CN110117035A - A kind of preparation method that mushroom bran carbon loads zero-valent iron composite material and its application in oil pollution wastewater treatment - Google Patents
A kind of preparation method that mushroom bran carbon loads zero-valent iron composite material and its application in oil pollution wastewater treatment Download PDFInfo
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- CN110117035A CN110117035A CN201910276834.8A CN201910276834A CN110117035A CN 110117035 A CN110117035 A CN 110117035A CN 201910276834 A CN201910276834 A CN 201910276834A CN 110117035 A CN110117035 A CN 110117035A
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- mushroom bran
- composite material
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Organic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of preparation method of mushroom bran carbon load zero-valent iron composite material and its applications in oil pollution wastewater treatment, it is reducing agent using sodium borohydride, ferrous ion is reduced to Zero-valent Iron, mushroom bran carbon is added in operation, utilize the Zero-valent Iron of the pore structure load reduction of mushroom bran carbon, stable composite material is formed, to handle oil pollution waste water.This method is easy to operate, and the addition of mushroom bran carbon overcomes the unstable disadvantage easy to reunite of nano zero valence iron, can play the suction-operated of mushroom bran carbon in oil removal process simultaneously and the high reduction of Zero-valent Iron, oil removal rate can reach 95.5% or more, excellent wastewater treatment effect.
Description
Technical field
The present invention relates to oil pollution waste water treatment fields, and in particular to a kind of mushroom bran carbon load zero-valent iron composite material system
Preparation Method and its application in oil pollution waste water treatment.
Background technique
In recent years, development of oil industry is rapid, and petroleum is revealed in several ways in exploitation, transport and process,
Substantial oil enters water body, causes water pollution, seriously endangers environment and human health.At currently used oil pollution waste water
Reason method mainly has bioanalysis, physical method, a chemical method, however the generally existing various disadvantages of these methods, as equipment cost is big, easily
Cause secondary pollution, generate more sludge etc., therefore it is useless to look for a kind of completely new efficient, quick, economic, environmentally friendly oil pollution
Method for treating water is extremely urgent.
Nano zero valence iron is cheap, reducing power is relatively strong and will not generate noxious material in use, has been used for
The improvement of various water bodies pollutant.However, go deep into research, extraction and nanometer iron metal there are the problem of also gradually manifest
Come, firstly, its partial size is smaller, the attraction between particle is stronger, easily reunites；Secondly, individual nano zero valence iron is not
Stablize, is easily oxidized, influences its reactivity.
To overcome the above disadvantages, often select porous material by nano zero valence iron immobilization at present, it is known that carrier material
Mainly there are resin, active carbon, tripoli etc., these carrier materials will receive non-natural existing region and the conditions such as non-renewable
And lack the limitation of availability.Therefore a kind of sustainable and widely applied carrier material is selected to seem especially urgent.
Summary of the invention
For the drawbacks described above for solving currently available technology technology, the present invention provides a kind of mushroom bran carbon load Zero-valent Iron composite wood
The method of material processing oil pollution waste water.
The principle of the present invention is: being reducing agent using sodium borohydride, ferrous ion is reduced to Zero-valent Iron, in operating process
Middle addition mushroom bran carbon forms stable composite material, to handle stone using the Zero-valent Iron of the pore structure load reduction of mushroom bran carbon
Oily pollution waste water.This method is easy to operate, and the addition of mushroom bran carbon overcomes the unstable disadvantage easy to reunite of nano zero valence iron, oil removing
The suction-operated of mushroom bran carbon and the high reduction of Zero-valent Iron can be played simultaneously in the process, oil removal rate can reach 95.5% or more, place
It is good to manage waste water effect.
Based on above-mentioned purpose and principle, the present invention adopts the following technical scheme:
One of present invention is to provide a kind of preparation method of mushroom bran carbon load zero-valent iron composite material, comprising the following steps:
(1) it will be pyrolyzed under nitrogen atmosphere after mushroom bran cleaning, drying, then obtain mushroom bran carbon through crushing；
(2) gained mushroom bran carbon is added to FeSO4·7H2In O ethanol water, impregnated after sonic oscillation；
(3) polyethylene glycol-4000 is added after the completion of dipping as dispersing agent and stirs completely, then leads to nitrogen deoxygenation；
(4) logical nitrogen is kept, sodium borohydride solution is added dropwise and sufficiently reacts；The sodium borohydride solution additional amount is with Fe2+: BH4-'s
Molar ratio is equal to 1:(3-5) subject to；
(5) solid phase is collected by centrifugation in the mixed liquor after reaction, and solid phase is repeatedly washed with by the distilled water and ethyl alcohol of nitrogen；
(6) material after washing is dry, and be stored at anaerobic dark.
It is further preferred that pyrolysis time is 3 h in the step (1), pyrolysis final temperature is 450 DEG C, heating rate 10
℃/min。
It is further preferred that FeSO in the step (2)4·7H2The concentration of O ethanol water is 0.1 mol/L, wherein
Water and ethyl alcohol volume ratio are 3:1.
It is further preferred that FeSO in the step (2)4·7H2The mass ratio of O and mushroom bran carbon is 1:1.01.
It is further preferred that 30 min of sonic oscillation in the step (2), impregnates 24 hours.
It is further preferred that the reaction time is 30min in the step (4)；Fe2+: BH4 -Molar ratio be 1:4
It is further preferred that dry in the step (5) use 70-80 DEG C of drying in a vacuum drying oven.
One of present invention is to provide a kind of application of mushroom bran carbon load zero-valent iron composite material, that is, it is useless to be added to oil pollution
For removing oil therein in water.
Further, that mushroom bran carbon load zero-valent iron composite material according to the mass ratio of 3-10% is added to crude oil is dense
Degree is mixed processing in the oil pollution waste water of 0.4-1g/L.
Still more preferably, mushroom bran carbon load zero-valent iron composite material is added to crude oil according to 5% mass ratio
Concentration is in the oil pollution waste water of 1g/L, and in 30 DEG C of isothermal reaction 5h；The particularly preferably oscillating reactions at 250 rpm.
Still more preferably, oil pollution waste water control pH is 4-0, especially preferably 4.
Compared with prior art, the invention has the following advantages:
(1) operation of the present invention is simple, and it is cheap and easy to get to prepare raw material, can play agricultural wastes as raw material using mushroom bran carbon and recycle
Effect；
(2) compared with individual nano zero valence iron, the present invention is capable of increasing nano zero-valence using mushroom bran carbon load nano zero valence iron
Iron specific surface area keeps its more stable, can overcome nano zero valence iron it is oxidizable, it is easy to reunite, pollutant process effect difference is lacked
Point.
(3) present invention can also play material to the suction-operated of pollutant and the high reduction of nano zero valence iron, play
Mushroom bran carbon and nano zero valence iron act on the removal of petroleum pollution, and the treatment effect of oil pollution waste water is substantially improved.
Detailed description of the invention
Fig. 1 is that individual nano zero valence iron, mushroom bran carbon and mushroom bran carbon prepared by the present invention load zero-valent iron composite material
SEM figure, left figure are individual nano zero valence iron, and centre is mushroom bran carbon, and right figure is that mushroom bran carbon loads zero-valent iron composite material.
Fig. 2 is that individual nano zero valence iron, mushroom bran carbon and mushroom bran carbon prepared by the present invention load zero-valent iron composite material
TEM figure, left figure are individual nano zero valence iron, and centre is mushroom bran carbon, and right figure is that mushroom bran carbon loads zero-valent iron composite material.
Fig. 3 is that the mushroom bran carbon load zero-valent iron composite material in embodiment 2 is bent to the when m- oil removal rate of oil pollution waste water
Line chart.
Fig. 4 is that the different mushroom bran carbon amounts in embodiment 3 load composite material processing oil pollution waste water prepared by Zero-valent Iron
When m- oil removal rate curve graph.
Fig. 5 be embodiment 4 in different pH under mushroom bran carbon load zero-valent iron composite material to oil pollution waste water when it is m-
Oil removal rate curve graph.
Fig. 6 is that mushroom bran carbon loads zero-valent iron composite material to oil pollution under the different crude oils initial concentration in embodiment 5
The when m- oil removal rate curve graph of waste water.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The preparation of 1 mushroom bran carbon of embodiment load zero-valent iron composite material
A, laboratory is taken to buy mushroom bran, distilled water cleans repeatedly, and the mushroom bran after drying is placed in crucible by drying, surface package
Masking foil is pyrolyzed 3 h to completely cut off air under nitrogen range in 450 DEG C in tubular heater, and setting heating rate is 10 DEG C/
Min is pyrolyzed products therefrom, that is, mushroom bran carbon, mushroom bran carbon is ground in mortar, crosses 20 meshes, in case subsequent use.
B, 2.7805 g FeSO are accurately weighed4·7H2O is dissolved in 100 mL, 25% ethanol water, and adds a small amount of iron
Powder prevents ferrous ions, takes in 2.8 g mushroom bran carbon vitriolization ferrous iron ethanol water obtained in step (1), ultrasound
30 min are vibrated, are impregnated 24 hours.
C, 0.5 g polyethylene glycol-4000 is added in step (b) solution as dispersing agent to be transferred to after stirring completely
250 mL three-necked flasks lead to nitrogen 15 minutes and remove wherein oxygen, one lead directly to nitrogen later.
D, 50 mL are added dropwise into the flask of step (c), 0.4 mol/L sodium borohydride solution makes Fe2+: BH4 -Molar ratio
For 1:4, stirred 30 minutes after being added dropwise.
E, liquid is centrifuged after step (d), is washed repeatedly with the distilled water and dehydrated alcohol by nitrogen, in 70 DEG C
It dries in a vacuum drying oven.It is stored at anaerobic dark.Its SEM figure is as shown in Figure 1, TEM figure is as shown in Figure 2.
Fig. 1, Fig. 2 are respectively that individual nano zero valence iron, mushroom bran carbon and mushroom bran carbon prepared by the present invention load Zero-valent Iron are multiple
SEM, TEM of condensation material scheme；Nano zero valence iron is in bright spherical shell structure as seen from the figure, since its magnetic action is gathered into
For miniliform long-chain, increase rapidly its partial size；Biological carbon surface is smooth, is being averaged for porous structure, hole prosperity, and hole
Diameter is greater than 1 μm, is conducive to the entrance of nano zero valence iron；Compared with individual nano zero valence iron, the addition of germ bran biological charcoal can
Obviously to prevent the agglomeration of nano zero valence iron.
2 mushroom bran carbon of embodiment loads the research of zero-valent iron composite material processing oil pollution waste water
(1) it takes 0.02 g crude oil to be placed in 50 mL centrifuge tubes, 20 mL distilled water is added, forming crude oil concentration is 1000 mg/L
Oil pollution waste water.
(2) 1.0 g of material prepared in Example 1 places it in water bath with thermostatic control oscillation in the centrifuge tube of step (1)
In device, vibrated under 30 DEG C, 250 rpm.
(3) completion that feeds intake starts timing, respectively at 1 h, 2 h, 3 h, 4 h, 5 h sampling, investigates petroleum hydrocarbon in waste water
Changes of contents, concrete outcome such as Fig. 3.
From figure 3, it can be seen that testing within 1 h of initial stage, material is to the removal rate very little of petroleum hydrocarbon, only 6%, work as reality
When testing progress 2h, material increases rapidly the degradation rate of petroleum hydrocarbon, can reach 79%, and after 3 h, material removes petroleum hydrocarbon
Except speed slows down gradually, after experiment carries out 5 h, iron carbon composite finally may be up to 95% to the removal rate of petroleum hydrocarbon.
The effect ratio of the composite material processing oil pollution waste water of the different mushroom bran carbon amounts load Zero-valent Iron preparations of embodiment 3
Compared with
(1) the made mushroom bran carbon of 2.8 g, 5.6 g, 8.4 g embodiment, 1 step (a) is weighed respectively, according to the preparation side of embodiment 1
Step (b)-(e) in method obtains 3 kinds of mushroom bran carbon and loads zero-valent iron composite material.
(2) material will be made in step (1) to be added in oil pollution waste water according to method in embodiment 2, investigates 3 kinds of materials
To the removal effect of petroleum hydrocarbon, concrete outcome such as Fig. 4.
As shown in figure 4, experiment initial stage, with the increase of mushroom bran carbon amounts, material gradually rises the removal rate of petroleum hydrocarbon；So
And test carry out 3 h after this trend it is just the opposite, i.e. removal rate highest of the least material of mushroom bran carbon amounts to petroleum, 5 h
When the material oil removal rate can reach 95%.
Influence of the initial pH of embodiment 4 to mushroom bran carbon load zero-valent iron composite material processing oil pollution waste water
(1) 2 Crude Oil pollutant effluents pH to 4.00 of embodiment is adjusted using 1 mol/L NaOH solution and HCl solution, 7.04,
10.08。
(2) three kinds of oil pollutions that step (1) is added according to method in embodiment 2 in the material prepared in Example 1 are useless
In water, removal effect of the material to different waste water petroleum hydrocarbons, concrete outcome such as Fig. 5 are investigated.
As shown in Figure 5, pH can influence reacting between material and petroleum hydrocarbon and the increase with wastewater pH, and material is to petroleum
The removal rate of hydrocarbon is gradually reduced.When pH is 4.00,5 h oil removal rates can reach 95.5%.Simultaneously petroleum hydrocarbon removal rate Integral Differential away from
It is not very greatly, to illustrate that the addition of germ bran biological charcoal being capable of influence of the buffer pH to nano zero valence iron and petroleum hydrocarbon reaction.
Influence of the 5 crude oil initial concentration of embodiment to mushroom bran carbon load zero-valent iron composite material processing oil pollution waste water
(1) it takes 0.0008,0.012,0.016,0.02 g crude oil to be placed in 50 mL centrifuge tubes respectively, 20 mL distilled water is added,
Formation crude oil concentration is 400 mg/L, 600 mg/L, 800 mg/L, and the oil pollution waste water of 1000 mg/L utilizes 1 mol/L
NaOH solution and HCl solution adjust each wastewater pH to 4.00.
(2) four kinds of oil pollutions that step (1) is added according to method in embodiment 2 in the material prepared in Example 1 are useless
In water, removal effect of the material to different waste water petroleum hydrocarbons, concrete outcome such as Fig. 6 are investigated.
As seen from Figure 6, with the increase of crude oil initial concentration, mushroom bran carbon loads zero-valent iron composite material to petroleum hydrocarbon
Removal rate gradually increase.Illustrate that 1 g material has enough reduction adsorption sites to handle the crude oil of the quality.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of preparation method of mushroom bran carbon load zero-valent iron composite material, which comprises the following steps:
(1) it will be pyrolyzed under nitrogen atmosphere after mushroom bran cleaning, drying, then obtain mushroom bran carbon through crushing；
(2) gained mushroom bran carbon is added to FeSO4·7H2In O ethanol water, impregnated after sonic oscillation；
(3) polyethylene glycol-4000 is added after the completion of dipping as dispersing agent and stirs completely, then leads to nitrogen deoxygenation；
(4) logical nitrogen is kept, sodium borohydride solution is added dropwise and sufficiently reacts；The sodium borohydride solution additional amount is with Fe2+: BH4 -'s
Molar ratio is equal to 1:(3-5) subject to；
(5) solid phase is collected by centrifugation in the mixed liquor after reaction, and solid phase is repeatedly washed with by the distilled water and ethyl alcohol of nitrogen；
(6) material after washing is dry, and be stored at anaerobic dark.
2. the preparation method of mushroom bran carbon load zero-valent iron composite material according to claim 1, which is characterized in that described
Pyrolysis time is 3 h in step (1), and pyrolysis final temperature is 450 DEG C, and heating rate is 10 DEG C/min.
3. the preparation method of mushroom bran carbon load zero-valent iron composite material according to claim 1, which is characterized in that described
FeSO in step (2)4·7H2The concentration of O ethanol water is that 0.1 mol/L, wherein water and ethyl alcohol volume ratio are 3:1.
4. the preparation method of mushroom bran carbon load zero-valent iron composite material according to claim 1, which is characterized in that the step
Suddenly FeSO in (2)4·7H2The mass ratio of O and mushroom bran carbon is 1:1.01.
5. the preparation method of mushroom bran carbon load zero-valent iron composite material according to claim 1, which is characterized in that described
30 min of sonic oscillation in step (2) impregnates 24 hours.
6. the preparation method of mushroom bran carbon load zero-valent iron composite material according to claim 1, which is characterized in that the step
Suddenly the reaction time is 30min in (4)；Fe2+: BH4 -Molar ratio be 1:4.
7. the preparation method of mushroom bran carbon load zero-valent iron composite material according to claim 1, which is characterized in that the step
Suddenly dry in (5) to use 70-80 DEG C of drying in a vacuum drying oven.
8. the application method for the mushroom bran carbon load zero-valent iron composite material that any one of the claim 1-7 preparation method obtains,
It is characterized in that, being added in oil pollution waste water for removing oil therein.
9. the application method of mushroom bran carbon load zero-valent iron composite material according to claim 8, which is characterized in that by the bacterium
Chaff carbon loads zero-valent iron composite material and is added in the oil pollution waste water that crude oil concentration is 1g/L according to 5% mass ratio, and in
In 30 DEG C of isothermal reaction 5h.
10. the application method of mushroom bran carbon load zero-valent iron composite material according to claim 8 or claim 9, which is characterized in that described
It is 4 that oil pollution waste water, which controls pH,.
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| CN112047419A (en) * | 2020-08-20 | 2020-12-08 | 哈尔滨工业大学 | Method for treating organic wastewater by rapidly adsorbing and catalytically oxidizing Congo red |
| CN115676803A (en) * | 2022-08-31 | 2023-02-03 | 洛阳生命宝石科技有限公司 | Extraction process of organism diamond raw material carbon |
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