CN103342813B - 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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- CN103342813B CN103342813B CN201310284036.2A CN201310284036A CN103342813B CN 103342813 B CN103342813 B CN 103342813B CN 201310284036 A CN201310284036 A CN 201310284036A CN 103342813 B CN103342813 B CN 103342813B
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- attapulgite
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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 adsorption Material Field, be specifically related to the preparation method of the polyaniline /attapulgite/zero valent iron composite 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 has good complexing action.Amino and imino-also has reductibility, redox reaction can be carried out with the heavy metal ion of some high oxidation potentials, polyaniline compound sorbent material has ion exchanging function to part metals ion simultaneously, therefore polyaniline can be used as a kind of novel heavy metal capturing agent, but when applying as sorbent material, cost is higher.Attapulgite clay (ATP) also known as polygorskite or Palygorskite, be a kind of tool chain laminate structure containing Shuifu County's magnesium silicate clay mineral.Unique crystalline structure makes attapulgite clay have good dispersing property under the effect of shearing force, the aspects such as coating, drilling well and slowly-releasing are widely used in as thickening material, thixotropic agent, suspension stabilizer, there is wider range of application and obvious cost advantage, and environmentally safe, but with pure attapulgite as its limited sorption capacity during sorbent material.
Zero-valent Iron low price has high reduction potential and fast response characteristic, and Zero-valent Iron can reduce chlorinated hydrocarbon, NO
3-, Cr (VI), perchlorate, the pollutent such as uranium.Zero-valent Iron has been widely used in permeable coefficient tensor and has removed Cr (VI) polluted-water in recent years, but nulvalent iron particle surface is easily oxidized and is easy to reunite, therefore solving ferrous powder granules easily reunites particularly important in actual applications with the problem of the easy passivation in surface, be necessary the method studying particle dispersion further, improve reaction efficiency.
Summary of the invention
the object of the invention issolve ferrous powder granules easily to reunite and the problem of the easy passivation in surface.
The preparation method of polyaniline /attapulgite/zero valent iron composite 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) add the aniline of attapulgite quality 5%-35%, stir 0.5h;
(3) add the ammonium persulphate of attapulgite quality 15 ~ 25% as initiator, after stirring, leave standstill 0.5h;
(4) iron powder of attapulgite quality 25-100% is added, dispersed with stirring 0.5h;
(5) suction filtration is to neutral, 60 DEG C of oven dry, and grinding, obtains matrix material.
Usefulness of the present invention is:
1. improve iron powder as the application of a kind of reductibility treatment agent in process is polluted, the pollutent of high density can be processed.Can reach more than 70mg/g to the hexavalent chromium solution loading capacity of 100mg/L, treatment effect is good.
2. ferrous powder granules surface coverage polyaniline, can avoid iron powder surface passivation and reduce processing efficiency.
3. the ferrous powder granules in matrix material is uniformly dispersed, and improves the utilization ratio of ferrous powder granules.
4. iron powder and the cheap easily acquisition of attapulgite in matrix material, polyaniline in the composite proportion is lower, causes its cost lower.
5. before iron powder runs out of, treatment effect exists always, has long-term disposal effect.
Accompanying drawing explanation
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 of the present invention absorption Cr (VI).
Embodiment
The preparation method of polyaniline /attapulgite/zero valent iron composite 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) add the aniline of attapulgite quality 5%-35%, stir 0.5h;
(3) add the ammonium persulphate of attapulgite quality 15 ~ 25% as initiator, after stirring, leave standstill 0.5h;
(4) iron powder of attapulgite quality 25-100% is added, dispersed with stirring 0.5h;
(5) suction filtration is to neutral, 60 DEG C of oven dry, and grinding, obtains matrix material.
The mass percent of attapulgite, iron powder, aniline is: attapulgite 25 ~ 50%, iron powder 25 ~ 50%, aniline 5 ~ 11%.
aboveattapulgite used is pure soil; Attapulgite is configured to the aaerosol solution of 0.01 ~ 0.03%; Ferrous powder granules size is 200 ~ 350 orders; Acid used is hydrochloric acid, or nitric acid, or sulfuric acid, or above-mentioned various mixture; Preparation temperature is at 0-25 degree.
The present invention utilizes Attapulgite and polyaniline suspension polymerization, forms full-bodied mixing solutions, adds nulvalent iron particle and is mixed, solve the problem that ferrous powder granules easily precipitates reunion.Common zero-valent iron particle is in water, and 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.The matrix material prepared at low temperatures has good electric conductivity, and electronics shifts on ferrous powder granules surface the reduction contributed to pollutent, and the matrix material under low-temperature growth has higher removal effect.Polyaniline can prevent nulvalent iron particle surface passivation as a kind of novel conductive layer, contributes to the transfer of electronics on its surface, improves the removal capacity of Zero-valent Iron to pollutent.
The present invention is launched further below by more specifically embodiment.
Embodiment 1: preparation temperature is 0 DEG C, takes 2.0g attapulgite, adds 0.5mol/L nitric acid 77mL and stirs 0.5h, adds 0.6mL aniline and stirs 0.5h, add 2.0g ammonium persulphate, leave standstill 0.5h after stirring.Add 350 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 DEG C of oven dry, grinding, obtains blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material, when pH=3, reaches 75.13mg/g to the loading capacity of Cr (VI).As shown in Figure 1, be the electron-microscope scanning picture of obtained product.
Embodiment 2: preparation temperature is 0 DEG C, takes 2.0g attapulgite, adds 0.5mol/L nitric acid 77mL and stirs 0.5h, adds 0.5mL aniline and stirs 0.5h, add 2.0g ammonium persulphate, leave standstill 0.5h after stirring.Add 320 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 DEG C of oven dry, grinding, obtains blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material, when pH=3, reaches 71.37mg/g to the loading capacity of Cr (VI).
Embodiment 3: preparation temperature is 0 DEG C, takes 2.0g attapulgite, adds 0.4mol/L nitric acid 77mL and stirs 0.5h, adds 0.5mL aniline and stirs 0.5h, add 2.0g ammonium persulphate, leave standstill 0.5h after stirring.Add 320 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 DEG C of oven dry, grinding, obtains blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material, when pH=3, reaches 62.91mg/g to the loading capacity of Cr (VI).
Embodiment 4: preparation temperature is 17 DEG C, takes 2.0g attapulgite, adds 0.4mol/L nitric acid 77mL and stirs 0.5h, adds 0.5mL aniline and stirs 0.5h, add 1.0g ammonium persulphate, leave standstill 0.5h after stirring.Add 320 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 DEG C of oven dry, grinding, obtains blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material, when pH=3, reaches 53.17mg/g to the loading capacity of Cr (VI).
Embodiment 5: preparation temperature is 25 DEG C, takes 2.0g attapulgite, adds 0.5mol/L nitric acid 77mL and stirs 0.5h, adds 0.4mL aniline and stirs 0.5h, add 1.0g ammonium persulphate, leave standstill 0.5h after stirring.Add 200 order iron powder 2.0g.Stir 0.5hn, suction filtration is to neutral, and 60 DEG C of oven dry, grinding, obtains blackish green Fe/PANI/ATP matrix material.As shown in Figure 2, matrix material, when pH=3, reaches 38.22mg/g to the loading capacity of Cr (VI).
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; other are any do not deviate from spirit of the present invention and principle under make change, modification, combination, simplification; 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 composite 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) add the aniline of attapulgite quality 5%-35%, stir 0.5h;
(3) add the ammonium persulphate of attapulgite quality 15 ~ 25% as initiator, after stirring, leave standstill 0.5h;
(4) iron powder of attapulgite quality 25-100% is added, dispersed with stirring 0.5h;
(5) suction filtration is to neutral, 60 DEG C of oven dry, and grinding, obtains matrix material.
2. the preparation method of polyaniline /attapulgite/zero valent iron composite material according to claim 1, 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/zero valent iron composite material according to claim 1, is characterized in that, attapulgite used is pure soil.
4. the preparation method of polyaniline /attapulgite/zero valent iron composite material according to claim 1, is characterized in that, attapulgite is configured to the aaerosol solution of 0.01 ~ 0.03%.
5. the preparation method of polyaniline /attapulgite/zero valent iron composite material according to claim 1, is characterized in that, ferrous powder granules size is 200 ~ 350 orders.
6. the preparation method of polyaniline /attapulgite/zero valent iron composite material according to claim 1, is characterized in that, acid used is hydrochloric acid, or nitric acid, or sulfuric acid, or above-mentioned various mixture.
7. the preparation method of polyaniline /attapulgite/zero valent iron composite material according to claim 1, is characterized in that, preparation temperature is at 0-25 degree.
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| CN103588988B (en) * | 2013-11-18 | 2015-04-08 | 兰州理工大学 | Preparation method of porous nano polymer composite material |
| CN104232251B (en) * | 2014-08-28 | 2016-08-17 | 陕西师范大学 | polyaniline composite electrorheological fluid |
| 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 |
| CN104402107B (en) * | 2014-12-02 | 2016-08-17 | 济南大学 | A kind of method processing organic wastewater based on Polyaniline-Supported type nano zero valence 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 |
| 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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| 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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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
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| 徐惠,等.聚苯胺/凹凸棒石黏土纳米纤维复合材料对溶液中痕量Cr(Ⅵ)的吸附性能.《应用化学》.2011,第28卷(第5期),第549-554页. * |
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