CN103342813A - Preparation method of polyaniline /attapulgite/zero valent iron composite material - Google Patents
Preparation method of polyaniline /attapulgite/zero valent iron composite material Download PDFInfo
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- CN103342813A CN103342813A CN2013102840362A CN201310284036A CN103342813A CN 103342813 A CN103342813 A CN 103342813A CN 2013102840362 A CN2013102840362 A CN 2013102840362A CN 201310284036 A CN201310284036 A CN 201310284036A CN 103342813 A CN103342813 A CN 103342813A
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- attapulgite
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- polyaniline
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- valent iron
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Abstract
The invention provides a preparation method of a polyaniline /attapulgite/zero valent iron composite material. The preparation method is aimed at solving the problems that iron powder granules are liable to aggregate and the surfaces are liable to passivate. The preparation method comprises the following steps: (1) adding 0.1-0.5 mol/L acid into a reaction container, wherein the mol ratio of the acid of the reaction solution is 0.1-0.5 mol/L; (2) adding the attapulgite clay to prepare a suspended solution; (3) adding aniline, and stirring to disperse the aniline; (4) adding ammonium persulfate to serve as an initiator, standing and polymerizing to form a viscous solution so as to disperse zero valent iron granules; and (5) carrying out suction filtering and drying to obtain the product.
Description
Technical field
The invention belongs to environmental protection sorbing material field, be specifically related to the preparation method of the polyaniline/Attapulgite/Zero-valent Iron matrix material for water treatment.
Background technology
Polyaniline (PANI) has linear polymer chain and contains a large amount of amino and imino-, and heavy metal ion is had good complexing action.Amino and imino-also has reductibility, can carry out redox reaction with the heavy metal ion of some high oxidation potentials, the polyaniline compound sorbent material has ion exchanging function to the part metals ion simultaneously, therefore polyaniline can be used as a kind of novel heavy metal capturing agent, but cost is higher when using as sorbent material.Attapulgite clay (ATP) claim polygorskite or Palygorskite again, be a kind of tool chain laminate structure contain Shuifu County's magnesium silicate clay mineral.Unique crystalline structure makes attapulgite clay have good dispersing property under the effect of shearing force, be widely used in aspects such as coating, drilling well and slowly-releasing as thickening material, thixotropic agent, suspension stabilizer, have wider range of application and tangible cost advantage, and environmentally safe, but with pure attapulgite during as sorbent material its adsorptive power limited.
The Zero-valent Iron low price has high reduction potential and fast response characteristic, and Zero-valent Iron can be reduced chlorinated hydrocarbon, NO
3-, pollutent such as Cr (VI), perchlorate, uranium.Zero-valent Iron has been widely used in and has removed Cr (VI) polluted-water in the permeability response wall in recent years, but nulvalent iron particle surface oxidation and be easy to reunite easily, therefore solving ferrous powder granules reunites particularly important in actual applications with the problem of surperficial passivation easily easily, be necessary further to study the method that particle disperses, improve reaction efficiency.
Summary of the invention
The objective of the invention isSolving ferrous powder granules reunites and the surperficial problem of passivation easily easily.
The preparation method of polyaniline/Attapulgite/Zero-valent Iron matrix material the steps include:
(1) attapulgite is added in the acid solution of 0.1-0.5mol/L, carry out dispersed with stirring 0.5h;
(2) aniline of adding attapulgite quality 5%-35% stirs 0.5h;
(3) ammonium persulphate that adds attapulgite quality 15～25% leaves standstill 0.5h as initiator after the stirring;
(4) iron powder of adding attapulgite quality 25-100%, dispersed with stirring 0.5h;
(5) suction filtration is to neutral, and 60 ℃ of oven dry are ground, and obtain matrix material.
Usefulness of the present invention is:
1. improve iron powder as the application of a kind of reductibility treatment agent in handling pollution, can handle the pollutent of high density.Sexavalent chrome solution absorbs capacity to 100mg/L can reach more than the 70mg/g, and treatment effect is good.
The ferrous powder granules surface coverage polyaniline, can avoid the iron powder surface passivation and reduce processing efficiency.
3. the ferrous powder granules in the matrix material is uniformly dispersed, and has improved the utilization ratio of ferrous powder granules.
4. iron powder and attapulgite are cheap in the matrix material obtains easily, and polyaniline proportion in matrix material is lower, causes its cost lower.
5. before iron powder ran out of, treatment effect existed always, had the long-term disposal effect.
Description of drawings
Fig. 1 is the electron-microscope scanning picture of case study on implementation 1, and Fig. 2 is the isothermal adsorption figure of matrix material absorption Cr of the present invention (VI).
Embodiment
The preparation method of polyaniline/Attapulgite/Zero-valent Iron matrix material the steps include:
(1) attapulgite is added in the acid solution of 0.1-0.5mol/L, carry out dispersed with stirring 0.5h;
(2) aniline of adding attapulgite quality 5%-35% stirs 0.5h;
(3) ammonium persulphate that adds attapulgite quality 15～25% leaves standstill 0.5h as initiator after the stirring;
(4) iron powder of adding attapulgite quality 25-100%, dispersed with stirring 0.5h;
(5) suction filtration is to neutral, and 60 ℃ of oven dry are ground, and obtain matrix material.
The mass percent of attapulgite, iron powder, aniline is: attapulgite 25～50%, iron powder 25 ~ 50%, aniline 5～11%.
More thanUsed attapulgite is pure soil; Attapulgite is configured to 0.01～0.03% aaerosol solution; The ferrous powder granules size is 200 ~ 350 orders; Used acid is hydrochloric acid, perhaps nitric acid, perhaps sulfuric acid, perhaps above-mentioned various mixture; Preparation temperature is at the 0-25 degree.
The present invention utilizes Attapulgite and polyaniline suspension polymerization, forms full-bodied mixing solutions, add nulvalent iron particle it is mixed, and has solved the problem that ferrous powder granules precipitates reunion easily.Common zero-valent iron particle is in water, and the surface can form Fe
3O
4And Fe
2O
3Cause passivation.The present invention utilizes the preservative property of polyaniline and electroconductibility to deal with problems, the Fe of iron particle surface
3O
4And Fe
2O
3Replaced by polyaniline, prevent its passivation.Zhi Bei matrix material has the favorable conductive rate at low temperatures, and electronics shifts the reduction that helps pollutent on the ferrous powder granules surface, and the matrix material under the low temperature preparation has higher removal effect.Polyaniline can prevent the nulvalent iron particle surface passivation as a kind of novel conductive layer, helps electronics in the transfer on its surface, has improved the removal performance of Zero-valent Iron to pollutent.
Further launch the present invention with embodiment more specifically below.
Embodiment 1: preparation temperature is 0 ℃, takes by weighing the 2.0g attapulgite, adds 0.5mol/L nitric acid 77mL and stirs 0.5h, adds 0.6mL aniline and stirs 0.5h, adds the 2.0g ammonium persulphate, leaves standstill 0.5h after the stirring.Add 350 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 ℃ of oven dry are ground, and obtain blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material reaches 75.13mg/g to the loading capacity of Cr (VI) when pH=3.As shown in Figure 1, be the electron-microscope scanning picture of the product that makes.
Embodiment 2: preparation temperature is 0 ℃, takes by weighing the 2.0g attapulgite, adds 0.5mol/L nitric acid 77mL and stirs 0.5h, adds 0.5mL aniline and stirs 0.5h, adds the 2.0g ammonium persulphate, leaves standstill 0.5h after the stirring.Add 320 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 ℃ of oven dry are ground, and obtain blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material reaches 71.37mg/g to the loading capacity of Cr (VI) when pH=3.
Embodiment 3: preparation temperature is 0 ℃, takes by weighing the 2.0g attapulgite, adds 0.4mol/L nitric acid 77mL and stirs 0.5h, adds 0.5mL aniline and stirs 0.5h, adds the 2.0g ammonium persulphate, leaves standstill 0.5h after the stirring.Add 320 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 ℃ of oven dry are ground, and obtain blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material reaches 62.91mg/g to the loading capacity of Cr (VI) when pH=3.
Embodiment 4: preparation temperature is 17 ℃, takes by weighing the 2.0g attapulgite, adds 0.4mol/L nitric acid 77mL and stirs 0.5h, adds 0.5mL aniline and stirs 0.5h, adds the 1.0g ammonium persulphate, leaves standstill 0.5h after the stirring.Add 320 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 ℃ of oven dry are ground, and obtain blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material reaches 53.17mg/g to the loading capacity of Cr (VI) when pH=3.
Embodiment 5: preparation temperature is 25 ℃, takes by weighing the 2.0g attapulgite, adds 0.5mol/L nitric acid 77mL and stirs 0.5h, adds 0.4mL aniline and stirs 0.5h, adds the 1.0g ammonium persulphate, leaves standstill 0.5h after the stirring.Add 200 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 ℃ of oven dry are ground, and obtain blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material reaches 38.22mg/g to the loading capacity of Cr (VI) when pH=3.
Above-described embodiment is preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other are any not to deviate from change, modification, combination, the simplification of making under spirit of the present invention and the principle; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. the preparation method of polyaniline/Attapulgite/Zero-valent Iron matrix material the steps include:
(1) attapulgite is added in the acid solution of 0.1-0.5mol/L, carry out dispersed with stirring 0.5h;
(2) aniline of adding attapulgite quality 5%-35% stirs 0.5h;
(3) ammonium persulphate that adds attapulgite quality 15～25% leaves standstill 0.5h as initiator after the stirring;
(4) iron powder of adding attapulgite quality 25-100%, dispersed with stirring 0.5h;
(5) suction filtration is to neutral, and 60 ℃ of oven dry are ground, and obtain matrix material.
2. the preparation method of polyaniline/Attapulgite according to claim 1/Zero-valent Iron matrix material is characterized in that, the mass percent of attapulgite, iron powder, aniline is: attapulgite 25～50%, iron powder 25 ~ 50%, aniline 5～11%.
3. the preparation method of polyaniline/Attapulgite according to claim 1/Zero-valent Iron matrix material is characterized in that, used attapulgite is pure soil.
4. the preparation method of polyaniline/Attapulgite according to claim 1/Zero-valent Iron matrix material is characterized in that, attapulgite is configured to 0.01～0.03% aaerosol solution.
5. the preparation method of polyaniline/Attapulgite according to claim 1/Zero-valent Iron matrix material is characterized in that, the ferrous powder granules size is 200 ~ 350 orders.
6. the preparation method of polyaniline/Attapulgite according to claim 1/Zero-valent Iron matrix material is characterized in that, used acid is hydrochloric acid, perhaps nitric acid, perhaps sulfuric acid, perhaps above-mentioned various mixture.
7. the preparation method of polyaniline/Attapulgite according to claim 1/Zero-valent Iron matrix material is characterized in that, preparation temperature is at the 0-25 degree.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588988A (en) * | 2013-11-18 | 2014-02-19 | 兰州理工大学 | Preparation method of porous nano polymer composite material |
| CN104232251A (en) * | 2014-08-28 | 2014-12-24 | 陕西师范大学 | Polyaniline composite electrorheological fluid |
| CN104310566A (en) * | 2014-11-03 | 2015-01-28 | 济南大学 | Organic wastewater treatment method based on polyaniline coated nanometer zero-valent iron |
| CN104402107A (en) * | 2014-12-02 | 2015-03-11 | 济南大学 | Method for treating organic wastewater based on polyaniline loaded nanoscale zero-valent iron |
| CN105175719A (en) * | 2015-06-29 | 2015-12-23 | 江苏艾科勒科技有限公司 | Preparation method of nanometer iron-polyaniline porous material having performances of adsorption and reduction |
| CN109433167A (en) * | 2018-11-30 | 2019-03-08 | 兰州理工大学 | A kind of polypyrrole-nano zero valence iron composite material and preparation method and application |
| CN112408527A (en) * | 2020-10-21 | 2021-02-26 | 西安交通大学 | Method for heating and cooling monatomic fluid to cooperatively treat wastewater |
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| CN102350322A (en) * | 2011-07-21 | 2012-02-15 | 陕西科技大学 | Method for removing hexavalent chromium from water by using polyaniline-modified palygouskite |
| CN102755883A (en) * | 2012-06-26 | 2012-10-31 | 南京大学 | Preparation method of attapulgite-loaded nanometre iron material |
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2013
- 2013-07-08 CN CN201310284036.2A patent/CN103342813B/en not_active Expired - Fee Related
Patent Citations (3)
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| WO1999025778A1 (en) * | 1997-11-14 | 1999-05-27 | Zipperling Kessler & Co. (Gmbh & Co.) | Synthesis and applications of intrinsically conductive polymer salts of polyphosphonic acids in anti-corrosion coatings |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588988A (en) * | 2013-11-18 | 2014-02-19 | 兰州理工大学 | Preparation method of porous nano polymer composite material |
| CN103588988B (en) * | 2013-11-18 | 2015-04-08 | 兰州理工大学 | Preparation method of porous nano polymer composite material |
| CN104232251A (en) * | 2014-08-28 | 2014-12-24 | 陕西师范大学 | Polyaniline composite electrorheological fluid |
| CN104232251B (en) * | 2014-08-28 | 2016-08-17 | 陕西师范大学 | polyaniline composite electrorheological fluid |
| CN104310566A (en) * | 2014-11-03 | 2015-01-28 | 济南大学 | Organic wastewater treatment method based on polyaniline coated nanometer zero-valent iron |
| CN104310566B (en) * | 2014-11-03 | 2016-03-02 | 济南大学 | A kind of method based on polyaniline-coated type nano zero valence iron process organic waste water |
| CN104402107A (en) * | 2014-12-02 | 2015-03-11 | 济南大学 | Method for treating organic wastewater based on polyaniline loaded nanoscale zero-valent iron |
| CN105175719A (en) * | 2015-06-29 | 2015-12-23 | 江苏艾科勒科技有限公司 | Preparation method of nanometer iron-polyaniline porous material having performances of adsorption and reduction |
| CN109433167A (en) * | 2018-11-30 | 2019-03-08 | 兰州理工大学 | A kind of polypyrrole-nano zero valence iron composite material and preparation method and application |
| CN112408527A (en) * | 2020-10-21 | 2021-02-26 | 西安交通大学 | Method for heating and cooling monatomic fluid to cooperatively treat wastewater |
| CN112408527B (en) * | 2020-10-21 | 2021-09-07 | 西安交通大学 | Method for heating and cooling monatomic fluid to cooperatively treat wastewater |
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| CN103342813B (en) | 2015-06-17 |
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