CN102179524B - Method for preparing coated nano zero valent iron by rheological phase reaction method, and prepared product thereof - Google Patents
Method for preparing coated nano zero valent iron by rheological phase reaction method, and prepared product thereof Download PDFInfo
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- CN102179524B CN102179524B CN201110095499A CN201110095499A CN102179524B CN 102179524 B CN102179524 B CN 102179524B CN 201110095499 A CN201110095499 A CN 201110095499A CN 201110095499 A CN201110095499 A CN 201110095499A CN 102179524 B CN102179524 B CN 102179524B
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Abstract
The invention relates to a method for preparing coated nano zero valent iron by a rheological phase reaction method, and a prepared product thereof. The method comprises the following steps: adding carboxy methylated cellulose (CMC) liquid medium at the concentration of 0.06g/ml into chemical pure ferrous sulfate and boracic acid which serve as main raw materials in a solid-to-liquid ratio of 1 to 2, performing rheological phase reaction for two hours, washing the product by using absolute ethanol, and distilling and separating to obtain the powdery nano zero valent iron. The preparation method is simple, and is easy to control, and environment-friendly, the steps of ball-milling, sintering and the like are saved, and the product has high environment friendliness, does not cause secondary pollution and can be widely applied to environment treatment and repairing.
Description
Technical field
The present invention relates to a kind ofly be equipped with the method for cladding nanometer Zero-valent Iron and the product that makes thereof, refer in particular to a kind of coated nano zero valence iron that can be applicable to environmental improvement and reparation with the rheological phase reaction legal system.
Background technology
The Zero-valent Iron electronegativity is bigger, has stronger reproducibility.Utilize it to handle some micro quantity organic pollutant in the water body, and can play the effect of catalyst, accelerated reaction process.The lab and field lab scale all shows; Zero-valent iron particle can degrade halogenated aliphatic hydrocarbon class, halogenated aryl hydrocarbon class and part polychlorinated biphenyl chemical pollutant etc.; Promptly after the halogen atom on the pollutants such as halogenated hydrocarbons or halogenated aryl hydrocarbon obtains electronics that Zero-valent Iron provides; Halogen just splits away off from molecule, makes the halo pollutant be converted into nontoxic or is prone to by biodegradable organic matter, like ethene etc.Zero-valent iron particle is because its low price; Aboundresources can be widely used in reparation and receive the soil and the water body of organochlorine contamination, and can handle multiple pollutant simultaneously; For example therefore heavy metal, dyestuff, substituted-nitrobenzene, agricultural chemicals etc. are widely used in environmental area.But the practicality of nano material is to be prerequisite with its fine dispersion in surrounding medium and long-term stability, otherwise one is to be difficult to bring into play its excellent performance; The 2nd, bring many difficulties to transportation, preservation and use.And in the existing technology of preparing, preparation condition is harsh mostly, complex equipments; Also can't improve its dispersed and aerial stability simultaneously preferably.
Summary of the invention
The technical problem that the present invention will solve provides a kind of method of the cladding nanometer Zero-valent Iron that can be applicable to environmental improvement and reparation with rheological phase reaction method preparation and the product that makes thereof.
Technical scheme of the present invention is:
A kind of method that is equipped with the cladding nanometer Zero-valent Iron with the rheological phase reaction legal system; It is characterized in that comprising the steps: that with ferrous sulfate and boron potassium hydrogen phthalate be raw material; At first ferrous sulfate and boron potassium hydrogen phthalate were joined in the reactor in 1: 2 in molar ratio and mix; In reactor, adding 40 ℃ of constant temperature, mass percent concentration by solid-to-liquid ratio 1: 2 again is 6% CMC liquid medium, is modulated into rheological body through mechanical agitation; Under the vacuum stirring at normal temperature, carry out rheological phase reaction then and obtain Zero-valent Iron and boric acid solidliquid mixture; At last, through behind the absolute ethanol washing in vacuum tank separated liquid obtain powdery cladding nanometer Zero-valent Iron.
The said rheological phase reaction time is 2 hours.
Said ferrous sulfate and boron potassium hydrogen phthalate material purity are chemical pure.。
The addition of said absolute ethyl alcohol is solid-to-liquid ratio 1: 2.
The temperature of said separated liquid is 100 ℃
A kind of cladding nanometer Zero-valent Iron product that makes by said method.
It is following that rheology phase legal system is equipped with the chemical equation of cladding nanometer iron:
Fe
2++2BH
4 -+6H
2O→Fe+2B(OH)
3+7H
2
From the transmission electron microscope photo of coated nano zero valence iron shown in the accompanying drawing 1; Can find out clearly that CMC is rolled into sphere with nano iron particles and is kept apart each other, be discrete state and do not interconnect; It is more even to be rolled into spherical fineness ratio; Size is explained the existence of surperficial dispersing agent C MC about 100nm, weakened the magnetic attracting force between the nano iron particles; Because of the nano iron particles surface is coated by the electronegative CMC molecular layer of one deck; Because electrostatic repulsion and space steric effect between the CMC molecule; Make between the nano iron particles and can not flock together because of magnetic attraction; Overcome small-size effect, skin effect, surface electronic effect preferably and that closely effect produced was soft-agglomerated, so the dispersiveness of nanometer iron is improved because of nano particle.
In addition; Chemical pure reducing agent (boron potassium hydrogen phthalate) and raw material (ferrous sulfate); Before getting into the reaction of rheology phase system had been superfine powdered form, added after liquid medium (CMC) is mixed with the rheology phase system again, generally chemically had complicated composition or structure owing to be in the material of rheology attitude; The character of removing solid but also the character that demonstrates liquid on mechanics, had not only been shown, in other words like solid non-solid, like the non-liquid of liquid; Can be the material that had not only comprised solid particle but also comprised liquid on physical composition, can flow or slowly flow, the uniform a kind of complex system of macroscopic view; Overcome in other preparation processes such as wet method the dispersiveness that has further improved nanometer iron because of hard aggregations that power produced such as capillary benefit, chemical bond, brilliant bridge, hydrogen bonds preferably.
Prepared cladding nanometer iron in the covert system of convection current of the present invention; Can effectively improve the dispersed and aerial stability of nano-iron particle; In the aqueous solution, have efficiently absorption property and have the character of slow release, can be used for the processing of waste water and the reparation of groundwater environment.This method has effectively reduced preparation environmental requirement and equipment requirements; Under the room temperature normal pressure, use common instrument just can accomplish, be expected to realize suitability for industrialized production, therefore effectively reduced energy consumption, material consumption; And be somebody's turn to do article tool environment compatibility preferably; Do not produce secondary pollution, meet the requirement that makes up recycling economy, friendly environment society, have considerable economic and social benefit.
Description of drawings
The transmission electron microscope check and analysis photo of the coated nano zero valence iron that accompanying drawing 1 makes for embodiment.
The specific embodiment
Embodiment:
The first step: 6gCMC is dissolved in the 100mL deionized water, under the condition of 40 ℃ of little heating, is mixed with liquid medium and is incubated subsequent use with magnetic stirrer stirring 1h;
Second step: accurately take by weighing chemical pure ferrous sulfate 2mol and boron potassium hydrogen phthalate 4mol, in mortar, mix 10min, it is subsequent use to make solid mixture;
The 3rd step: take by weighing the 50g solid mixture in the 200ml beaker, add the 100mlCMC liquid medium and mix, stir 30min and be mixed with the rheology attitude;
The 4th step: under the vacuum stirring at normal temperature, carry out rheological phase reaction 2h, obtain Zero-valent Iron and boric acid solidliquid mixture;
The 5th step: clean Zero-valent Iron and boric acid solidliquid mixture 3 times with the 100mL absolute ethyl alcohol, during washing with the attraction solid matter in the bottom so that liquid pouring is gone out, each washing need quick stirring 3 minutes, leaves standstill 10 minutes;
The 6th step: will wash good black solid material 100 ℃ of evaporates to dryness in vacuum tank and become cladding nanometer Zero-valent Iron powdery to get final product.
The JSM-2010 type transmission electron microscope that uses Jeol Ltd. to produce makes cladding nanometer Zero-valent Iron product to the foregoing description and carries out the check and analysis of grain morphology, granular size.
Claims (6)
1. method that is equipped with the cladding nanometer Zero-valent Iron with the rheological phase reaction legal system; It is characterized in that comprising the steps: that with ferrous sulfate and boron potassium hydrogen phthalate be raw material; At first ferrous sulfate and boron potassium hydrogen phthalate were joined in the reactor in 1: 2 in molar ratio and mix; In reactor, adding 40 ℃ of constant temperature, mass percent concentration by solid-to-liquid ratio 1: 2 again is 6% CMC liquid medium, is modulated into rheological body through mechanical agitation; Under the vacuum stirring at normal temperature, carry out rheological phase reaction then and obtain Zero-valent Iron and boric acid solidliquid mixture; At last, through behind the absolute ethanol washing in vacuum tank separated liquid obtain powdery cladding nanometer Zero-valent Iron.
2. preparation method according to claim 1 is characterized in that: the said rheological phase reaction time is 2 hours.
3. preparation method according to claim 1 is characterized in that: said ferrous sulfate and boron potassium hydrogen phthalate material purity are chemical pure.
4. preparation method according to claim 1 is characterized in that: the addition of said absolute ethyl alcohol is solid-to-liquid ratio 1: 2.
5. preparation method according to claim 1 is characterized in that: the temperature of said separated liquid is 100 ℃.
6. one kind is equipped with the nano zero-valence iron product that the method for cladding nanometer Zero-valent Iron makes by claim 1 is said with the rheological phase reaction legal system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110095499A CN102179524B (en) | 2011-04-18 | 2011-04-18 | Method for preparing coated nano zero valent iron by rheological phase reaction method, and prepared product thereof |
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| CN201110095499A CN102179524B (en) | 2011-04-18 | 2011-04-18 | Method for preparing coated nano zero valent iron by rheological phase reaction method, and prepared product thereof |
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| CN102179524A CN102179524A (en) | 2011-09-14 |
| CN102179524B true CN102179524B (en) | 2012-10-03 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104785793B (en) * | 2015-03-25 | 2017-06-13 | 昆明理工大学 | The preparation method of cellulose modifying modified Nano iron particle |
| CN105945299A (en) * | 2016-04-28 | 2016-09-21 | 杭州电子科技大学 | Application of nano-iron synthesized by tea leaves in p,p'-DDT removal |
| CN108043188B (en) * | 2017-11-23 | 2020-08-18 | 浙江海洋大学 | Organic waste gas purification process for adhesive products |
| CN107899388B (en) * | 2017-11-23 | 2020-08-18 | 浙江海洋大学 | Fluorine-containing waste gas treatment process |
| CN109718224A (en) * | 2019-03-05 | 2019-05-07 | 深圳大学 | A kind of iron-based Nano medication and preparation method thereof with sour responsiveness release hydrogen |
| CN112920808B (en) * | 2020-02-20 | 2021-10-29 | 北京航空航天大学 | CMC-coated NZVI particles for repairing halogenated organic matters in electronic refuse landfill and preparation method thereof |
| CN113716545B (en) * | 2021-08-19 | 2023-03-21 | 南开大学 | Method for preparing charcoal-loaded nano zero-valent iron by using particle structure regulation and control strategy |
-
2011
- 2011-04-18 CN CN201110095499A patent/CN102179524B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 钱慧静.浙江大学硕士学位论文.《CMC对纳米零价铁去除污染水体中六价铬的影响》.2008,第23页. * |
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