CN101875721A - Aniline-o-aminophenol copolymer, preparation method thereof and application for removing mercury ions in water bodies - Google Patents
Aniline-o-aminophenol copolymer, preparation method thereof and application for removing mercury ions in water bodies Download PDFInfo
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- CN101875721A CN101875721A CN200910234580XA CN200910234580A CN101875721A CN 101875721 A CN101875721 A CN 101875721A CN 200910234580X A CN200910234580X A CN 200910234580XA CN 200910234580 A CN200910234580 A CN 200910234580A CN 101875721 A CN101875721 A CN 101875721A
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- Prior art keywords
- aniline
- aminophenol
- hydrochloric acid
- multipolymer
- ammonium persulphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052753 mercury Inorganic materials 0.000 title abstract description 21
- 229920001577 copolymer Polymers 0.000 title abstract description 8
- -1 mercury ions Chemical class 0.000 title abstract 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 62
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 claims abstract description 30
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000178 monomer Substances 0.000 claims abstract description 13
- 239000004160 Ammonium persulphate Substances 0.000 claims description 18
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- BQPIGGFYSBELGY-UHFFFAOYSA-N mercury(2+) Chemical compound [Hg+2] BQPIGGFYSBELGY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 18
- 239000002351 wastewater Substances 0.000 abstract description 13
- 238000001914 filtration Methods 0.000 abstract 2
- 238000006116 polymerization reaction Methods 0.000 abstract 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 238000001878 scanning electron micrograph Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000004088 simulation Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000002795 fluorescence method Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- QFAXIZQBSCGJMA-UHFFFAOYSA-N mercury;hydrate Chemical compound O.[Hg] QFAXIZQBSCGJMA-UHFFFAOYSA-N 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses an aniline-o-aminophenol copolymer, a preparation method thereof and an application for removing mercury ions in water bodies. The preparation method comprises the following steps: adding a proper amount of ammonium persulfate used as an oxidizer in aniline, hydrochloric acid and o-aminophenol monomer solution at room temperature for carrying out polymerization; washing after polymerization; filtering until the filtered solution is colorless; and drying to obtain the nano-copolymer shown in the scanning electron micrograph. The application comprises the following steps: adding a proper amount of the copolymer into simulated wastewater containing mercury, oscillating for 24 hours at room temperature, filtering, and then, measuring the concentration of the mercury in the diluted filtered solution by atomic fluorescence. The result shows that the copolymer has excellent performance of adsorbing mercury ions in water under wide pH conditions.
Description
Technical field
The present invention relates to a kind of multipolymer, particularly a kind of aniline-o-aminophenol multipolymer and chemical preparation process thereof the invention still further relates to the application that this multipolymer is removed mercury ion in the water in absorption.
Background technology
Along with expanding economy, the mercury consumption increases year by year, and the mercury contaminants that is discharged in the environment is also increasing, and mercury ion produces great harm to water ecological environment in the water body, simultaneously may pass through food chain enrichment in vivo, harmful to human central nervous system, Digestive tract and kidney etc.People are seeking the improvement method of mercury-containing waste water always for a long time, and wherein absorption method is because of easy and simple to handle more commonly used, but have that loading capacity is little, adsorption effect is not good or shortcoming such as water chemistry condition adaptability is not strong.Conductive polymers enjoys people to pay close attention to because of having aspect special performances such as light, electricity, magnetic, has been applied to fields such as store battery, transmitter, magnetotherapy appliance at present.Contain nitrogen-atoms in aniline-o-aminophenol copolymer structure than multipotency and heavy metal generation complexing action, and the o-aminophenol tool in the structure is educated the effect of buffer pH, its performance has certain adaptability to the pH of relative broad range, is expected to become novel heavy metal sorbing material.
Summary of the invention
Technical problem solved by the invention provides a kind of aniline-its chemical preparation process of o-aminophenol multipolymer that is adapted to the wide pH value scope, utilizes this multipolymer absorption to remove mercury ion in the water, and easy to operate, removal effect is good.
Aniline involved in the present invention-o-aminophenol multipolymer is to be prepared from by following chemical process:
1) aniline monomer and hydrochloric acid are dissolved in the deionized water, agitation condition adds o-aminophenol down, and wherein the mol ratio of aniline, hydrochloric acid and o-aminophenol is 60～80: 200～220: 1.1～1.5;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate, hydrochloric acid and step 1) obtain is 11～15: 200～220: 60～80;
3) ammonium persulphate and hydrochloric acid soln are slowly added above-mentioned steps 1) configuration reaction solution in, magnetic agitation was reacted 5～12 hours;
4) it is colourless until filtrate with deionized water wash, suction filtration to obtain reactant;
5) with above-mentioned steps 4) solid matter that obtains dries in vacuum drying oven under 60～90 ℃ of conditions, obtains aniline-o-aminophenol multipolymer.
In addition, the present invention also asks for protection the preparation method of aniline-o-aminophenol multipolymer and the application that reaches this multipolymer mercury ion in removing water.
The preparation method of aniline among the present invention-o-aminophenol multipolymer is simple, realizes that easily cost of material is cheap.Utilize the absorption of this multipolymer to remove in water mercury ion to have widely water body pH environmental compatibility, removal effect is good, and is and easy to operate, is applicable to the processing of a large amount of mercury-containing waste waters.
Description of drawings
Fig. 1 is the scanning electron microscope shape appearance figure of the aniline-o-aminophenol copolymer powder that the present invention relates to.
Fig. 2 is that the different pH that contain mercury solution that the present invention relates to adsorb the influence of removing mercury ion to aniline-o-aminophenol multipolymer.
Fig. 3 is that mercury ion is respectively I=0.2molL in ionic strength in the aniline-o-aminophenol multipolymer planar water that the present invention relates to
-1And I=1mol
-1LNaNO
3Langmuir adsorption isothermal line under the condition.
Specific embodiment
1, the chemical preparation process of aniline-o-aminophenol multipolymer
Embodiment 1:
1) aniline monomer and hydrochloric acid are dissolved in the deionized water, agitation condition adds o-aminophenol down, and wherein the mol ratio of aniline, hydrochloric acid and o-aminophenol is 60: 200: 1.1;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate, hydrochloric acid and step 1) obtain is 11: 200: 60;
3) ammonium persulphate and hydrochloric acid soln are slowly added above-mentioned steps 1) configuration reaction solution in, magnetic agitation was reacted 8 hours;
4) it is colourless until filtrate with deionized water wash, suction filtration to obtain reactant;
5) with above-mentioned steps 4) solid matter that obtains dries in vacuum drying oven under 70 ℃ of conditions, obtains aniline-o-aminophenol multipolymer.Its shape appearance figure as shown in Figure 1.
Fig. 1 is the sem photograph of aniline-o-aminophenol copolymer powder.As can be seen from the figure: the particle of this multipolymer presents sphere.
Embodiment 2:
1) aniline monomer and hydrochloric acid are dissolved in the deionized water, agitation condition adds o-aminophenol down, and wherein the mol ratio of aniline, hydrochloric acid and o-aminophenol is 70: 210: 1.3;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate, hydrochloric acid and step 1) obtain is 13: 210: 70;
3) ammonium persulphate and hydrochloric acid soln are slowly added above-mentioned steps 1) configuration reaction solution in, magnetic agitation was reacted 8 hours;
4) it is colourless until filtrate with deionized water wash, suction filtration to obtain reactant;
5) with above-mentioned steps 4) solid matter that obtains dries in vacuum drying oven under 70 ℃ of conditions, obtains aniline-o-aminophenol multipolymer.
Embodiment 3:
1) aniline monomer and hydrochloric acid are dissolved in the deionized water, agitation condition adds o-aminophenol down, and wherein the mol ratio of aniline, hydrochloric acid and o-aminophenol is 80: 220: 1.5;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate, hydrochloric acid and step 1) obtain is 15: 220: 80;
3) ammonium persulphate and hydrochloric acid soln are slowly added above-mentioned steps 1) configuration reaction solution in, magnetic agitation was reacted 8 hours;
4) it is colourless until filtrate with deionized water wash, suction filtration to obtain reactant;
5) with above-mentioned steps 4) solid matter that obtains dries in vacuum drying oven under 70 ℃ of conditions, obtains aniline-o-aminophenol multipolymer.
2, the method for mercury ion in aniline-o-aminophenol multipolymer adsorbed water body
Embodiment 4:
1) 20mg aniline-o-aminophenol multipolymer is joined 100mg L
-1The simulation mercury-containing waste water in, the pH of mercury-containing waste water is 2～12;
2) with above-mentioned steps 1) the simulation mercury-containing waste water 40mL that contains multipolymer that obtains joins in the Glass Containers sealing;
3) with above-mentioned steps 2) in Glass Containers place vibration culture oven, 25 ℃ of constant temperature vibration 24 hours;
4) after vibration finishes, extract the 10ml mercury-containing waste water and filter;
5) get 1ml above-mentioned steps 4) filtrate dilution, measure ion concentration of mercury (Ce) with atomic fluorescence method;
6) calculate multipolymer eliminating rate of absorption R,
Fig. 2 is 25 ℃, 20mg multipolymer sorbent material, C
0=100mgL
-1Contain of the influence of the condition of different pH of mercury ion simulated wastewater to adsorption effect.As can be seen from Figure 2: between pH 4.5～8.5 in the wide pH value scope, with the clearance of this multipolymer adsorbents adsorb mercury ion all about 95%.
Embodiment 5:
1) 10mg aniline-o-aminophenol multipolymer is joined 1～400mg L
-1The simulation mercury-containing waste water in, the pH of mercury-containing waste water is 5.5;
2) with above-mentioned steps 1) the simulation mercury-containing waste water 40mL that contains multipolymer that obtains joins in the Glass Containers sealing;
3) with above-mentioned steps 2) in Glass Containers place vibration culture oven, 25 ℃ of constant temperature vibration 24 hours;
4) after vibration finishes, extract the 10mL mercury-containing waste water and filter;
5) get 1ml above-mentioned steps 4) filtrate dilution, measure ion concentration of mercury (C with atomic fluorescence method
e);
6) calculate multipolymer loading capacity Q
e,
Fig. 3 is 25 ℃, 10mg multipolymer sorbent material, and the simulation mercury-containing waste water of different starting point concentrations, ionic strength is respectively 0.2molL
-1And 1molL
-1NaNO
3Langmuir adsorption isothermal line under the condition.This material is fine to the adsorption effect of mercury ion as can be seen, and loading capacity can reach 212.13mgg
-1
More than be thinking of the present invention and implementation method, concrete application approach is a lot, should be understood that; for those skilled in the art; under the prerequisite that does not break away from the principle of the invention, can also make some improvement, these improvement also should be considered as protection scope of the present invention.
Claims (3)
1. aniline-o-aminophenol multipolymer is characterized in that being prepared from by following method:
1) aniline monomer and hydrochloric acid are dissolved in the deionized water, agitation condition adds o-aminophenol down, and wherein the mol ratio of aniline, hydrochloric acid and o-aminophenol is 60～80: 200～220: 1.1～1.5;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate, hydrochloric acid and step 1) obtain is 11～15: 200～220: 60～80;
3) ammonium persulphate and hydrochloric acid soln are slowly added above-mentioned steps 1) preparation reaction solution in, magnetic agitation was reacted 5～12 hours;
4) reactant that obtains is colourless until filtrate with deionized water wash, suction filtration;
5) with above-mentioned steps 4) solid matter that obtains dries in vacuum drying oven under 60～90 ℃ of conditions, obtains aniline-o-aminophenol multipolymer.
2. the preparation method of aniline-o-aminophenol multipolymer is characterized in that may further comprise the steps:
1) aniline monomer and hydrochloric acid are dissolved in the deionized water, agitation condition adds o-aminophenol down, and wherein the mol ratio of aniline, hydrochloric acid and o-aminophenol is 60～80: 200～220: 1.1～1.5;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate, hydrochloric acid and step 1) obtain is 11～15: 200～220: 60～80;
3) ammonium persulphate and hydrochloric acid soln are slowly added above-mentioned steps 1) preparation reaction solution in, magnetic agitation was reacted 5～12 hours;
4) reactant that obtains is colourless until filtrate with deionized water wash, suction filtration;
5) with above-mentioned steps 4) solid matter that obtains dries in vacuum drying oven under 60～90 ℃ of conditions, obtains aniline-o-aminophenol multipolymer.
3. the application of the described aniline of claim 1-o-aminophenol multipolymer mercury ion in removing water body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910234580XA CN101875721A (en) | 2009-11-23 | 2009-11-23 | Aniline-o-aminophenol copolymer, preparation method thereof and application for removing mercury ions in water bodies |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910234580XA CN101875721A (en) | 2009-11-23 | 2009-11-23 | Aniline-o-aminophenol copolymer, preparation method thereof and application for removing mercury ions in water bodies |
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| CN101875721A true CN101875721A (en) | 2010-11-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104801287A (en) * | 2015-04-03 | 2015-07-29 | 齐鲁工业大学 | Method for preparing phenol amine copolymer capable of capturing heavy metal ions by utilizing ethylidene amines |
-
2009
- 2009-11-23 CN CN200910234580XA patent/CN101875721A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104801287A (en) * | 2015-04-03 | 2015-07-29 | 齐鲁工业大学 | Method for preparing phenol amine copolymer capable of capturing heavy metal ions by utilizing ethylidene amines |
| CN104801287B (en) * | 2015-04-03 | 2017-07-28 | 齐鲁工业大学 | A kind of ethylene-amines can catch the preparation method of heavy metal ion phenol amine copolymer thing |
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Open date: 20101103 |