with sodium peroxydisulfate, generate sufficient amount of potentiometric titrations, from
And the production rate of potentiometric titrations is improved, improve the clearance of organic pollution.Additionally, Fe3O4Nanocages possess good surpassing
Paramagnetism, can be recycled and reused using externally-applied magnetic field.Beneficial effects of the present invention are：
1st, Fe prepared by the present invention3O4Nanocages specific surface area is big, can efficiently activate sodium peroxydisulfate；
2nd, the Fe that the present invention is used3O4Nanocages are a kind of green catalysts, will not cause secondary pollution to water body；
3rd, Fe prepared by the present invention3O4Preparation manipulation it is simple, be easy to implement；
4th, the Fe that the present invention is used3O4Nanocages possess superparamagnetism, it is easy to reclaim, and cut operating costs；
5th, Fe prepared by the present invention3O4Nanocages activation sodium peroxydisulfate need not be combined the modes such as ultraviolet radioactive, ultrasound and heating and enter
Row reinforcing, more energy-conservation.
Brief description of the drawings
The graph of a relation that Fig. 1 is changed over time for rhodamine B percentage in embodiment 1, comparative example 1 ~ 3.
Specific embodiment
Technical solution of the present invention is not limited to specific implementation method exemplified below, also including any between each specific embodiment
Combination.
Embodiment 1：
First, Fe3O4The preparation of nanocages：
（1）By FeCl3·6H2O, NaOH and triethanolamine are dissolved in the mixed solution of ethylene glycol and water, under magnetic agitation
Obtain yellow transparent solution A；
Step one（1）In, the ratio of ethylene glycol and water is 3:1；
Step one（1）In, FeCl3·6H2The mol ratio of O, NaOH and triethanolamine is about 0.6:6:1；
Step one（1）In, FeCl3·6H2Concentration of the O in water and alcohol mixeding liquid is about 0.12 mol/L；
（2）By FeCl2·4H2O, NaOH and triethanolamine are dissolved in the mixed solution of ethylene glycol and water, in magnetic agitation
Green transparent solution M is obtained under effect；
Step one（2）In, the ratio of ethylene glycol and water is 3:1；
Step one（2）In, FeCl2·4H2The mol ratio of O, NaOH and triethanolamine is about 0.4:6:1；
Step one（2）In, FeCl2·4H2Concentration of the O in water and ethylene glycol mixture is about 0.08 mol/L；
（3）By step（1）Solution A and step（2）Solution M magnetic agitation effect under mix, obtain colloidal solution C；
（4）By step（3）The colloidal solution C for obtaining heats 20 h at being placed in 100 DEG C, obtains black precipitate；
（5）Step（4）After the black precipitate for obtaining is cooled to room temperature, with alternately cleaning three times of water and ethanol, collected with magnet
After be placed in 75 DEG C at dry, the black powder for obtaining is Fe3O4Nanocages；
Step one（5）In, the Fe for obtaining3O4Nanocages are fully ground rear standby.
2nd, the Fe that will be obtained3O4Nanocages are sufficiently mixed with the rhodamine B aqueous solution, go to brown bottle and are reacted；
In step 2, Fe3O4The dosage of nanocages is 0.1 ~ 0.5 g/L；
In step 2, the concentration of rhodamine B solution is 1 ~ 50 mg/L；
In step 3, equipped with Fe3O430 min are vibrated in the brown bottle elder generation water bath with thermostatic control of nanocages and rhodamine B mixed liquor, to reach
To adsorption equilibrium；
3rd, by the solution in sodium peroxydisulfate input step 2,30 ~ 120 min are reacted, bath temperature is set as 20 ~ 40 DEG C,
Frequency of oscillation is 60 ~ 180 times/min；
In step 3, the mol ratio of sodium peroxydisulfate and rhodamine B is (5 ~ 25):1；
4th, reacted Fe3O4Nanocages are collected by externally-applied magnetic field, 75 DEG C of dryings after alternately cleaning three times with water and ethanol,
Fe is reclaimed with this3O4Nanocages.The Fe of recovery3O4Nanocages can be re-used for the degraded of rhodamine B.
Embodiment 2：Present embodiment is with the difference of embodiment 1：In step 2, the concentration of rhodamine B solution for 50 ~
100 mg/L, other steps are same as Example 1；
Embodiment 3：Present embodiment is with the difference of embodiment 1：In step 2, Fe3O4The dosage of nanocages be 0.5 ~
1.0 g/L, other steps are same as Example 1；
Embodiment 4：Present embodiment is with the difference of embodiment 1：In step 3, the mol ratio of sodium peroxydisulfate and rhodamine B is
(25~50):1, other steps are same as Example 1；
Embodiment 5：Present embodiment is with the difference of embodiment 1：In step 3, the mol ratio of sodium peroxydisulfate and rhodamine B is
(50~100):1, other steps are same as Example 1；
Embodiment 6：Present embodiment is with the difference of embodiment 1：In step 3, bath temperature is set as 40 ~ 60 DEG C, other
Step is same as Example 1；
Comparative example 1：Individually add Fe3O4Nanocages are carried out according to the following steps to rhodamine B removal experiment：
First, Fe is prepared3O4Nanocages：It is identical with embodiment 1；
2nd, the Fe that will be prepared3O4Nanocages are sufficiently mixed with the rhodamine B aqueous solution, go to reaction, reaction temperature in brown bottle
It is set as 25 ± 1 DEG C, frequency of oscillation is 180 times/min, the min of reaction time 60；
In step 2, Fe3O4The dosage of nanocages is 0.5 g/L；
In step 2, the concentration of the rhodamine B aqueous solution is 20 mg/L；
3rd, reacted Fe3O4Nanocages are collected by externally-applied magnetic field, and with water and ethanol, alternately cleaning is done for three times after 75 DEG C
It is dry, to reclaim Fe3O4Nanocages.The Fe of recovery3O4Nanocages can be re-used for the degraded of rhodamine B.
Comparative example 2：Individually throw sodium peroxydisulfate is carried out according to the following steps to rhodamine B removal experiment：
First, rhodamine B solution is prepared：In going to brown bottle after certain density rhodamine B solution is prepared；
In step one, the concentration of the rhodamine B aqueous solution is 20 mg/L；
2nd, sodium peroxydisulfate is added：To be reacted in the brown bottle equipped with rhodamine B solution in sodium peroxydisulfate input step one, reaction
Temperature is set as 25 ± 1 DEG C, and frequency of oscillation is 180 times/min, the min of reaction time 60；
In step 2, sodium peroxydisulfate is 24 with the mol ratio of rhodamine B:1；
Comparative example 3：General commercial Fe3O4Removal experiment of the nanoparticulate activated sodium peroxydisulfate to rhodamine B is entered according to the following steps
OK：
First, by general commercial Fe3O4Nano particle is sufficiently mixed with the rhodamine B aqueous solution, goes to reaction in brown bottle, reaction temperature
Degree is set as 25 ± 1 DEG C, and frequency of oscillation is 180 times/min, the min of reaction time 60；
In step 2, Fe3O4The dosage of nano particle is 0.5 g/L；
In step 2, the concentration of the rhodamine B aqueous solution is 20 mg/L；
2nd, reacted Fe3O4Nano particle is collected by externally-applied magnetic field, and three times are alternately cleaned after 75 DEG C with water and ethanol
Dry, to reclaim Fe3O4Nano particle.
Rhodamine B percentage versus time curve is shown in accompanying drawing 1 in testing example 1, comparative example 1 ~ 3.Pass through
Comparative example 1, comparative example 1, comparative example 2, the removal efficiency of the rhodamine B of comparative example 3, it is found that Fe3O4Nanocages are combined
Sodium peroxydisulfate removes the efficiency significantly larger than Fe of organic dyestuff in water removal3O4Nanocages and the independent of sodium peroxydisulfate are added, and
Fe3O4Nanocages will be much stronger than general commercial Fe to the catalytic efficiency of sodium peroxydisulfate3O4Catalysis of the nano particle to sodium peroxydisulfate is imitated
Rate.
Listed above is only preferred scheme of the invention, and protection scope of the present invention is not limited to that, art technology
Any change that personnel are made within the scope of the invention as claimed is each fallen within the scope of the present invention.
Claims (10)
1. a kind of method that utilization ferriferrous oxide nano cage activates organic dyestuff in sodium peroxydisulfate degradation water, it is characterised in that
Include the following steps：
First, Fe3O4The preparation of nanocages：
（1）By FeCl3·6H2O, NaOH and triethanolamine are dissolved in the mixed solution of ethylene glycol and water, and stirring obtains yellow
Clear solution A；
（2）By FeCl2·4H2O, NaOH and triethanolamine are dissolved in the mixed solution of ethylene glycol and water, and stirring obtains green
Clear solution M；
（3）By step（1）Solution A and step（2）Solution M stirring mixing, obtain colloidal solution C；
（4）By step（3）The colloidal solution C for obtaining heats 20 h at being placed in 100 DEG C, obtains black precipitate；
（5）Step（4）After the black precipitate for obtaining is cooled to room temperature, with alternately cleaning three times of water and ethanol, collected with magnet
After be placed in 75 DEG C at dry, the black powder obtained after being fully ground is Fe3O4Nanocages；
2nd, by obtained Fe3O4In nanocages solution of the input containing rhodamine B, 30 min are vibrated in water bath with thermostatic control, to reach absorption
Balance；
3rd, by the solution in sodium peroxydisulfate input step 2,30 ~ 120 min are reacted, bath temperature is set as 20 ~ 60 DEG C,
Frequency of oscillation is 60 ~ 180 times/min；
4th, reacted Fe3O4Nanocages are collected by externally-applied magnetic field, are done at 75 DEG C after alternately cleaning three times with water and ethanol
It is dry, Fe is reclaimed with this3O4Nanocages, the Fe of recovery3O4Nanocages can be re-used for the degraded of rhodamine B.
2. in degradation water as claimed in claim 1 organic dyestuff method, it is characterised in that step one（1）Described in second two
The volume ratio of alcohol and water is 3:1.
3. in degradation water as claimed in claim 1 organic dyestuff method, it is characterised in that step one（1）Described in
FeCl3·6H2The mol ratio of O, NaOH and triethanolamine is 0.6:6:1.
4. in the degradation water as described in claim 1 organic dyestuff method, it is characterised in that step one（1）Described in
FeCl3 .6H2Concentration of the O in water and alcohol mixeding liquid is 0.12 mol/L.
5. in degradation water as claimed in claim 1 organic dyestuff method, it is characterised in that step one（2）Described in second two
The ratio of alcohol and water is 3:1.
6. in degradation water as claimed in claim 1 organic dyestuff method, it is characterised in that step one（2）Described in
FeCl2·4H2The mol ratio of O, NaOH and triethanolamine is 0.4:6:1.
7. in degradation water as claimed in claim 1 organic dyestuff method, it is characterised in that step one（2）Described in
FeCl2·4H2Concentration of the O in water and ethylene glycol mixture is 0.08 mol/L.
8. in degradation water as claimed in claim 1 organic dyestuff method, it is characterised in that rhodamine B described in step 2
Solution concentration is 1 ~ 100 mg/L.
9. in the degradation water as described in claim 1 organic dyestuff method, it is characterised in that Fe described in step 23O4Nanometer
The dosage of cage is 0.1 ~ 1 g/L.
10. in degradation water as claimed in claim 1 organic dyestuff method, it is characterised in that the over cure described in step 3
Sour sodium is 5 ~ 100 with the mol ratio of rhodamine B:1.
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| CN108176401A (en) * | 2018-01-10 | 2018-06-19 | 扬州工业职业技术学院 | A kind of preparation method of the nano ferriferrous oxide Fenton catalyst of selenium doping |
| CN109928482A (en) * | 2019-04-26 | 2019-06-25 | 常州大学 | A kind of method of persulfate activation |
| CN114505095A (en) * | 2022-01-11 | 2022-05-17 | 浙江工业大学绍兴研究院 | Spherical Fe with strong dispersibility3O4Preparation method and application of @ ZSM-5 composite material |
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| CN103739056A (en) * | 2013-11-20 | 2014-04-23 | 上海大学 | Method for degrading organic dye wastewater by utilizing Fe3O4 to activate potassium persulphate |
| CN103787423A (en) * | 2014-01-17 | 2014-05-14 | 哈尔滨工程大学 | Method for thermally preparing ferroferric oxide nanoparticle by using low-temperature solvent |
| CN106045152A (en) * | 2016-07-08 | 2016-10-26 | 常州大学 | Method for degrading rhodamine B through nanometer Fe3O4/Na2S2O8 jointly |
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| CN103739056A (en) * | 2013-11-20 | 2014-04-23 | 上海大学 | Method for degrading organic dye wastewater by utilizing Fe3O4 to activate potassium persulphate |
| CN103787423A (en) * | 2014-01-17 | 2014-05-14 | 哈尔滨工程大学 | Method for thermally preparing ferroferric oxide nanoparticle by using low-temperature solvent |
| CN106045152A (en) * | 2016-07-08 | 2016-10-26 | 常州大学 | Method for degrading rhodamine B through nanometer Fe3O4/Na2S2O8 jointly |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108176401A (en) * | 2018-01-10 | 2018-06-19 | 扬州工业职业技术学院 | A kind of preparation method of the nano ferriferrous oxide Fenton catalyst of selenium doping |
| CN109928482A (en) * | 2019-04-26 | 2019-06-25 | 常州大学 | A kind of method of persulfate activation |
| CN114505095A (en) * | 2022-01-11 | 2022-05-17 | 浙江工业大学绍兴研究院 | Spherical Fe with strong dispersibility3O4Preparation method and application of @ ZSM-5 composite material |
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