CN104888815A - Magnetic neodymium-iron-boron active carbon Fenton catalyst, and preparation method and application thereof - Google Patents
Magnetic neodymium-iron-boron active carbon Fenton catalyst, and preparation method and application thereof Download PDFInfo
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- CN104888815A CN104888815A CN201510269480.6A CN201510269480A CN104888815A CN 104888815 A CN104888815 A CN 104888815A CN 201510269480 A CN201510269480 A CN 201510269480A CN 104888815 A CN104888815 A CN 104888815A
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Abstract
The invention relates to a magnetic neodymium-iron-boron active carbon Fenton catalyst, and a preparation method and application thereof. The magnetic neodymium-iron-boron active carbon Fenton catalyst is prepared from the following raw materials in parts by weight: 1-10g of active carbon, 1-10g of neodymium-iron-boron powder and 10-100ml of ferrous sulfate. The invention also comprises the preparation method of the magnetic neodymium-iron-boron active carbon Fenton catalyst and the application of the magnetic neodymium-iron-boron active carbon Fenton catalyst prepared by adopting the method in the field of organic industrial waste water.
Description
Technical field
The present invention relates to a kind of can the catalyst of hardly degraded organic substance in catalytic degradation sewage, especially after disposing of sewage, do not produce mud, and a kind of magnetic neodymium iron boron active carbon fenton catalyst of recycling from aqueous phase and preparation method thereof and application can be easy to after a procedure.
Background technology
Water environment protection is a problem of current mankind society extensive concern, and along with the fast development of Chinese national economy, the water resource of organic wastewater to China's preciousness of high concentration causes serious threat.Fwaater resources protection becomes with effective utilization the basic guarantee that China realizes Ecological Civilization Construction, the key that the technology of dealing carefully with of exploitation stain disease and sewage reuse techuique are also fwaater resources protection and effectively utilize.The method of sewage disposal comprises Physical, chemical method, physical-chemical process, bioanalysis.High-level oxidation technology in chemical method can direct mineralising or improve the biodegradability of pollutant by oxidation, in the process of the micro-harmful chemicals such as Environmental estrogen, there is very large advantage simultaneously, most organic permineralization or decomposition can be made, have reaction speed fast, process the advantages such as complete, nuisanceless, applied widely, become one of possible technique of administering stain disease.There is good application prospect.Fenton technology relative maturity in numerous advanced oxidation processes, homogeneous phase fenton catalyst has and the mixing of solution, excellent catalytic effect and the advantage such as to be swift in response, but homogeneous phase fenton catalyst is not easy to reclaim, the molysite added flows out with water, improve the colourity of water outlet, affect outlet effect, dosage also can produce a large amount of iron mud comparatively greatly, increases and disposes operating cost.A kind of organic matter that can better be oxidized in sewage of present urgent need, and can the fenton catalyst of recycling.
Summary of the invention
The object of the invention is the defect being not easy to be separated from aqueous phase recycling in order to overcome after existing homogeneous catalyst produces a large amount of mud in use and uses, a kind of magnetic neodymium iron boron active carbon fenton catalyst and preparation method thereof and the application in treatment of Organic Wastewater thereof are provided, this magnetic neodymium iron boron active carbon fenton catalyst does not produce mud when disposing of sewage, and can be easy to recycle from aqueous phase by Magneto separate after a procedure.
Object of the present invention is achieved by following technical proposals:
This magnetic neodymium iron boron active carbon fenton catalyst, described catalyst is made up of the raw material of following weight portion:
Active carbon 1-10g
Neodymium iron boron powder 1-10g
Ferrous sulfate 10-100ml
The weight portion of each raw material optimum of described catalyst is:
Active carbon 5 g
Neodymium iron boron powder 5 g
Ferrous sulfate 50ml
The preparation method of magnetic neodymium iron boron active carbon fenton catalyst, comprises step below:
(1) by active carbon 5 ~ 10%HNO
3filter after solution impregnation 24h, be washed till neutrality by deionized water, put into baking oven, dry under 40 ~ 50 DEG C of conditions;
(2) the active carbon 1-10g that step (1) processed is added in beaker, in beaker, adds 1-3ml deionized water make catalyst wetted, wetting catalyst is joined in bottle,suction, take out 90 ~ 95Kpa negative pressure 10min;
(3) keep negative pressure state, by 1 ~ 10g neodymium iron boron powder, spray on wetting active carbon, after shaking up 2min, open rapidly the pressure balance that valve makes inside and outside bottle,suction, Ultrasonic Cleaning 5min, puts into baking oven, dry 24h under 40 ~ 50 DEG C of conditions;
(4) putting into 500ml bottle,suction by processing through step (3) active carbon obtained, after taking out 90 ~ 95Kpa negative pressure 5min, in bottle,suction, adding 1mol/LFeSO
4solution 10-100ml, keeps negative pressure state to shake up 20min, dry 4h under 40 ~ 50 DEG C of conditions, obtains magnetic neodymium iron boron active carbon fenton catalyst.
The application of magnetic neodymium iron boron active carbon fenton catalyst on organic industrial sewage field prepared by method recited above.
The invention has the beneficial effects as follows:
1, magnetic neodymium iron boron active carbon fenton catalyst preparation method is simple, gets final product treatment of dyeing and printing at ambient temperature.In effective degradation of sewage while hardly degraded organic substance, the catalyst after by use can be easy to and be recycled and reused by the mode of Magneto separate.
2, magnetic neodymium iron boron active carbon fenton catalyst is prepared with neodymium iron boron, ferrous sulfate and active carbon for raw material,
Magnetic neodymium iron boron powder loads on active carbon and makes catalyst have magnetic, and catalyst is recycled by the mode separating treatment of Magneto separate after the reaction.The good stability of catalyst, catalytic activity is high, does not need heating greatly to save the energy.
3,1 is tested: use this catalyst treatment dye wastewater (methyl orange solution)
Reaction target solution volume: 200mL
Reaction target solution: dye wastewater (methyl orange solution),
Methyl orange solution concentration is: 20mg/L
Reaction condition is:
Under room temperature condition
PH is 3.0
Hydrogen peroxide initial concentration is 0.6mmol/L
Treatment effect is as shown in table 1, and magnetic neodymium iron boron active carbon fenton catalyst recycling effect is as shown in table 2.
The effect of table 1 embodiment 1 treatment of simulated waste water from dyestuff (methyl orange solution) different catalysts dosage
| Magnetic neodymium iron boron active carbon fenton catalyst dosage | 5g/L | 10g/L | 15g/L | 20g/L |
| Initial concentration | 20mg/L | 20mg/L | 20mg/L | 20mg/L |
| Concentration after reaction | 1.5mg/L | 1.3mg/L | 1.44mg/l | 1.5mg/L |
| Clearance | 92.5% | 93.5% | 92.8% | 92.5% |
Time table 2 embodiment 1 treatment of simulated waste water from dyestuff (methyl orange solution), effect reused by catalyst
| Reuse number of times | 1 | 2 | 3 | 4 | 5 |
| Initial concentration | 20mg/L | 20mg/L | 20mg/L | 20mg/L | 20mg/L |
| Concentration after reaction | 0.44mg/L | 0.7mg/L | 1.76mg/L | 0.6mg/L | 0.58mg/L |
| Clearance | 97.8% | 96.5% | 91.2% | 97.0% | 97.1% |
As can be seen from embodiment 1, this magnetic neodymium iron boron active carbon fenton catalyst has good treatment effect on treatment of simulated dyeing waste water, first time uses the effect of catalyst treatment simulated wastewater to reach more than 95%, and reusable effect also can reach more than 90%.
4,2 are tested: use this catalyst treatment dye wastewater (methyl orange solution)
Reaction target solution volume: 200mL
Reaction target solution: dye wastewater (methyl orange solution),
Methyl orange solution concentration is: 20mg/L
Reaction condition is:
Under room temperature condition
PH is 3.0
Magnetic neodymium iron boron active carbon fenton catalyst dosage is 10g/L
Treatment effect is as shown in table 3.
The effect of table 3 embodiment 2 treatment of simulated waste water from dyestuff (methyl orange solution) different concentration of hydrogen peroxide
| Hydrogen peroxide initial concentration | 0.4mmol/L | 0.6mmol/L | 0.8mmol/L | 1.0mmol/L | 1.2mmol/L |
| Initial concentration | 20mg/L | 20mg/L | 20mg/L | 20mg/L | 20mg/L |
| Concentration after reaction | 1.28mg/L | 1.04mg/L | 0.9mg/l | 0.86mg/L | 1.12mg/L |
| Clearance | 93.6% | 94.8% | 95.5% | 95.7% | 94.40% |
As can be seen from embodiment 2, this magnetic neodymium iron boron active carbon fenton catalyst has good treatment effect on treatment of simulated dyeing waste water, and in the environment of different concentration of hydrogen peroxide, the clearance of reaction can reach more than 90%.
Detailed description of the invention
The specific embodiment of the present invention is:
Adopt the dust technology of 5 ~ 10% to soak the active carbon (AC) 24 hour of particle diameter at 0.3-2mm under room temperature condition, dry in the baking oven of 40 ~ 50 DEG C after active carbon deionized water is washed till neutrality.Get 1-10g on active carbon that 1 ~ 3 ml deionized water joins oven dry, shake makes activated carbon granule wetted, is put in the bottle,suction of 500mL, opens vavuum pump by wetting activated carbon granule, makes system keep the negative pressure of 90 ~ 95 kPas.After ten minutes, put in the middle of syringe, be connected on bottle,suction by neodymium iron boron powder 1-10g, due to suction function, neodymium iron boron powder understands the surface of active carbon in spirt bottle,suction and bottle,suction.Mixing vibration is after 2 minutes, and the valve of bottle,suction is opened rapidly, allows pressure balance inside and outside bottle,suction.The neodymium iron boron being adsorbed on activated carbon surface by these operations is inhaled in the middle of the duct of active carbon, and activated carbon granule Ultrasonic Cleaning has washed unnecessary neodymium iron boron for 5 minutes off.Dry after 24 hours under 40 ~ 50 DEG C of conditions, by permanent magnet, magnetic neodymium iron boron active carbon (NdFeB-AC) is separated.The magnetic neodymium iron boron active carbon obtained is placed in the bottle,suction of 500mL again, opens vavuum pump, make system keep the negative pressure of 90 ~ 95 kPas.Join in bottle,suction by 1mol/L copperas solution 10-100ml after 5 minutes, shake bottle,suction 20 minutes, remains the environment of negative pressure in the process of mixing always.Then at normal atmospheric pressure, the mode of magnetic neodymium iron boron active carbon Magneto separate is separated from copperas solution, put in baking oven and dry 4 hours under 40 ~ 50 DEG C of conditions, just obtain magnetic neodymium iron boron fenton catalyst (NdFeB-AC-FC).
Embodiment one. by 5g active carbon and 1g magnetic neodymium iron boron powder preparation magnetic neodymium iron boron active carbon fenton catalyst, the method comprises following steps:
(1) by active carbon 5%HNO
3filter after solution impregnation 24h, be washed till neutrality by deionized water, dry under putting into baking oven 50 DEG C of conditions;
(2) the active carbon 5g that step (1) processed is added in beaker, in beaker, add 3ml deionized water make catalyst wetted, wetting catalyst is added in bottle,suction, take out 95Kpa negative pressure 10min;
(3) keep negative pressure state, by 1g magnetic neodymium iron boron powder, spray on wetting active carbon, after shaking up 2min, open rapidly the pressure balance that valve makes inside and outside bottle,suction, Ultrasonic Cleaning 5min, puts into baking oven, dry 24h under 50 DEG C of conditions;
(4) putting into 500ml bottle,suction by processing through step (3) active carbon obtained, after taking out 95Kpa negative pressure 5min, in bottle,suction, adding 1mol/LFeSO
4solution 50ml, keeps negative pressure state to shake up 20min, dry 4h under 50 DEG C of conditions, obtains magnetic neodymium iron boron active carbon fenton catalyst.
Embodiment two: by 5g active carbon and 5g magnetic neodymium iron boron powder preparation magnetic neodymium iron boron active carbon fenton catalyst
Embodiment two is with the difference of embodiment one:
(3) keep negative pressure state, by 5g magnetic neodymium iron boron powder, spray on wetting active carbon, after shaking up 2min, open rapidly the pressure balance that valve makes inside and outside bottle,suction, Ultrasonic Cleaning 5min, puts into baking oven, dry 24h under 50 DEG C of conditions;
(4) putting into 500ml bottle,suction by processing through step (3) active carbon obtained, after taking out 95Kpa negative pressure 5min, in bottle,suction, adding 1mol/LFeSO
4solution 50ml, keeps negative pressure state to shake up 20min, dry 4h under 50 DEG C of conditions, obtains magnetic neodymium iron boron active carbon fenton catalyst.
Claims (5)
1. a magnetic neodymium iron boron active carbon fenton catalyst, is characterized in that: described catalyst is made up of the raw material of following weight portion:
Active carbon 1-10g
Neodymium iron boron powder 1-10g
Ferrous sulfate 10-100ml.
2. a kind of magnetic neodymium iron boron active carbon fenton catalyst according to claim 1, is characterized in that: the weight portion of each raw material optimum of described catalyst is:
Active carbon 5 g
Neodymium iron boron powder 5 g
Ferrous sulfate 50ml.
3. the preparation method of magnetic neodymium iron boron active carbon fenton catalyst described in claim 1, is characterized in that: comprise step below:
(1) by active carbon 5 ~ 10%HNO
3filter after solution impregnation 24h, be washed till neutrality by deionized water, put into baking oven, dry under 40 ~ 50 DEG C of conditions;
(2) the active carbon 1-10g that step (1) processed is added in beaker, in beaker, adds 1-3ml deionized water make catalyst wetted, wetting catalyst is joined in bottle,suction, take out 90 ~ 95Kpa negative pressure 10min;
(3) keep negative pressure state, by 1 ~ 10g neodymium iron boron powder, spray on wetting active carbon, after shaking up 2min, open rapidly the pressure balance that valve makes inside and outside bottle,suction, Ultrasonic Cleaning 5min, puts into baking oven, dry 24h under 40 ~ 50 DEG C of conditions;
(4) putting into 500ml bottle,suction by processing through step (3) active carbon obtained, after taking out 90 ~ 95Kpa negative pressure 5min, in bottle,suction, adding 1mol/LFeSO
4solution 10-100ml, keeps negative pressure state to shake up 20min, dry 4h under 40 ~ 50 DEG C of conditions, obtains magnetic neodymium iron boron active carbon fenton catalyst.
4. the preparation method of a kind of magnetic neodymium iron boron active carbon fenton catalyst according to claim 3, is characterized in that: comprise step below:
(1) by active carbon 5 ~ 10%HNO
3filter after solution impregnation 24h, be washed till neutrality by deionized water, put into baking oven, dry under 40 ~ 50 DEG C of conditions;
(2) the active carbon 5g that step (1) processed is added in beaker, in beaker, adds 1-3ml deionized water make catalyst wetted, wetting catalyst is joined in bottle,suction, take out 90 ~ 95Kpa negative pressure 10min;
(3) keep negative pressure state, by 5g neodymium iron boron powder, spray on wetting active carbon, after shaking up 2min, open rapidly the pressure balance that valve makes inside and outside bottle,suction, Ultrasonic Cleaning 5min, puts into baking oven, dry 24h under 40 ~ 50 DEG C of conditions;
(4) putting into 500ml bottle,suction by processing through step (3) active carbon obtained, after taking out 90 ~ 95Kpa negative pressure 5min, in bottle,suction, adding 1mol/LFeSO
4solution 50ml, keeps negative pressure state to shake up 20min, dry 4h under 40 ~ 50 DEG C of conditions, obtains magnetic neodymium iron boron active carbon fenton catalyst.
5. the application of magnetic neodymium iron boron active carbon fenton catalyst on organic industrial sewage field prepared by method according to claim 3.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105439238A (en) * | 2015-12-11 | 2016-03-30 | 哈尔滨工业大学宜兴环保研究院 | Method for integrated treatment of dyeing wastewater by using magnetic activated carbon |
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| CN102909073A (en) * | 2012-10-12 | 2013-02-06 | 浙江理工大学 | Preparation method and application of heterogeneous Fenton-like catalyst |
| CN102989460A (en) * | 2011-09-13 | 2013-03-27 | 苏州科技学院 | Preparation method of heterogeneous Fenton catalyst, and method for visible photocatalytic degradation of organic pollutants |
| JP2014198286A (en) * | 2013-03-29 | 2014-10-23 | 栗田工業株式会社 | Method for treating poorly biodegradable organic matter-containing water and treatment apparatus thereof |
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| CN102989460A (en) * | 2011-09-13 | 2013-03-27 | 苏州科技学院 | Preparation method of heterogeneous Fenton catalyst, and method for visible photocatalytic degradation of organic pollutants |
| CN102909073A (en) * | 2012-10-12 | 2013-02-06 | 浙江理工大学 | Preparation method and application of heterogeneous Fenton-like catalyst |
| JP2014198286A (en) * | 2013-03-29 | 2014-10-23 | 栗田工業株式会社 | Method for treating poorly biodegradable organic matter-containing water and treatment apparatus thereof |
Non-Patent Citations (2)
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| CHUNWEI YANG,ET AL: "Magnetic Nd2Fe14B Actived Carbon: Fabrication and Heterogeneous Fenton Oxidation of Congo Red", 《APPLIED MECHANICS AND MATERIALS》 * |
| CHUNWEI YANG,ET AL: "The synthesis of NdFeB magnetic activated carbon and its application in degradation of azo dye methyl orange by Fenton-like process", 《JOURNAL OF THE TAIWAN INSTITUTE OF CHEMICAL ENGINEERS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439238A (en) * | 2015-12-11 | 2016-03-30 | 哈尔滨工业大学宜兴环保研究院 | Method for integrated treatment of dyeing wastewater by using magnetic activated carbon |
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