CN105251434B - The synthetic method of the flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation - Google Patents
The synthetic method of the flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation Download PDFInfo
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- CN105251434B CN105251434B CN201510769009.3A CN201510769009A CN105251434B CN 105251434 B CN105251434 B CN 105251434B CN 201510769009 A CN201510769009 A CN 201510769009A CN 105251434 B CN105251434 B CN 105251434B
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- methyl orange
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- room temperature
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Abstract
The invention discloses a kind of synthetic method of the flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation, belong to the synthesis technical field of nano material, substance A is dissolved in absolute ethyl alcohol, 5 ~ 15 min are stirred at 30 ~ 50 DEG C, the nitric acid that concentration is 16mol/L is added into obtained settled solution and is well mixed, A ethanol solution and the volume ratio of nitric acid are 200：1, mixed liquor is transferred in inner liner stainless steel kettle, mixed liquor heats 2 ~ 3 h in 150 ~ 250 DEG C, after temperature is down to room temperature, takes out sample, with 8000 ~ 12000 r/min centrifugation, washing, is finally dried in vacuum environment, at room temperature obtained；Wherein substance A is C2H6NiO4•4H2O or NiCl2In one kind.Preparation method is simple, and low cost materials are cheap, and has significant adsorption selectivity to organic dyestuff methyl orange.
Description
Technical field
The invention belongs to the synthesis technical field of nano material, is related to a kind of the flower-shaped of methyl orange high-selectivity adsorption separation
The synthetic method of nickel base nanometer material.
Background technology
With industry and the development of technology, dyestuff enters all kinds of industries as indispensable a kind of chemical permeation, such as
Print, electroplate, etc..However, the residual of dyestuff constitutes serious threat to the mankind and Environmental Health in trade effluent.Dyestuff is made
Into water pollution be the most serious of face of mankind nowadays the problem of one of.Therefore, the improvement for waste water containing dye has attracted
In the world increasing concern.At present, the most widely used method in the processing of sewage dyestuff has absorption, UF membrane, light to urge
Change degraded adsorption-flocculation and solidification.These methods are inexpensive, easily operated, efficiency high and simple design and operation, thus
It is the most commonly used.
Up to the present, many materials with excellent physics and chemistry and mechanical property have been used for research for dyestuff in water
Absorption property, such as clay material, activated carbon, CNT and alphabetical sponge.But still to show some bright for prior art
The drawbacks of aobvious, such as building-up process complexity, low cost materials are expensive, and poor selectivity, adsorption capacity are low in application process.
Given up it would therefore be desirable to pursue a kind of new simple adsorbent of inexpensive and synthetic method to handle dyestuff
Water.In addition, although existing substantial amounts of research reports effective Dye Adsorption, but rarely research is emphasized to dye mixture
Selective absorption.
The content of the invention
It is an object of the invention to provide a kind of synthesis of the flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation
Method, preparation method is simple, and low cost materials are cheap, and has efficient, quick Selective adsorption to organic dyestuff methyl orange
Energy.
The technical solution adopted in the present invention is a kind of flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation
Synthetic method, specifically follow the steps below：
Substance A is dissolved in absolute ethyl alcohol, concentration 0.005g/ml, stirred, the solution clarified, to what is obtained
The nitric acid that concentration is 16mol/L is added in settled solution and is well mixed, A ethanol solution and the volume ratio of nitric acid are 200：1,
Mixed liquor is transferred in inner liner stainless steel kettle, mixed liquor heats 2 ~ 3 h in 150 ~ 250 DEG C, after temperature is down to room temperature, takes out
Sample, centrifugation, and washed with distilled water and absolute ethyl alcohol, finally dry, produce in vacuum environment, at room temperature；Substance A is
C2H6NiO4•4H2O or NiCl2In one kind.
The present invention is further characterized in that further, the whipping temp is 30 ~ 50 DEG C, and the time is 5 ~ 15 min.
Further, centrifugal rotational speed is 8000 ~ 12000 r/min.
The beneficial effects of the invention are as follows synthesized a kind of to have methyl orange the new of high-selectivity adsorption effect at room temperature
There is efficient selective absorption to act on to the organic dyestuff methyl orange in sewage for type low cost nickel base nanometer material, the material,
It is further preferred that, methyl orange dye and other dyestuffs can be rapidly separated under alkaline environment, there is very high practicality, in sewage disposal
There is considerable application value with terms of environmental improvement.
Brief description of the drawings
Fig. 1 is the flower-shaped nickel base nanometer material electron microscope of the present invention.
Fig. 2 a are the adsorption effect figures for methyl orange dye.
Fig. 2 b are influence figure of the pH value to methyl orange dye adsorption effect.
Fig. 2 c be the present invention in methyl orange and rhodamine B mixed solution to the high-selectivity adsorption design sketch of methyl orange.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Embodiment 1：By 0.1 g C2H6NiO4•4H2O is dissolved in 20 mL absolute ethyl alcohols, and 10 min are stirred at 40 DEG C,
The solution clarified, 100 μ L concentration are added into obtained settled solution as 16mol/L nitric acid and are well mixed, so
Afterwards, mixed liquor is transferred in 40 mL Teflon inner liner stainless steel kettles, 2 h is heated at 200 DEG C；Treat that temperature is down to room temperature
Afterwards, sample is taken out, with 10000 r/min centrifugation, and is washed with distilled water and absolute ethyl alcohol, finally in vacuum environment
In, and in room temperature（18~22℃）Lower drying, obtain the flower-shaped nickel base nanometer material of the present invention.
Embodiment 2：By 0.1 g NiCl220 mL absolute ethyl alcohols are dissolved in, 10 min are stirred at 40 DEG C to promote to dissolve,
The solution clarified, 100 μ L concentration are added into obtained settled solution as 16mol/L nitric acid and are well mixed, then
Mixed liquor is transferred in 40 mL Teflon inner liner stainless steel kettles, 2 h are heated at 200 DEG C；Subsequent operation and the phase of method 1
Together, the flower-shaped nickel base nanometer material of the present invention is finally given.
Fig. 1 is the structure chart of the flower-shaped nickel base nanometer material prepared under Electronic Speculum using the above method.
Embodiment 3
By 0.1 g C2H6NiO4•4H2O is dissolved in 20 mL absolute ethyl alcohols, and 15 min are stirred at 30 DEG C, are clarified
Solution, added into obtained settled solution 100 μ L concentration be 16mol/L nitric acid and be well mixed, then, will mix
Liquid is transferred in 40 mL Teflon inner liner stainless steel kettles, and 3 h are heated at 150 DEG C；After temperature is down to room temperature, sample is taken out
Product, with 8000 r/min centrifugation, and washed with distilled water and absolute ethyl alcohol, finally in vacuum environment, and in room
Temperature（18~22℃）Lower drying, obtain the flower-shaped nickel base nanometer material of the present invention.
Embodiment 4
By 0.1 g C2H6NiO4•4H2O is dissolved in 20 mL absolute ethyl alcohols, and 5 min are stirred at 50 DEG C, are clarified
Solution, 100 μ L concentration are added into obtained settled solution as 16mol/L nitric acid and are well mixed, then, by mixed liquor
It is transferred in 40 mL Teflon inner liner stainless steel kettles, 2 h is heated at 250 DEG C；After temperature is down to room temperature, sample is taken out
Product, with 12000 r/min centrifugation, and washed with distilled water and absolute ethyl alcohol, finally in vacuum environment, and in room
Temperature（18~22℃）Lower drying, obtain the flower-shaped nickel base nanometer material of the present invention.
Embodiment 5
Select methyl orange（MO）It is flower-shaped Ni-based by being prepared using above-described embodiment 1 as the representative of organic dye molecule
The mg of nano material 10 is dispersed in the methyl orange solution that 4 mL concentration are 20 mg/l, pH 7, is stirred respectively at room temperature
10th, 20,30 minutes.Adsorbent after absorption is centrifuged, the concentration after dyestuff is adsorbed by UV spectrophotometer measuring,
By detecting adsorption effect of the methyl orange in the front and rear change in concentration measure methyl orange dye of absorption.
Fig. 2 a are the adsorption effect figure of the present invention for methyl orange dye, flower-shaped Ni-based are received what is prepared using the above method
The rice mg of material 10 is dispersed in the methyl orange solution that 4 mL concentration are 20 mg/l, is stirred at room temperature 0 ~ 10 minute time,
The adsorbance of methyl orange dye is substantially increased, at room temperature mixing time after 10 minutes, to the adsorbance of methyl orange dye after
Continuous increase, at room temperature during mixing time 30 minutes, the adsorbance of methyl orange dye is continued to increase, reach preferable and stable
State.
Embodiment 6
It is 5 × 10 by concentration-5 Mol/L methyl oranges and concentration are 5 × 10-5 Mol/L rhodamine Bs are with 1:1 proportioning mixing,
4 mL mixed solutions are taken, add flower-shaped nickel base nanometer material 10 mg, pH 7 prepared using above-described embodiment 2, at room temperature
120min is stirred, with UV spectrophotometer measuring adsorption effect.Fig. 2 c are the present invention in methyl orange and rhodamine B mixed solution
In to the high-selectivity adsorption design sketch of methyl orange, the nm of wave band 400 ~ 500 is methyl orange, and 500 ~ 600nm of wave band is rhodamine B,
Find out from Fig. 2 c, selective absorption significant effect of the flower-shaped nickel base nanometer material prepared using the above method to methyl orange.
From Fig. 2 c it can also be seen that the flower-shaped nickel base nanometer material prepared using the above method reaches suction in 30min
Attached stable state, show that the flower-shaped nickel base nanometer material of the present invention can be with quick adsorption methyl orange dye.
Embodiment 7
In 298 K, the methyl using flower-shaped nickel base nanometer material prepared by the above method to initial concentration for 20 mg/L
Orange dyestuff is adsorbed, and the pH value of methyl orange dye is adjusted with 0.1 mol/L HCl or 0.1 mol/L NaOH solutions.Exist respectively
PH is 3,5,7 and 11, and initial concentration is in 20 mg/L methyl orange dye, adds and utilizes the flower-shaped Ni-based of above method preparation
Nano material, stirring, makes absorption reach stable state, with UV spectrophotometer measuring adsorption effect.Fig. 2 b are pH value to the present invention
Influence to methyl orange dye adsorption effect, when pH is raised to 5 from 3, the adsorbance increase to methyl orange dye is right when pH is 7
The adsorbance of methyl orange dye substantially increases, and when pH is 11, the adsorbance of methyl orange dye is continued to increase, reaches preferable and steady
Fixed state.
The present invention has quick significant adsorption effect for organic dyestuff methyl orange, can adsorb a large amount of first in the short time rapidly
Base orange dyestuff, it can be seen that in the basic conditions, the present invention for methyl orange adsorption effect it is further preferred that, when pH value be 11 when, first
Base orange is almost adsorbed completely；In addition, the present invention can also be adsorbed from fast and stable in the mixed solution of methyl orange and rhodamine B
Methyl orange, there is efficient adsorption selectivity.
The present invention relates to applied to environmental science, can be directed to for the organic dyestuff methyl orange contained in trade effluent
Property carry out high selectivity quick adsorption, can as dye wastewater processing a kind of new way, provided for vast sewage treatment plant
It is a kind of it is highly efficient, cheap, be easily-synthesized to organic dyestuff methyl orange high-selectivity adsorption method, help to improve water quality, pole
The earth improves the security of resident living water and drinking water.
Claims (1)
1. a kind of synthetic method of the flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation, it is characterised in that specific
Follow the steps below：
Substance A is dissolved in absolute ethyl alcohol, concentration 0.005g/mL, stirred, the solution clarified, to obtained clarification
The nitric acid that concentration is 16mol/L is added in solution and is well mixed, A ethanol solution and the volume ratio of nitric acid are 200：1, will be mixed
Close liquid to be transferred in inner liner stainless steel kettle, mixed liquor heats 2~3h in 150~250 DEG C, after temperature is down to room temperature, takes out sample
Product, centrifugation, and washed with distilled water and absolute ethyl alcohol, finally dry, produce in vacuum environment, at room temperature；The substance A is
C2H6NiO4·4H2O or NiCl2In one kind；
The whipping temp is 30~50 DEG C, and the time is 5~15min；
The centrifugal rotational speed is 8000~12000r/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510769009.3A CN105251434B (en) | 2015-11-12 | 2015-11-12 | The synthetic method of the flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation |
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| CN201510769009.3A CN105251434B (en) | 2015-11-12 | 2015-11-12 | The synthetic method of the flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation |
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| CN105251434A CN105251434A (en) | 2016-01-20 |
| CN105251434B true CN105251434B (en) | 2018-01-16 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080280751A1 (en) * | 2007-03-16 | 2008-11-13 | Honda Motor Co., Ltd. | Method of preparing carbon nanotube containing electrodes |
| CN102218321A (en) * | 2011-05-06 | 2011-10-19 | 重庆理工大学 | Method for preparing heterogeneous phase Fenton catalyst used for methyl orange wastewater treatment |
| CN102674484A (en) * | 2012-05-29 | 2012-09-19 | 南京工业大学 | Preparation method of flower-like alpha-nickel hydroxide |
-
2015
- 2015-11-12 CN CN201510769009.3A patent/CN105251434B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080280751A1 (en) * | 2007-03-16 | 2008-11-13 | Honda Motor Co., Ltd. | Method of preparing carbon nanotube containing electrodes |
| CN102218321A (en) * | 2011-05-06 | 2011-10-19 | 重庆理工大学 | Method for preparing heterogeneous phase Fenton catalyst used for methyl orange wastewater treatment |
| CN102674484A (en) * | 2012-05-29 | 2012-09-19 | 南京工业大学 | Preparation method of flower-like alpha-nickel hydroxide |
Non-Patent Citations (4)
| Title |
|---|
| Combustion Synthesis of a Nickel Supported Catalyst: Effect of Metal Distribution on the Activity during Ethanol Decomposition;Allison Cross等;《Industrial & Engineering Chemistry Research》;20120827;第51卷;全文 * |
| Hydrothermal synthesis of nickel hydroxide nanostructures in mixed solvents of water and alcohol;Li-Xia Yang等;《Journal of solid state chemistry》;20070518;第180卷;全文 * |
| Ni-TiO2介孔材料的低热固相合成及其光降解甲基橙的动力学;刘少友等;《无机材料学报》;20090930;第24卷(第5期);全文 * |
| The location of nickel oxide and nickle in silica-supported catalyst:two forms of "NiO" and the assignment of temperature-programmed reduction profiles;BRYNMOR MILE等;《JOURNAL OF CATALYSIS》;19881231;第114卷;全文 * |
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