CN103084585A - Preparation method of active carbon / vermiculite supported zero valent nano iron - Google Patents
Preparation method of active carbon / vermiculite supported zero valent nano iron Download PDFInfo
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- CN103084585A CN103084585A CN 201310053197 CN201310053197A CN103084585A CN 103084585 A CN103084585 A CN 103084585A CN 201310053197 CN201310053197 CN 201310053197 CN 201310053197 A CN201310053197 A CN 201310053197A CN 103084585 A CN103084585 A CN 103084585A
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Abstract
The invention provides a preparation method of active carbon / vermiculite supported zero valent nano iron, and relates to the development and innovation of environment friendly materials. The preparation method uses cheap active carbon, vermiculite and ferrous sulfate as raw materials, fully uses the adsorptive property of the active carbon and the vermiculite, prepares the active carbon / vermiculite supported zero valent nano iron, and expands the application range and the value of the active carbon / vermiculite supported zero valent nano iron in the environment. The preparation method comprises the following steps: moderate vitriolic ferrite, dispersing agent and active carbon / vermiculite are added into a reactor, then the pH of potassium borohydride solution is adjusted to 6, and the potassium borohydride solution is dripped into the reactor dropwise. During the preparation process, nitrogen is kept to be supplied, velocity mixing is continuously carried out, timing is started from the dripping adding, reaction time is 30 min, and the active carbon / vermiculite supported zero valent nano iron can be obtained. The preparation method of the active carbon / vermiculite supported zero valent nano iron has the advantages that the raw materials are cheap and easy to obtain, the steps are simple, equipment needed is simple, and a process is simple, the obtained supported zero valent nano iron has better dispersity and inoxidizability compared with individual zero valent nano iron.
Description
Technical field
The present invention relates to the development innovation of ep-type material, specifically, exactly take active carbon/vermiculite as matrix, with the preparation method of thereon active carbon of zeroth order Nanoscale Iron load/vermiculite support type zeroth order Nanoscale Iron, thereby reduce the easily oxidizable energy of even avoiding simple zeroth order Nanoscale Iron.
Background technology
Active carbon/vermiculite support type zeroth order Nanoscale Iron, take active carbon and vermiculite as carrier, with zeroth order Nanoscale Iron load support type zeroth order Nanoscale Iron thereon, has surface area large, reduce and avoid the easily oxidizable energy of simple zeroth order Nanoscale Iron, thereby improved its range of application aspect environment, extended to soil from water body, bed mud, had broad application prospects.
The zeroth order Nanoscale Iron is very easily oxidation in air, and in water body, agglomeration can occur, and Supported Nano Zero-valent Iron can not only zeroth order strengthen the non-oxidizability of Nanoscale Iron, and has improved its dispersiveness in medium.Due to the special construction of active carbon and vermiculite, the absorption of nutriment in soil and pollutant, migration are all played a very important role.
At present, the preparation method of zeroth order Nanoscale Iron mainly contains Physical and chemical method, and chemical method comprises liquid phase chemical reduction method, reactive hydrogen-molten reactant metal method, gas chemistry reducing process and gas phase thermal decomposition method etc.The present invention adopts the method for liquid-phase reduction, synthetic zeroth order Nanoscale Iron under the condition of high-speed stirred.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of active carbon/vermiculite support type zeroth order Nanoscale Iron, utilize cheap active carbon, vermiculite and ferrous sulfate to be raw material, take full advantage of the absorption property of active carbon and vermiculite, prepare active carbon/vermiculite support type zeroth order Nanoscale Iron, thereby improved the dispersive property of zeroth order Nanoscale Iron in medium, expanded its range of application and value in environment.
The preparation method of active carbon proposed by the invention/vermiculite support type zeroth order Nanoscale Iron is as follows: add appropriate ferrous sulfate, dispersant and active carbon/vermiculite in reactor, the pH that then regulates solution of potassium borohydride is 6, dropwise adds in reactor.Keep during this time logical nitrogen, constantly high-speed stirred, be 30min from beginning to drip the solution of potassium borohydride timing, reacting, and gets final product to get active carbon/vermiculite support type zeroth order Nanoscale Iron.
To the XRD of the active carbon of the inventive method preparation/vermiculite support type zeroth order Nanoscale Iron and TEM test as seen, with respect to independent active carbon and vermiculite, on support type zeroth order Nanoscale Iron diffraction curve, obvious Fe peak (Fig. 1) is arranged; Absorption has a large amount of zeroth order Nanoscale Irons on active carbon and vermiculite matrix, and its particle diameter shows to have generated active carbon/vermiculite support type zeroth order Nanoscale Iron (Fig. 2) in the 80nm left and right.
The available useful technique effect of the present invention is: the method raw material is cheap to be easy to get, and step is simple, and equipment needed thereby is simple, the more independent zeroth order Nanoscale Iron of support type zeroth order Nanoscale Iron of simple process gained, dispersed and not easily oxidizable be greatly improved.
Description of drawings
The scanning electron microscope (SEM) photograph of the activated carbon supported type Nanoscale Iron of Fig. 1
The scanning electron microscope (SEM) photograph of Fig. 2 vermiculite Supported Nano Zero-valent Iron
The powder diagram of the X ray of the activated carbon supported type Nanoscale Iron of Fig. 3
The powder diagram of the X ray of Fig. 4 vermiculite Supported Nano Zero-valent Iron
The specific embodiment
The preparation method of active carbon/vermiculite support type zeroth order Nanoscale Iron is as follows:
With ferrous sulfate (FeSO
4) be raw material, 0.278g ferrous sulfate, 0.3g polyethylene glycol and appropriate active carbon and vermiculite are joined (absolute ethyl alcohol/deionized water=4/1) in 30mL solution, the 0.212g potassium borohydride is joined in the 20mL deionized water, add 1mL0.5molL
-1Sodium hydroxide solution, regulating pH is 6, dropwise add in reactor with constant voltage titration funnel, during keep logical nitrogen, the stirring of broken height speed, then can obtain support type zeroth order Nanoscale Iron.
The loaded nano ferrous solution namely gets the loaded nano iron powder through magnetic separation, washing, vacuum drying.
The experiment test explanation
The interpretation of result of the active carbon that the present invention of use TEM (transmission electron microscope), XRD (X-ray diffraction) mensuration obtains/vermiculite loaded with nano iron powder is as follows:
(1) test result of TEM:
TEM result (Fig. 1 and Fig. 2) shows that this nano particle is the irregular particle shape, and particle diameter is nanoscale in the 100nm left and right.
(2) test result of XRD:
Adopt X-ray diffraction to carry out material phase analysis to product, wherein X-ray diffracting spectrum (Fig. 3 and Fig. 4) at 44.75 ° of characteristic peaks that iron occurs (A), proves in the load product and contains Zero-valent Iron.The particle of Zero-valent Iron is little, and crystallographic grain is little, causes peak shape wider.
Claims (4)
1. the preparation method of active carbon/vermiculite support type zeroth order Nanoscale Iron, it is characterized in that take soluble-salt as raw material, soluble-salt is dissolved dispersion in the aqueous solution, add appropriate dispersant and the vermiculite through grinding, preparation potassium borohydride alkali lye, pH is 6 with the alkali lye adjustment, be added drop-wise in reactor, from dripping the beginning timing, 30min reacts end, gets final product to get active carbon/vermiculite support type zeroth order Nanoscale Iron.
2. require the preparation method of 1 described active carbon/vermiculite support type zeroth order Nanoscale Iron according to patent, it is characterized in that regulator solution pH is faintly acid (6 left and right).
3. require the preparation method of 2 described active carbons/vermiculite support type zeroth order Nanoscale Iron according to patent, the solution that it is characterized in that regulator solution pH is 0.5molL
-1
4. require the preparation method of 1 described active carbon/vermiculite support type zeroth order Nanoscale Iron according to patent, it is characterized in that soluble-salt is ferrous oxide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787430A (en) * | 2014-01-20 | 2014-05-14 | 浙江理工大学 | Composite material for rapidly and deeply treating organo-chlorine pesticide wastewater |
| CN104084125A (en) * | 2014-06-25 | 2014-10-08 | 华南理工大学 | Nano-iron-loaded sintered active carbon as well as preparation method and application thereof |
| CN105728744A (en) * | 2016-04-29 | 2016-07-06 | 蒋军荣 | Preparation method of stabilized activated carbon/nanometer Pd/Fe (palladium/ferrous) composite particle |
| CN109821878A (en) * | 2019-01-28 | 2019-05-31 | 四川大学 | Vermiculite loads nanometer iron-based material to the fixing means of heavy metal-polluted soil lead |
-
2013
- 2013-02-19 CN CN 201310053197 patent/CN103084585A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787430A (en) * | 2014-01-20 | 2014-05-14 | 浙江理工大学 | Composite material for rapidly and deeply treating organo-chlorine pesticide wastewater |
| CN103787430B (en) * | 2014-01-20 | 2015-07-22 | 浙江理工大学 | Composite material for rapidly and deeply treating organo-chlorine pesticide wastewater |
| CN104084125A (en) * | 2014-06-25 | 2014-10-08 | 华南理工大学 | Nano-iron-loaded sintered active carbon as well as preparation method and application thereof |
| CN104084125B (en) * | 2014-06-25 | 2016-08-24 | 华南理工大学 | A kind of sintering activity charcoal loading Nanoscale Iron and its preparation method and application |
| CN105728744A (en) * | 2016-04-29 | 2016-07-06 | 蒋军荣 | Preparation method of stabilized activated carbon/nanometer Pd/Fe (palladium/ferrous) composite particle |
| CN109821878A (en) * | 2019-01-28 | 2019-05-31 | 四川大学 | Vermiculite loads nanometer iron-based material to the fixing means of heavy metal-polluted soil lead |
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Application publication date: 20130508 |