CN107032474A - A kind of method of alta-mud load sulfide modifier nanometer iron composite material processing waste water containing chrome under magnetic fields - Google Patents
A kind of method of alta-mud load sulfide modifier nanometer iron composite material processing waste water containing chrome under magnetic fields Download PDFInfo
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- CN107032474A CN107032474A CN201710419858.5A CN201710419858A CN107032474A CN 107032474 A CN107032474 A CN 107032474A CN 201710419858 A CN201710419858 A CN 201710419858A CN 107032474 A CN107032474 A CN 107032474A
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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
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/48—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
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to a kind of method of alta-mud load sulfide modifier nanometer iron composite material processing waste water containing chrome under magnetic fields, step is：Alta-mud load sulfide modifier nano-iron material, under magnetic fields, stirring reaction are added into chromate waste water.The present invention improves the reactivity of alta-mud load sulfide modifier Nanoscale Iron by the method for sulfide modifier and externally-applied magnetic field, accelerates the removal rate of heavy metal chromium.This method is much larger than alta-mud loaded nano iron for the removal efficiency of chromium, and alta-mud load sulfide modifier nano-iron material using it is simple, reduce added amount of chemical, it is environment-friendly；It is with a wide range of applications in terms of the wastewater treatment containing heavy metal.
Description
Technical field
The invention belongs to water treatment field, and in particular to a kind of alta-mud load sulfide modifier nanometer iron composite material is in magnetic
The method of processing waste water containing chrome under field action.
Background technology
Heavy metal chromium, especially Cr VI, have been classified as with potential carcinogenicity, to human body, animal, plant and micro-
Biology has high causing toxicity.The processing method of current chromate waste water mainly has chemical precipitation method, ion-exchange and membrane separation process.Change
Learn the precipitation method and calcium hydroxide is mainly added into waste water, but calcium hydroxide dosage is too big, can produce largely containing heavy metal-polluted
Mud ion；Exchange process complex process, the easy aging of resin；Membrane separation process cost is too high, and fenestra is easily blocked.Find high activity material
The chromium that material is removed in waste water is paid close attention to by water treatment field.
Removing chromium with Zero-valent Iron, especially nano zero valence iron becomes a very active research field, but in reality
Zero-valent iron material, which still has some problems, in needs solution, the synthesis condition of such as nano zero valence iron is whard to control,
Easily reunite, air stability difference and hydrophily difference etc..Alta-mud loaded nano iron is to the removal of Cr VI in waste water compared with nanometer
Zero-valent Iron clearance increases, such as：Chinese patent document CN101314496A discloses a kind of modified alta-mud loaded nano
Hot metal treating agent, after modified alta-mud is uniformly mixed for 3: 7~9: 1 by weight with Nanoscale Iron, is reduced using strong reductant,
It is prepared into modified alta-mud loaded nano-hot metal treating agent.Although the effect such as bentonitic Coulomb repulsion and steric hindrance can make iron
Particle is difficult aggregation, is not easy to be oxidized, still, bentonite surface is negatively charged, and Nanoscale Iron hydrophobicity is stronger, to anion chromic acid
The adsorption capacity of root is still weaker, and removal effect is not ideal enough.
The content of the invention
For the defect of prior art, especially alta-mud loaded nano iron adsorption capacity is poor in the prior art, and
The poor defect of reactivity.The present invention provides a kind of alta-mud load sulfide modifier nanometer iron composite material under magnetic fields
The method of processing waste water containing chrome.This method can be greatly enhanced the removal efficiency of chromium, and with it is environment-friendly, use letter
Single, added amount of chemical is few, with low cost, the advantages of be applicable relatively wide, solves the deficiency of Zero-valent Iron application aspect.
Alta-mud loaded nano iron is carried out simple sulfide modifier by the present invention, prepares alta-mud load sulfide modifier
Nano-iron material, is used for processing waste water containing chrome under weak magnetic field action by the material.
Technical scheme is as follows：
A kind of method of alta-mud load sulfide modifier nanometer iron composite material processing waste water containing chrome under magnetic fields, bag
Include step as follows：
The addition alta-mud load sulfide modifier nano-iron material into chromate waste water, the stirring reaction under magnetic field condition, i.e.,
Complete the processing of chromate waste water.
, according to the invention it is preferred to, concentration≤100mg/L of chromium in 0 ＜ waste water, chromium in further preferred 0 ＜ waste water
Concentration≤50mg/L.
, according to the invention it is preferred to, magnetic field intensity≤20mT of described magnetic field condition；Further preferably, can be in waste water
Place the non-uniform magnetic-field that annular magnet provides magnetic field intensity≤20mT in treatment reactor bottom.
, according to the invention it is preferred to, the dosage of alta-mud load sulfide modifier nano-iron material is 0.1-1g/L waste water.
, according to the invention it is preferred to, the speed of agitator of stirring reaction is 300-500r/min, further preferred 400r/
min；
It is preferred that, the stirring reaction time is 10-60min.
According to the present invention, when reaction proceeds to 3min, the clearance of chromium can reach 79%, and reaction proceeds to chromium after 15min
Clearance up to more than 94%.
, according to the invention it is preferred to, sulphur iron mol ratio is in described alta-mud load sulfide modifier nano-iron material
0.5-0.6:1, further preferred 0.56：1；
It is preferred that, sulfide modifier nano zero valence iron and bentonite in described alta-mud load sulfide modifier nano-iron material
Mass ratio is 1:1.
, according to the invention it is preferred to, chromate waste water is adjusted to acid or neutral；It is further preferred that by chromate waste water
Adjust to pH=4-7, most preferably 4-5.
, according to the invention it is preferred to, described alta-mud load sulfide modifier nano-iron material is prepared as follows
Arrive：
(A) sodium borohydride and sodium thiosulfate are dissolved in ethanol water, obtain mixed liquor；
(B) bentonite is added into step (A) mixed liquor, be well mixed；
(C) nitrogen is passed through into step (B) mixed liquor, stirring removes oxygen；
(D) liquor ferri trichloridi is added into step (C) mixed liquor, persistently stirs 30-40min, obtain containing bentonite
The mixed solution of load vulcanization modified Nano iron material；
(E) product for obtaining step (D) carries out separation of solid and liquid, and solid vacuum freeze drying obtains alta-mud load sulphur
Change modified Nano iron material.
According to the preparation method of alta-mud load sulfide modifier nano-iron material of the present invention, it is preferred that ethanol in step (A)
The volume ratio of ethanol and water is 1 in the aqueous solution：(3-5), further preferred 1:4；
It is preferred that, the mass ratio of sodium borohydride and sodium thiosulfate is 1：(0.34-0.5), the quality and second of sodium borohydride
The volume ratio of alcohol solution is 1：(450-500)g/mL.
According to the preparation method of alta-mud load sulfide modifier nano-iron material of the present invention, it is preferred that by most in step (B)
Whole sulfide modifier nano zero valence iron is 1 with bentonite mass ratio:The 1 bentonitic addition of control；
According to the preparation method of alta-mud load sulfide modifier nano-iron material of the present invention, it is preferred that trichlorine in step (D)
It is (2-3) to change the addition of iron with the mass ratio of sodium borohydride in step (A)：1；
It is preferred that, the concentration of liquor ferri trichloridi is 9-10g/L.
According to the preparation method of alta-mud load sulfide modifier nano-iron material of the present invention, it is preferred that solid-liquid in step (E)
The mode of separation is centrifugation.
Beneficial effects of the present invention are as follows：
The present invention removes the waste water containing heavy metal chromium to alta-mud load sulfide modifier nano-iron material under weak magnetic field action
Studied, it is found that alta-mud load sulfide modifier nano-iron material can be greatly enhanced the reaction work of alta-mud loaded nano iron
Property, while low-intensity magnetic field can significantly improve the activity of alta-mud load sulfide modifier nano-iron material, accelerate the removal of pollutant.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of alta-mud load sulfide modifier nano-iron material made from embodiment 1.
Fig. 2 is the curve drawn to the processing procedure of the heavy metal chromium in waste water in test example 1.
Fig. 3 is the curve drawn to the processing procedure of the heavy metal chromium in waste water in test example 2.
Embodiment
With reference to specific embodiment, the present invention is described further, but the scope of protection of present invention is not only
It is limited to this.
The table-type low-speed centrifuge that centrifuge used produces for the permanent promise experimental instruments and equipment limited in Hunan in embodiment；Very
Vacuum freecing-dry device is Shanghai than freeze drier that bright instrument manufacturing Co., Ltd produces.
Alta-mud load sulfide modifier nano-iron material used, is prepared as follows obtaining in embodiment：
(A) by 0.2027g sodium borohydrides and 0.0871g sodium thiosulfate be dissolved in 100mL ethanol solutions (80mL ethanol,
20mL water) in, obtain mixed liquor；
(B) mixed liquor described in step (A) is moved in three-necked flask, and adds 0.1g bentonites, sulfide modifier is received
Rice Zero-valent Iron is 1 with bentonite mass ratio:1；
(C) nitrogen gas stirring will be passed through 10 minutes in step (B) described mixed liquor, removes the oxygen in mixed liquor；
(D) claim 0.4827g iron chloride to be dissolved in 50mL water, ferric chloride solution is transferred in pear-shaped flask；
(E) under conditions of lasting stirring and being passed through nitrogen, by the ferric chloride solution described in step (D) with 2-3 drops/sec
Rate of addition is added in the three-necked flask described in step (B), and reaction continues to stir 40 minutes after terminating, and mixing speed is 250 turns/
Minute；Obtained mixed liquor carries out separation of solid and liquid, and the solid of acquisition is washed 3 times using absolute ethyl alcohol, solid vacuum refrigeration is done
Dry to stay overnight, it is alta-mud load sulfide modifier nanometer iron composite material to obtain black solid, and nitrogen is stored in before sample use
It is prevented to be oxidized in gas atmosphere.
In obtained alta-mud load sulfide modifier nano-iron material, sulphur iron mol ratio is 0.56：1.
Embodiment 1：
A huge sum of money in removing waste water in the presence of additional low-intensity magnetic field using alta-mud load sulfide modifier nano-iron material
Belong to the method for chromium, chromium content is 25mg/L waste water in the waste water, including step is as follows：
The waste water 1L containing chromium is taken, is placed in reactor, 0.1mol/L sodium hydroxides regulation pH=5 is added；Add 0.2g swollen
Moisten soil load vulcanization modified Nano iron material, annular magnet is placed in reactor bottom, the non-equal of magnetic field intensity≤20mT is provided
Even low-intensity magnetic field, with rotating speed 400r/min stirring reactions to 3min under the weak magnetic field action, the clearance of chromium is up to more than 79%.
Continue with rotating speed 400r/min stirring reactions to 15min, the clearance approximate exact of chromium to 94%.
Embodiment 2：
A huge sum of money in removing waste water in the presence of additional low-intensity magnetic field using alta-mud load sulfide modifier nano-iron material
Belong to the method for chromium, chromium content is 25mg/L waste water in the waste water, including step is as follows：
The waste water 1L containing chromium is taken, is placed in reactor, 0.1mol/L sodium hydroxides regulation pH=5 is added；Add 0.5g swollen
Moisten soil load vulcanization modified Nano iron material, annular magnet is placed in reactor bottom, the non-equal of magnetic field intensity≤20mT is provided
Even low-intensity magnetic field, with rotating speed 400r/min stirring reactions 10 minutes under the weak magnetic field action, the clearance of chromium reaches 94%.
Embodiment 3：
A huge sum of money in removing waste water in the presence of additional low-intensity magnetic field using alta-mud load sulfide modifier nano-iron material
Belong to the method for chromium, chromium content is 25mg/L waste water in the waste water, including step is as follows：
The waste water 1L containing chromium is taken, is placed in reactor, 0.1mol/L sodium hydroxides regulation pH=5 is added；Add 1g swellings
Soil load vulcanization modified Nano iron material, places annular magnet in reactor bottom, provides the non-homogeneous of magnetic field intensity≤20mT
Low-intensity magnetic field, with rotating speed 400r/min stirring reactions 3 minutes under the weak magnetic field action, the clearance of chromium reaches 94%.
Embodiment 4
As described in Example 1, unlike：
Adjust the pH=4 of chromate waste water.
Embodiment 5
As described in Example 1, unlike：
Adjust the pH=6 of chromate waste water.
Embodiment 6
As described in Example 1, unlike：
Adjust the pH=7 of chromate waste water.
Comparative example 1,
As described in Example 1, unlike：
Heavy metal chromium in waste water is removed using alta-mud loaded nano iron material, is prepared as follows obtaining：
(A) 0.2027g sodium borohydrides are dissolved in 100mL ethanol solutions (80mL ethanol, 20mL water), obtain mixed liquor；
(B) mixed liquor described in step (A) is moved in three-necked flask, and adds 0.1g bentonites, make nano zero valence iron
It is 1 with bentonite mass ratio:1；
(C) nitrogen gas stirring will be passed through 10 minutes in step (B) described mixed liquor, removes the oxygen in mixed liquor；
(D) claim 0.4827g iron chloride to be dissolved in 50mL water, ferric chloride solution is transferred in pear-shaped flask；
(E) under conditions of lasting stirring and being passed through nitrogen, by the ferric chloride solution described in step (D) with 2-3 drops/sec
Rate of addition is added in the three-necked flask described in step (B), and reaction continues to stir 40 minutes after terminating, and mixing speed is 250 turns/
Minute；Obtained mixed liquor carries out separation of solid and liquid, and the solid of acquisition is washed 3 times using absolute ethyl alcohol, solid vacuum refrigeration is done
Dry to stay overnight, it is alta-mud loaded nano iron composite material to obtain black solid.
And it is not added with magnetic field during processing waste water.
Comparative example 2
As described in Example 1, unlike：
Magnetic field is not used to be acted on.
Test example 1
Embodiment 1 and comparative example 1-2 are drawn into curve to the processing procedure of the heavy metal chromium in waste water, as shown in Figure 2.
As shown in Figure 2, the processing method of embodiment 1 in the clearance approximate exact of 15min chromium to 94%；Comparative example 2
Do not use magnetic field to be acted on, 45min is needed when the clearance approximate exact of chromium is to 94%；Magnetic field is not used in comparative example 1
And remove the heavy metal chromium in waste water using alta-mud loaded nano iron material, handle the clearance of 60min chromium only up to
78%.It can be seen that, processing method of the invention can reach higher chromium removal efficiency in the most short time.
Test example 2
Embodiment 1 and embodiment 4-6 are drawn into curve to the processing procedure of the heavy metal chromium in waste water, as shown in Figure 3.
As shown in Figure 3, the processing method of embodiment 1 in the clearance approximate exact of 15min chromium to 94%；Embodiment 4
Initial pH on wastewater=4 are adjusted, clearance and the embodiment 1 of chromium are more or less the same；Initial pH on wastewater=6, processing are adjusted in embodiment 5
Method 15min chromium clearance approximate exact to 83%；Initial pH on wastewater=7 are adjusted in embodiment 6, processing method exists
The clearance approximate exact of 15min chromium is to 75%.It can be seen that, processing method of the invention can reach higher in acid waste water
Chromium removal efficiency.
Claims (10)
1. a kind of method of alta-mud load sulfide modifier nanometer iron composite material processing waste water containing chrome under magnetic fields, including
Step is as follows：
Alta-mud load sulfide modifier nano-iron material is added into chromate waste water, the stirring reaction under magnetic field condition completes
The processing of chromate waste water.
2. according to the method described in claim 1, it is characterised in that concentration≤100mg of chromium in 0 ＜ waste water.
3. according to the method described in claim 1, it is characterised in that magnetic field intensity≤20mT of described magnetic field condition.
4. according to the method described in claim 1, it is characterised in that the dosage of alta-mud load sulfide modifier nano-iron material
For 0.1-1g/L waste water.
5. according to the method described in claim 1, it is characterised in that the speed of agitator of stirring reaction is 300-500r/min, is stirred
The reaction time is mixed for 10-60min.
6. according to the method described in claim 1, it is characterised in that in described alta-mud load sulfide modifier nano-iron material
Sulphur iron mol ratio is 0.5-0.6:1.
7. according to the method described in claim 1, it is characterised in that in described alta-mud load sulfide modifier nano-iron material
Sulfide modifier nano zero valence iron is 1 with bentonite mass ratio:1.
8. according to the method described in claim 1, it is characterised in that adjust chromate waste water to acid or neutral.
9. according to the method described in claim 1, it is characterised in that described alta-mud load sulfide modifier nano-iron material is pressed
Following methods are prepared：
(A) sodium borohydride and sodium thiosulfate are dissolved in ethanol water, obtain mixed liquor；
(B) bentonite is added into step (A) mixed liquor, be well mixed；
(C) nitrogen is passed through into step (B) mixed liquor, stirring removes oxygen；
(D) liquor ferri trichloridi is added into step (C) mixed liquor, persistently stirs 30-40min, obtain containing alta-mud load
The mixed solution of sulfide modifier nano-iron material；
(E) product for obtaining step (D) carries out separation of solid and liquid, and solid vacuum freeze drying obtains alta-mud load vulcanization and changed
Property nano-iron material.
10. method according to claim 9, it is characterised in that in step (A) in ethanol water ethanol and water volume
Than for 1：The mass ratio of (3-5), sodium borohydride and sodium thiosulfate is 1：(0.34-0.5), the quality and ethanol water of sodium borohydride
The volume ratio of solution is 1：(450-500)g/mL.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601642A (en) * | 2017-10-13 | 2018-01-19 | 山东大学 | The method of complexing agent collaboration sulfide modifier Zero-valent Iron processing waste water from dyestuff |
| CN109570219A (en) * | 2018-11-12 | 2019-04-05 | 同济大学 | Heavy metal-polluted soil restorative procedure based on modified Zero-valent Iron |
| CN109821508A (en) * | 2019-01-15 | 2019-05-31 | 华北电力大学 | The preparation method and application of dictyophora phalloidea load vulcanization nano zero valence iron |
| CN110240249A (en) * | 2019-05-20 | 2019-09-17 | 中国地质大学（武汉） | One kind is gone down based on low-intensity magnetic field except heavy metal Cr in water body6+Method |
| CN112028131A (en) * | 2020-06-16 | 2020-12-04 | 暨南大学 | Vulcanized nano zero-valent iron and preparation method and application thereof |
| CN112427019A (en) * | 2020-08-11 | 2021-03-02 | 广西大学 | Anaerobic granular sludge loaded vulcanized nano zero-valent iron adsorbing material and preparation method and application thereof |
| CN113070076A (en) * | 2021-02-25 | 2021-07-06 | 山东大学 | Preparation method and application of zero-valent iron sulfide |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601642A (en) * | 2017-10-13 | 2018-01-19 | 山东大学 | The method of complexing agent collaboration sulfide modifier Zero-valent Iron processing waste water from dyestuff |
| CN109570219A (en) * | 2018-11-12 | 2019-04-05 | 同济大学 | Heavy metal-polluted soil restorative procedure based on modified Zero-valent Iron |
| CN109821508A (en) * | 2019-01-15 | 2019-05-31 | 华北电力大学 | The preparation method and application of dictyophora phalloidea load vulcanization nano zero valence iron |
| CN110240249A (en) * | 2019-05-20 | 2019-09-17 | 中国地质大学（武汉） | One kind is gone down based on low-intensity magnetic field except heavy metal Cr in water body6+Method |
| CN110240249B (en) * | 2019-05-20 | 2021-08-27 | 中国地质大学（武汉） | Remove heavy metal Cr in water under weak magnetic field6+Method (2) |
| CN112028131A (en) * | 2020-06-16 | 2020-12-04 | 暨南大学 | Vulcanized nano zero-valent iron and preparation method and application thereof |
| CN112028131B (en) * | 2020-06-16 | 2024-03-12 | 暨南大学 | Vulcanized nano zero-valent iron and preparation method and application thereof |
| CN112427019A (en) * | 2020-08-11 | 2021-03-02 | 广西大学 | Anaerobic granular sludge loaded vulcanized nano zero-valent iron adsorbing material and preparation method and application thereof |
| CN113070076A (en) * | 2021-02-25 | 2021-07-06 | 山东大学 | Preparation method and application of zero-valent iron sulfide |
| CN113070076B (en) * | 2021-02-25 | 2022-04-12 | 山东大学 | Preparation method and application of zero-valent iron sulfide |
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