CN101633733B - Conductive polyaniline humic acid complex, preparation method thereof and application of mercury ion in adsorbed water body - Google Patents
Conductive polyaniline humic acid complex, preparation method thereof and application of mercury ion in adsorbed water body Download PDFInfo
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- CN101633733B CN101633733B CN2009100341109A CN200910034110A CN101633733B CN 101633733 B CN101633733 B CN 101633733B CN 2009100341109 A CN2009100341109 A CN 2009100341109A CN 200910034110 A CN200910034110 A CN 200910034110A CN 101633733 B CN101633733 B CN 101633733B
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- Prior art keywords
- humic acid
- hydrochloric acid
- conductive polyaniline
- reaction soln
- ammonium persulphate
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- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000004021 humic acid Substances 0.000 title claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 24
- BQPIGGFYSBELGY-UHFFFAOYSA-N mercury(2+) Chemical compound [Hg+2] BQPIGGFYSBELGY-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 50
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000004160 Ammonium persulphate Substances 0.000 claims abstract description 19
- 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 19
- 235000019395 ammonium persulphate Nutrition 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000000178 monomer Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 239000002351 wastewater Substances 0.000 abstract description 9
- 229910052753 mercury Inorganic materials 0.000 abstract description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract 2
- 238000006116 polymerization reaction Methods 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- -1 mercury ions Chemical class 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 6
- 229920001940 conductive polymer Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- BGARROUSYWXSED-UHFFFAOYSA-N dimercury(2+) Chemical compound [Hg+][Hg+] BGARROUSYWXSED-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002653 magnetic therapy Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
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- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a conductive polyaniline humic acid complex, a preparation method thereof and an application of mercury ion in an adsorbed water body and the preparation method comprises the following steps: adding a certain amount of humic acid into aniline and hydrochloric acid monomer solution; stirring by magnetic force; adding a moderate amount of oxidizing agent ammonium persulphate to realize polymerization; washing and filtering after polymerization until the filter liquor is colorless; drying to obtain the nano complex as shown in a scanning electron microscope picture; adding a moderate amount of the complex into mercury-contained simulated waste water in room temperature; oscillating for 24 hours; filtering; measuring the concentration of mercury by atomic fluorescence after the filter liquor is diluted. Results prove that the conductive polyaniline humic acid complex has superior adsorption property on mercury ions under extensive pH conditions.
Description
Technical field:
The present invention relates to a kind of conductive polymers, particularly a kind of conductive polymers humic acid complex and preparation method thereof the invention still further relates to the application of this mixture in the adsorbed water body mercury ion.
Background technology:
Along with economic sustained and rapid development, the mercury-containing waste water that is discharged in the environment is increasing, and not only serious environment pollution has also caused grave danger and restriction to the Sustainable development of the whole society.Heavy metal Hg enters behind the environment can not be by biological degradation, and participates in the food chain circulation, and finally accumulation in vivo destroys the metabolism of organism normal physiological, causes many environmental problems thus.People are always in novel material and the new technology of constantly making great efforts to seek to handle heavy metal contamination.Conducting polymer nano material has performances such as special light, electricity, magnetic, and its wide material sources, structure is various and inexpensive, has received increasing concern.Various fields such as store battery, transmitter, magnetic therapy medicine have been applied at present.In conductive polymers, polyaniline and derivative thereof are the most attractive, contain the nitrogen-atoms than multipotency and heavy metal complexing in its structure, make it be expected to become the novel environmental sorbing material.But its aqueous stability and activity etc. all are limited by water body pH environment.
Summary of the invention:
Technical problem to be solved by this invention provides the conductive polyaniline humic acid complex of the scalable water body pH of a kind of energy environment, and its preparation method reaches the application of mercury ion in adsorbed water body.
Conductive polyaniline humic acid complex of the present invention is to be prepared from by following method:
1) with humic acid with appropriate amount of deionized water scattered after, add aniline and hydrochloric acid and stir and be settled to 250mL and make reaction soln, the humic acid quality in the reaction soln is 0.05～2.0g, the aniline volume is 1.5～6.0mL, the hydrochloric acid volume is 2.0～9.5mL;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in ammonium persulphate and the reaction soln is 1～2: 1;
3) hydrochloric acid soln of ammonium persulphate is slowly joined in the reaction soln after the abundant stirring, magnetic agitation was reacted 5～12 hours;
4) products therefrom is colourless with deionized water wash, suction filtration until filtrate;
5) with above-mentioned steps 4) solid matter that obtains dries in 50～95 ℃ of vacuum, obtains conductive polyaniline humic acid complex.
In addition, the present invention also provides the application of this conductive polyaniline humic acid complex in the adsorbed water body mercury ion.
The scalable water body pH environment of conductive polyaniline humic acid complex energy of the present invention utilizes nano-conductive polyaniline adsorbed water body mercury ion, and utilizes the compound humic acid to improve the aqueous stability and the activity of polyaniline.This method efficient economy is applicable to the processing of a large amount of mercury-containing waste waters.
Description of drawings:
Fig. 1 is the transmission electron microscope shape appearance figure of the conductive copolymer humic acid complex that the present invention relates to.
Fig. 2 is the aqueous solution pH that the present invention relates to influence to conductive copolymer humic acid complex adsorbed water body mercury ion.
Specific embodiment:
1, the preparation method of conductive polyaniline humic acid complex
Embodiment 1:
1) with humic acid with appropriate amount of deionized water scattered after, add aniline and hydrochloric acid and stir and be settled to 250mL, making humic acid quality wherein is 0.05g, the aniline volume is 1.5mL, the hydrochloric acid volume is 3.0mL;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate and step 1) obtain is 1: 1;
3) hydrochloric acid soln of ammonium persulphate is slowly joined in the reaction soln after the abundant stirring, magnetic agitation was reacted 10 hours;
4) products therefrom is colourless with deionized water wash, suction filtration until filtrate;
5) with above-mentioned steps 4) solid matter that obtains dries in 65 ℃ of vacuum, obtains conductive polyaniline humic acid complex.
Embodiment 2:
1) with humic acid with appropriate amount of deionized water scattered after, add aniline and hydrochloric acid and stir and be settled to 250mL, making humic acid quality wherein is 0.5g, the aniline volume is 3.7mL, the hydrochloric acid volume is 7.0mL;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate and step 1) obtain is 2: 1;
3) hydrochloric acid soln of ammonium persulphate is slowly joined in the reaction soln after the abundant stirring, magnetic agitation was reacted 7 hours;
4) products therefrom is colourless with deionized water wash, suction filtration until filtrate;
5) with above-mentioned steps 4) solid matter that obtains dries in 80 ℃ of vacuum, obtains conductive polyaniline humic acid complex.Its shape appearance figure as shown in Figure 1.
Fig. 1 is the sem photograph of conductive polyaniline humic acid complex.As can be seen from the figure: the particle of this mixture presents sphere, and mean diameter is 50～60nm.
1) with humic acid with appropriate amount of deionized water scattered after, add aniline and hydrochloric acid and stir and be settled to 250mL, making humic acid quality wherein is 2.0g, the aniline volume is 6.0mL, the hydrochloric acid volume is 9.5mL;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in the solution that ammonium persulphate and step 1) obtain is 1.5: 1;
3) hydrochloric acid soln of ammonium persulphate is slowly joined in the reaction soln after the abundant stirring, magnetic agitation was reacted 12 hours;
4) products therefrom is colourless with deionized water wash, suction filtration until filtrate;
5) with above-mentioned steps 4) solid matter that obtains dries in 95 ℃ of vacuum, obtains conductive polyaniline humic acid complex.
2, conductive polyaniline humic acid complex adsorbed water body mercury ion
Embodiment 4:
A) conductive polyaniline humic acid complex is joined contain in the mercury ion simulated wastewater, making the quality of mixture is 20mg, contains the concentration (C of mercury ion simulated wastewater
0) be 20mg L
-1, the pH of waste water is 3;
B) with above-mentioned steps a) gained contain mixture and contain mercury ion simulated wastewater 40mL and join in the Glass Containers, sealing;
C) with above-mentioned steps b) in Glass Containers put into the shaking culture case, vibrated 24 hours, controlled temperature is 25 ℃;
D) after vibration finishes, extract the mercurous ion waste water of 10mL, filter;
E) get the 2mL clear liquid, dilution is measured ion concentration of mercury (Ce) with atomic fluorescence method.
F) calculate adsorption efficiency, removal%=100% (C
0-Ce)/C
0
Fig. 2 is 25 ℃, 20mg mixture sorbent material, C
0=20mg L
-1Contain mercury ion simulated wastewater adsorption effect figure under condition of different pH.As can be seen from Figure 2: in the broad pH scope of pH 4.3～7.5, with the efficient of this mixture adsorbents adsorb mercury ion all about 95%.
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. conductive polyaniline humic acid complex is characterized in that it being to be prepared from by following method:
1) with humic acid with appropriate amount of deionized water scattered after, add aniline and hydrochloric acid and stir and be settled to 250mL and make reaction soln, the humic acid quality in the reaction soln is 0.05～2.0g, the aniline volume is 1.5～6.0mL, the hydrochloric acid volume is 2.0～9.5mL;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in ammonium persulphate and the reaction soln is 1～2: 1;
3) hydrochloric acid soln of ammonium persulphate is slowly joined in the reaction soln after the abundant stirring, magnetic agitation was reacted 5～12 hours;
4) products therefrom is colourless with deionized water wash, suction filtration until filtrate;
5) with above-mentioned steps 4) solid matter that obtains dries in 50～95 ℃ of vacuum, obtains conductive polyaniline humic acid complex.
2. the preparation method of a conductive polyaniline humic acid complex is characterized in that may further comprise the steps:
1) with humic acid with appropriate amount of deionized water scattered after, add aniline and hydrochloric acid and stir and be settled to 250mL and make reaction soln, the humic acid quality in the reaction soln is 0.05～2.0g, the aniline volume is 1.5～6.0mL, the hydrochloric acid volume is 2.0～9.5mL;
2) ammonium persulphate and hydrochloric acid are made into the aqueous solution, making the aniline monomer mol ratio in ammonium persulphate and the reaction soln is 1～2: 1;
3) hydrochloric acid soln of ammonium persulphate is slowly joined in the reaction soln after the abundant stirring, magnetic agitation was reacted 5～12 hours;
4) products therefrom is colourless with deionized water wash, suction filtration until filtrate;
5) with above-mentioned steps 4) solid matter that obtains dries in 50～95 ℃ of vacuum, obtains conductive polyaniline humic acid complex.
3. the application of the described conductive polyaniline humic acid complex of claim 1 in the adsorbed water body mercury ion.
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| CN101633733B true CN101633733B (en) | 2011-09-07 |
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| CN101928048B (en) * | 2010-08-27 | 2012-05-09 | 陕西科技大学 | Method for purifying humic acid pollutants in water by utilizing polyaniline |
| CN107556474A (en) * | 2017-09-30 | 2018-01-09 | 江苏瑞腾涂装科技有限公司 | A kind of high-specific surface area polyaniline and preparation method thereof |
| CN109865503A (en) * | 2019-03-20 | 2019-06-11 | 安徽工业大学 | A kind of magnetic conductive polymer/sepiolite/humic acid complex microsphere preparation and its application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041124A (en) * | 2007-04-28 | 2007-09-26 | 同济大学 | Diaminobenzenesulfonate polymerization modification polymer materials -PAN Hg ion sorbent and the preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101041124A (en) * | 2007-04-28 | 2007-09-26 | 同济大学 | Diaminobenzenesulfonate polymerization modification polymer materials -PAN Hg ion sorbent and the preparing method |
Non-Patent Citations (2)
| Title |
|---|
| 李新贵,窦强,黄美荣.共聚苯胺吸附剂对含汞废水的处理.《南方水产》.2007,第3卷(第6期),8-13. * |
| 雷志芳,叶常明.苯胺在水体悬浮颗粒物上吸附特征.《环境科学》.1998,70-72. * |
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