CN107716942B - The method that ferronickel bimetallic material is prepared in situ using nickel ion pollutant effluents is repaired - Google Patents
The method that ferronickel bimetallic material is prepared in situ using nickel ion pollutant effluents is repaired Download PDFInfo
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- CN107716942B CN107716942B CN201710784183.4A CN201710784183A CN107716942B CN 107716942 B CN107716942 B CN 107716942B CN 201710784183 A CN201710784183 A CN 201710784183A CN 107716942 B CN107716942 B CN 107716942B
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- bimetallic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- 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
-
- 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
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The present invention relates to a kind of methods that Ni/Fe bimetallic material is prepared in situ using nickel ion pollutant effluents is repaired, comprising the following steps: (1) alta-mud load Zero-valent Iron is by bentonite, FeSO4·7H2O and NaBH4It is mixed together reaction, through deoxidized water and ethanol washing, vacuum freeze drying is prepared；(2) adjusting the pH containing heavy metal Ni (II) ion waste water is 3-7；(3) the alta-mud load Zero-valent Iron being prepared is mixed in an oscillator by inert gas shielding with containing heavy metal Ni (II) ion waste water；(4) after reaction, Ni/Fe bimetallic material is prepared in washed, vacuum freeze drying.Present invention process is simple, and cost is relatively low, does not generate secondary pollution to environment, is a kind of simple and effective, low in cost, green method for preparing Ni/Fe bimetallic material.
Description
Technical field
The invention belongs to material processing preparation and environment-friendly engineering technical fields, are specifically related to a kind of using alta-mud load
Zero-valent Iron repairs Ni (II) pollution, the method for being prepared in situ to obtain the Fe/Ni bimetallic material of high activity in waste water, and it is useless to reach change
For precious purpose.
Background technique
The features such as nano zero valence iron has large specific surface area, and reactivity is high is widely used in weight in environmental pollution water body
The organic matter degradations such as metal removal and nitrobenzene compounds.But since Zero-valent Iron is easy to reunite, surface is easy passivation, so that
Zero-valent Iron is to the dechlorination of the highly toxic chlorinatedorganic such as chlorinated phenol and chlorohydrocarbon and degradation effect and bad.In contrast, Ni/
Fe bimetallic material can not only slow down the ironing surface passivation of zeroth order, and Zero-valent Iron can also be reacted production with water by zero-valent metal Ni
Raw Hydrogen activation is reactive hydrogen atom, therefore has higher dechlorination and reduction activation, being capable of the highly toxic chlorine of efficient degradation
For organic matter.Currently, the common preparation method of Ni/Fe bimetallic material is in addition to utilizing hydrogen direct-reduction Fe (III) and Ni
(II) except mixture, mainly Ni (II) ion is added dropwise on a small quantity in zeroth order ferrous solution, passes through going back for Zero-valent Iron
Ni/Fe bimetallic material is made in original.This method is stringenter to the control of pH, and general pH is 6 or so, pH too low or excessively high all can
Influence the generation of bimetallic material.In addition, this method is also relatively stringenter to the control of Ni (II) concentration and content, once Ni(II)
Reaction surface that is excessive then will lead to nickel oxide and hydroxide covering Zero-valent Iron, to influence the bimetallic preparation of Ni/Fe
And reactivity.In general, Ni used (II) concentration is no more than 20ppm, and nickel content is no more than Fe content in bimetallic
10%.It can be seen that condition needed for the preparation method is harsher, the Ni (II) of additional toxic and easy pollution environment is also needed.And
And Zero-valent Iron due to reunite and its surface oxide layer passivation so that part Ni (II) is not reduced to zero-valent nickel.
If mishandling, it be easy to cause the heavy metal pollution of environment.
Metallic nickel is widely used in the industries such as alloy material and stainless steel preparation, plated film, due to arbitrarily discharging and handling not
When heavy metal Ni (II) increasingly accumulates in environment water, seriously threatens the health of people and the balance of ecological environment.Mesh
Before, common processing method has absorption, ion exchange and UF membrane etc., but these methods can not change the chemical valence state of Ni (II)
And toxicity.Although in nano zero valence iron has certain reducing power, the ironing surface oxide layer of zeroth order to hinder Ni (II)
The reduction of Zero-valent Iron verification Ni (II) in face can not reduce Ni (II) so that Ni (II) is largely attracted to zeroth order iron surface
Toxicity.Moreover, the solid material obtained using the administering method also can not secondary use, need further progress depth
Reason.Therefore, if can invent one kind can effectively remove Ni in polluted-water (II) and by the removal product secondary use in it
The method of the degradation of his environmental contaminants, can achieve turn waste into wealth, the purpose of the treatment of wastes with processes of wastes against one another, meet current sustainable development
It is required that.
For this purpose, the present invention is using bentonite as carrier loaded Zero-valent Iron, and the Ni(II to be polluted in waste water) it is raw material, lead to
Crossing Zero-valent Iron reduction Ni (II) dispersed on carrier is zero-valent nickel and carrier to remaining Ni (II) and Zero-valent Iron oxide on surface
Absorption, not only realized completely removing for Ni in polluted-water (II), but also a step in situ is prepared and has to chlorinatedorganic
The Ni/Fe bimetallic material of high degrading activity can be used for chloro so that the heavy metal nickel pollutant in waste water be turned waste into wealth
The reparation of the environment water and soil of organic pollution.This method simple process and low cost, while realizing and turn waste into wealth again
Purpose.But the Ni/Fe for up to the present, being prepared in situ to obtain high activity using Ni (II) pollution in Zero-valent Iron reparation waste water is bis-
Metal material yet there are no document report and patent disclosure.
Summary of the invention
The purpose of the present invention is to provide a kind of Ni that various concentration in waste water is repaired using alta-mud load Zero-valent Iron
(II) method that pollution is prepared in situ to obtain the Ni/Fe bimetallic material of high activity, a small amount of Ni is individually restored with Zero-valent Iron
(II), hydrogen reducing Fe (III) is compared with preparation methods such as Ni (II), and this method is with the heavy metal Ni (II) polluted in waste water
Raw material, and do not influenced (concentration range 10-500ppm) by the variation of Ni (II) concentration, pH adaptability is wider, can not only be effective
The Ni (II) that pollutes in removal waste water, moreover it is possible to make full use of heavy metal ion is secondary, the difficult drop of removal chlorohydrocarbon and chlorinated phenol etc.
Chloro pollutant is solved, achievees the purpose that turn waste into wealth.
In order to achieve the above objectives, the present invention is achieved by the following technical solutions:
A method of Ni/Fe bimetallic material being prepared in situ using nickel ion pollutant effluents is repaired, comprising the following steps:
(1) alta-mud load Zero-valent Iron is by bentonite, FeSO4·7H2O and NaBH4Be mixed together reaction, through deoxidized water and
Ethanol washing, vacuum freeze drying are prepared, and partial size is 50-300 mesh；
(2) adjusting the pH containing heavy metal Ni (II) ion waste water is 3-7；
(3) by the alta-mud load Zero-valent Iron being prepared and (II) ion waste water containing heavy metal Ni at one by indifferent gas
It is mixed in the oscillator of body protection, wherein Ni (II) concentration is 10-500ppm, and Fe content is 1.2 times or more of Ni (II) content；
(4) after reaction, Ni/Fe bimetallic material is prepared in washed, vacuum freeze drying.
Bentonite, the FeSO of the step (1)4·7H2O and NaBH4Weight ratio be 5:1:2.
The revolving speed of oscillator is 100-200r/min in the step (3), and reaction time 2-4h, temperature is 20-40 DEG C.
A kind of application that Ni/Fe bimetallic material being prepared in situ using multiple nickel ion pollutant effluents, in the reaction solution of pH5-7
In, a certain amount of pollutant is added, restores 1-3h using the Ni/Fe bimetallic material being prepared, obtains reduzate.
The pollutant is chloronitrobenzene, and the amount of pollutant is 10-100ppm.
The iron-content of the Ni/Fe bimetallic material is 20-50mg.
The present invention has using the method and its application that Ni/Fe bimetallic material is prepared in situ in nickel ion pollutant effluents are repaired
It is following the utility model has the advantages that
1, the present invention repairs the heavy metal Ni (II) in waste water using alta-mud load Zero-valent Iron for the first time, is prepared in situ to obtain
The Ni/Fe bimetallic material of high activity, the chlorinatedorganic polluted in the active material energy efficient degradation environment.The present invention takes into account
Heavy metal pollution in wastewater processing and pollutant secondary use, reaching turns waste into wealth, the purpose of the treatment of wastes with processes of wastes against one another.
2, compared with conventional Zero-valent Iron reduction Ni (II) method, the present invention can handle and completely remove various concentration
The activity of Ni (II) pollutant, obtained bimetallic material is not influenced by Ni (II) concentration and content, and pH adaptability is wider, work
Skill is simple, and material therefor is green material, risk without secondary pollution.
3, made from the conventional method compared with Ni/Fe bimetallic material, the dechlorination of bimetallic material produced by the present invention is living
Property is higher, and faster, stability is more preferable for speed.
4, compared with for the Ni/Fe bimetallic material of load, bentonite carrier used in the present invention is good to heavy metal ion
Suction-operated, it is possible to prevente effectively from the heavy metal ion such as the Fe (II) generated in reaction process, Fe (III) and Ni (II) are again
It is discharged into reaction solution.
5, reaction condition of the invention is mild, and low energy consumption.It can be reacted at normal temperatures and pressures, no heating refrigeration pressurization
Etc. energy consumptions, operating cost it is very low.
Detailed description of the invention
Fig. 1 is that sodium bentonite loads XPS figure of the Zero-valent Iron processing containing solid product after Ni (II) waste water；
Fig. 2 is that sodium bentonite loads Zero-valent Iron deoxygenization chlorination nitrobenzene；
Fig. 3 is that sodium bentonite loads Zero-valent Iron processing containing the product deoxygenization chlorination nitrobenzene after Ni (II) waste water；
Fig. 4 is that sodium bentonite load Zero-valent Iron handles Ni/ made from product and conventional method after containing Ni (II) waste water
The lot stability of Fe bimetallic material deoxygenization chlorination nitrobenzene compares.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, but protection scope of the present invention is not limited to
This.
Embodiment 1
(1) in N2Under protection, 0.5g/L sodium bentonite, 0.05mol/L FeSO4·7H2O and 0.1mol/L NaBH4It is mixed
Stirring 2 hours is closed, through deoxidized water, ethanol washing, alta-mud loaded nano Zero-valent Iron is made after vacuum freeze drying.
(2) alta-mud load Zero-valent Iron (iron-content 25mg) made from step (1) is weighed to be added to containing 200mg/L
In the waste water of Ni (II) (pH is adjusted to 6).In N2Under protection, oscillating reactions 2 hours (revolving speed 150rpm, 25 DEG C).Reaction terminates
Afterwards, centrifugation obtains solid, and measures remnants Ni(II in supernatant) removal rate that is zero, Ni (II) is 100%.The solid is through washing
It washs, vacuum freeze drying, and measured by XPS, which contains zero-valent nickel active component as shown in Figure 1, the result is confirmed swollen
During profit soil load Zero-valent Iron processing Ni (II), Fe/Ni (II) bimetallic is generated really.
(3) the identical alta-mud load Zero-valent Iron of Ni/Fe bimetallic material and iron-content that step (2) obtains is added respectively
Enter into the waste water containing 50mg/L chloronitrobenzene (p-CNB) (pH 5), N2Protecting lower oscillating reactions 2 hours, (revolving speed is
150rpm, 25 DEG C).After reaction, the product and its concentration in waste water are measured respectively.The results show that alta-mud load zeroth order
It is chloro aminobenzen (p-CAN) that iron, which restores resulting product, as shown in Fig. 2, substantially without dechlorination effect.In contrast, Ni/Fe is bis-
It is aniline (AN) that metal material, which restores resulting product, as shown in figure 3, nitro is not only reduced to amino, but also on phenyl ring
Chlorine is all sloughed, dechlorination efficiency 100%, shows very high dechlorination reaction activity.
Embodiment 2
(1) alta-mud load Zero-valent Iron is made according to the method for step (1) in embodiment (1).
(2) alta-mud load Zero-valent Iron (iron-content 15mg) made from step (1) is weighed to be added to containing 100mg/L
In the waste water of Ni (II) (pH is adjusted to 5), in N2Under protection, oscillating reactions 2 hours (revolving speed 150rpm, 25 DEG C).Reaction terminates
Afterwards, centrifugation obtains Ni/Fe bimetallic material, and measures remnants Ni(II in supernatant) removal rate that is zero, Ni (II) is 100%.
(3) (two kinds of Ni/Fe bimetallic material made from the Ni/Fe bimetallic material and conventional method obtained step (2)
The iron-content of material is identical), (pH 6), N are added separately in the waste water containing 20mg/L chloronitrobenzene2The lower oscillation of protection
Reaction 2 hours (revolving speed 150rpm, 25 DEG C).After reaction, the product and its concentration in waste water are measured respectively.As a result it shows
Show, dechlorination efficiency is 90% after Ni/Fe bimetallic material reductase 12 hour made from conventional method.In contrast, the present invention is made
Ni/Fe bimetallic material restore 0.5 hour after dechlorination efficiency reach 100%, show faster dechlorination speed and higher de-
Chlorine activity.
Embodiment 3
(1) alta-mud load Zero-valent Iron is made according to the method for step (1) in embodiment (1).
(2) alta-mud load Zero-valent Iron (iron-content 10mg) made from step (1) is weighed to be added to containing 50mg/L Ni
(II) in waste water (pH is adjusted to 6.5), in N2Under protection, oscillating reactions 1 hour (revolving speed 150rpm, 25 DEG C).Reaction terminates
Afterwards, centrifugation obtains Ni/Fe bimetallic material, and measures remnants Ni(II in supernatant) removal rate that is zero, Ni (II) is 100%.
(3) the Ni/Fe bimetallic material that step (2) obtains is added to (pH in the waste water containing 20mg/L parachlorophenol
For 6), N2Protect lower oscillating reactions 2 hours (revolving speed 150rpm, 25 DEG C).After reaction, the product in waste water is measured respectively
And its concentration.The results show that parachlorophenol is all reduced to phenol by Ni/Fe bimetallic material, illustrate parachlorophenol phenyl ring
On chlorine all slough, show very high dechlorination reaction activity.
Embodiment 4
Successively according to step (1), the method for (2) in embodiment (1), Ni/Fe bimetallic material is made.
By (the two kinds of materials of Ni/Fe bimetallic material made from Ni/Fe bimetallic material made from step (1) and conventional method
The iron-content of material is identical), (pH 6), N are added in the waste water containing 20mg/L chloronitrobenzene2Protect lower oscillating reactions 2 small
When (revolving speed 150rpm, 25 DEG C).After reaction, the chloronitrobenzene of same concentrations is added, successively reacts 5 batches in this way
It is secondary, by measuring each batch reaction after Aniline content, obtain each both bimetallic materials of batch reaction
Dechlorination activity.As a result such as Fig. 4 is shown, after reacting 5 batches, the dechlorination efficiency of bimetallic material made from conventional method is fallen to
70% or so, and the dechlorination efficiency of bimetallic material produced by the present invention is still maintained at 92% or more, shows higher reaction
Stability.
Present invention process is simple, and cost is relatively low, does not generate secondary pollution to environment, be it is a kind of it is simple and effective, low in cost,
The method that green prepares Ni/Fe bimetallic material.
Above-described embodiment is only used for illustrating inventive concept of the invention, rather than the restriction to rights protection of the present invention,
It is all to be made a non-material change to the present invention using this design, protection scope of the present invention should all be fallen into.
Claims (3)
1. a kind of method that Ni/Fe bimetallic material is prepared in situ using nickel ion pollutant effluents is repaired, it is characterised in that including
Following steps:
(1) alta-mud load Zero-valent Iron is by bentonite, FeSO4·7H2O and NaBH4It is mixed together reaction, through deoxidized water and ethyl alcohol
Washing, vacuum freeze drying are prepared, and partial size is 50-300 mesh；
(2) adjusting the pH containing heavy metal Ni (II) ion waste water is 3-7；
(3) the alta-mud load Zero-valent Iron being prepared is protected at one by inert gas with (II) ion waste water containing heavy metal Ni
It is mixed in the oscillator of shield, wherein Ni (II) concentration is 10-500ppm, and Fe content is 1.2 times or more of Ni (II) content；
(4) after reaction, Ni/Fe bimetallic material is prepared in washed, vacuum freeze drying.
2. the method that Ni/Fe bimetallic material is prepared in situ using nickel ion pollutant effluents is repaired as described in claim 1, special
Sign is: bentonite, the FeSO of the step (1)4·7H2O and NaBH4Weight ratio be 5:1:2.
3. the method that Ni/Fe bimetallic material is prepared in situ using nickel ion pollutant effluents is repaired as described in claim 1, special
Sign is: the revolving speed of oscillator is 100-200r/min in the step (3), and reaction time 2-4h, temperature is 20-40 DEG C.
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| CN201710784183.4A CN107716942B (en) | 2017-09-04 | 2017-09-04 | The method that ferronickel bimetallic material is prepared in situ using nickel ion pollutant effluents is repaired |
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