CN101537489A - Nanometer zero-valent iron particle capable of stably existing in air, and preparation method thereof - Google Patents
Nanometer zero-valent iron particle capable of stably existing in air, and preparation method thereof Download PDFInfo
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- CN101537489A CN101537489A CN200810052476A CN200810052476A CN101537489A CN 101537489 A CN101537489 A CN 101537489A CN 200810052476 A CN200810052476 A CN 200810052476A CN 200810052476 A CN200810052476 A CN 200810052476A CN 101537489 A CN101537489 A CN 101537489A
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Abstract
The invention relates to a nanometer zero-valent iron particle capable of stably existing in air, and a preparation method thereof. The nanometer zero-valent iron particle capable of stably existing in air takes a nanometer zero-valent iron particle as a core of which the surface is coated with a nanometer chitosan particle. The preparation method adopts a liquid-phase reduction method to prepare the nanometer zero-valent iron particle capable of stably existing in air, utilizes a strong reducing agent KBH4 or NaBH4 to reduce Fe<2+> so as to obtain Fe<0>, and performs surface modification through chitosan so as to greatly improve the oxidation resistance of the nanometer zero-valent iron particle. In addition, the prepared nanometer zero-valent iron particle has the advantages of uniform distribution, small average particle size, large specific surface area, much higher pollutant-removing capability than common iron powder and capability of being widely applied to the field of treating environmental pollution and restoring environment.
Description
Technical field
The present invention relates to field of nanometer technology, especially a kind of nanometer nulvalent iron particle that can existence stable in the air and preparation method thereof.
Background technology
The electronegativity of Zero-valent Iron is bigger, has stronger reproducibility, and adopting the Zero-valent Iron reduction to remove environmental contaminants is technology that domestic and international in recent years broad research is used, and especially adopts a kind of so high-new pollution control technology of nano zero valence iron.Nano zero valence iron is compared with common iron powder, have the advantages that particle diameter is little, specific area big, the surface can be big, with the reaction of other material in have higher activity, treatment effect is far superior to common iron powder, have good application prospects, but the sp act of nano zero valence iron makes it need harsh operating condition in preparation and use.
The preparation method of nanometer nulvalent iron particle mainly comprises gas phase process, liquid phase process and solid phase method at present.
The nanometer nulvalent iron particle of gas phase process preparation, its purity height, particle diameter be little, be uniformly dispersed, but equipment is had relatively high expectations, and apparatus expensive requires HTHP simultaneously, operates dangerous; Though method for preparing solid phase is fairly simple, workable, reunite easily, and the particle diameter skewness etc.
Principle is simple, equipment is simple though liquid phase reduction has, workable, characteristics such as production cost is low, but therefore defectives such as also existing the particle diameter skewness, reunite easily, reactivity is lower must overcome this defective by adding certain dispersant; Simultaneously, the nano zero valence iron air stability is poor, easily oxidation even spontaneous combustion in environment, for nano zero valence iron use and transportation has brought inconvenience, these factors make nano zero valence iron be subjected to many restrictions in actual applications.In order to solve the problem of the easy oxidation of nano-iron particle, generally adopt the coating method that the nanometer nulvalent iron particle of preparation is coated.The nano-iron particle coating adopts inorganic material usually, as carbon-coating, boron nitride, nickel dam etc.Yet the method for this class clad nano nulvalent iron particle can not be prevented oxidation and existence stable in the air fully, and preparation process is comparatively loaded down with trivial details, equipment requires still higher.
Shitosan is a kind of natural biological macromolecular material, have avirulence, nonirritant, excellent biological compatibility, separating property of biosoluble, the present invention carries out finishing by shitosan, make the antioxygenic property of nanometer nulvalent iron particle obtain bigger raising, preparation can existence stable in the air nanometer nulvalent iron particle, and about the preparation of stable existence nanometer nulvalent iron particle in air research report not.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of nanometer nulvalent iron particle that can existence stable in the air and preparation method thereof is provided, this method equipment needed thereby is simple, technology is easy, and obtained nanometer nulvalent iron particle has air stability and reactivity preferably.
The present invention is achieved through the following technical solutions:
A kind of nanometer nulvalent iron particle that can existence stable in the air, the nanometer nulvalent iron particle that this can existence stable in the air is to be core with the nanometer nulvalent iron particle, is coated with the Nano chitosan particle on its surface.
And the molecular weight of described shitosan is 50000-100000.
A kind of preparation method of nanometer nulvalent iron particle that can existence stable in the air, this preparation method may further comprise the steps:
(1). preparation shitosan salpeter solution:
With molecular weight is that the shitosan of 50000-100000 is dissolved in 0.05mol/L HNO
3In the solution, obtaining the quality percentage composition is the shitosan salpeter solution of 0.3-0.8%;
(2). deoxygenation:
In the above-mentioned shitosan salpeter solution of 3ml, add and contain FeSO
47H
2The aqueous solution of O, the molar concentration that makes iron ion is 0.01-1.0mol/L, feeds nitrogen deoxygenation 20-40min then, mechanical agitation 9-11min obtains mixed solution so that mix fully then;
(3). preparation nanometer ferrous solution:
Under mechanical agitation to the freshly prepd KBH of mixed solution and dripping
4Solution or NaBH
4Solution reacts 80-100min, obtains the nanometer ferrous solution of black;
(4). the preparation nanometer nulvalent iron particle:
The nanometer ferrous solution is isolated nanometer nulvalent iron particle through magnetic method, fully wash three times with distilled water, vacuum drying promptly obtain can existence stable in the air nanometer nulvalent iron particle.
And, described to the freshly prepd KBH of mixed solution and dripping
4Solution or NaBH
4The molar concentration of solution is 5-8 a times of iron ion molar concentration.
Advantage of the present invention and beneficial effect are:
1. equipment required for the present invention is simple, technology is easy, and reaction is finished at normal temperatures, and product is a solid phase, and reaction system is a liquid phase, and product separates easily, is applicable to large-scale industrial production.
2. the prepared nanometer nulvalent iron particle of the present invention is evenly distributed, and average grain diameter is little, and specific area is big, far above common iron powder, can be widely used in the processing and the environment remediation field of environmental pollution to the removal ability of pollutant.
3. the particle size distribution range of nanometer nulvalent iron particle of the present invention is 20-80nm, and average grain diameter is 60-70nm, and the stabilizing material shitosan that is adopted is cheap and easy to get, good biocompatibility, and low toxicity and biodegradable can not produce secondary pollution; Carry out finishing by shitosan, make the antioxygenic property of nanometer nulvalent iron particle obtain bigger raising, thereby, have market prospects preferably for the storage of material and transportation have brought facility.
Description of drawings
Fig. 1 removes Cr in the water for the nanometer nulvalent iron particle and the common zeroth order iron powder of the present invention's preparation
6+The performance comparison diagram;
Fig. 2 is the nanometer nulvalent iron particle transmission electron microscope photo of the present invention's preparation;
Fig. 3 deposits the XRD spectra of front and back for the nanometer nulvalent iron particle of the present invention's preparation in air;
Fig. 4 is the thermogravimetric analysis curve of the nanometer nulvalent iron particle of the present invention's preparation.
The specific embodiment
The present invention is described in further detail in conjunction with the accompanying drawings by following examples, but the technology contents that present embodiment is narrated is illustrative, rather than determinate, should not limit to protection scope of the present invention according to this.
Embodiment 1:
A kind of nanometer nulvalent iron particle that can existence stable in the air, this nanometer nulvalent iron particle is to be core with the nanometer nulvalent iron particle, its surface is coated with the Nano chitosan particle.Its preparation method may further comprise the steps:
(1). preparation shitosan salpeter solution:
With molecular weight is that 100000 shitosan is dissolved in 0.05mol/L HNO
3In the solution, obtain the quality percentage composition and be 0.5% shitosan salpeter solution;
(2). deoxygenation:
In the above-mentioned shitosan salpeter solution of 3ml, add the FeSO that 10ml contains 0.2978g
47H
2The aqueous solution of O, the molar concentration that makes iron ion is 0.082mol/L, feeds nitrogen deoxygenation 30min then, mechanical agitation 10min obtains mixed solution so that mix fully then;
(3). preparation nanometer ferrous solution:
Under mechanical agitation to the freshly prepd KBH of mixed solution and dripping 10ml 0.535mol/L
4Solution reacts 90min, obtains the nanometer ferrous solution of black;
(4). the preparation nanometer nulvalent iron particle:
The nanometer ferrous solution is isolated nanometer nulvalent iron particle through magnetic method, fully wash three times with distilled water, vacuum drying promptly obtain can existence stable in the air nanometer nulvalent iron particle.
Embodiment 2:
When the nanometer ferrous solution of preparation black, its reactant adopts NaBH
4Solution substitutes KBH
4Solution gets final product, and other all are same as embodiment 1.
Embodiment 3:
A kind of nanometer nulvalent iron particle that can existence stable in the air, this nanometer nulvalent iron particle is to be core with the nanometer nulvalent iron particle, its surface is coated with the Nano chitosan particle.Its preparation method may further comprise the steps:
(1). preparation shitosan salpeter solution:
With molecular weight is that 50000 shitosan is dissolved in 0.05mol/L HNO
3In the solution, obtain the quality percentage composition and be 0.3% shitosan salpeter solution;
(2). deoxygenation:
In the above-mentioned shitosan salpeter solution of 3ml, add the FeSO that 10ml contains 0.1489g
47H
2The aqueous solution of O, the molar concentration that makes iron ion is 0.041mol/L, feeds nitrogen deoxygenation 20min then, mechanical agitation 10min obtains mixed solution so that mix fully then;
(3). preparation nanometer ferrous solution:
Under mechanical agitation to the freshly prepd KBH of mixed solution and dripping 8ml 0.535mol/L
4Solution reacts 80min, obtains the nanometer ferrous solution of black;
(4). the preparation nanometer nulvalent iron particle:
The nanometer ferrous solution is isolated nanometer nulvalent iron particle through magnetic method, fully wash three times with distilled water, vacuum drying promptly obtain can existence stable in the air nanometer nulvalent iron particle.
Embodiment 4:
When the nanometer ferrous solution of preparation black, its reactant adopts NaBH
4Solution substitutes KBH
4Solution gets final product, and other all are same as embodiment 3.
Embodiment 5:
A kind of nanometer nulvalent iron particle that can existence stable in the air, this nanometer nulvalent iron particle is to be core with the nanometer nulvalent iron particle, its surface is coated with the Nano chitosan particle.Its preparation method may further comprise the steps:
(1). preparation shitosan salpeter solution:
With molecular weight is that 80000 shitosan is dissolved in 0.05mol/L HNO
3In the solution, obtain the quality percentage composition and be 0.8% shitosan salpeter solution;
(2). deoxygenation:
In the above-mentioned shitosan salpeter solution of 3ml, add the FeSO that 10ml contains 0.0745g
47H
2The aqueous solution of O, the molar concentration that makes iron ion is 0.021mol/L, feeds nitrogen deoxygenation 40min then, mechanical agitation 10min obtains mixed solution so that mix fully then;
(3). preparation nanometer ferrous solution:
Under mechanical agitation to the freshly prepd KBH of mixed solution and dripping 3ml 0.535mol/L
4Solution reacts 100min, obtains the nanometer ferrous solution of black;
(4). the preparation nanometer nulvalent iron particle:
The nanometer ferrous solution is isolated nanometer nulvalent iron particle through magnetic method, fully wash three times with distilled water, vacuum drying promptly obtain can existence stable in the air nanometer nulvalent iron particle.
Embodiment 6:
When the nanometer ferrous solution of preparation black, its reactant adopts NaBH
4Solution substitutes KBH
4Solution gets final product, and other all are same as embodiment 5.
The present invention utilizes strong reductant KBH
4Or NaBH
4Reduction Fe
2+Obtain Fe
0, its reaction equation is:
Fe
2++2BH
4 -+6H
2O→Fe
0+2B(OH)
3+7H
2↑
The performance comparative test of Cr (VI) is as follows in the nano zero valence iron of the present invention's preparation and the common zeroth order iron powder removal water:
In being Cr (VI) solution of 40mg/L, the 100ml initial concentration adds nanometer nulvalent iron particle and common zeroth order iron powder respectively, normal temperature and pressure is reaction down, adopt diphenyl carbazide spectrophotometry to measure residual Cr (VI) in the solution, add under the condition of dosage far below common zeroth order iron powder at nano zero valence iron, its removal effect is better than common zeroth order iron powder far away, as shown in Figure 1.
The nanometer nulvalent iron particle interpretation of result of using TEM (transmission electron microscope), mensuration the present invention of XRD (X-ray diffraction), TG-DTA (the comprehensive heat of thermogravimetric/differential thermal is analyzed) to obtain is as follows:
(1) test result of TEM
TEM result shows that this nanometer nulvalent iron particle particle size distribution range is 20-80nm, and average grain diameter is 60-70nm, is coated with shitosan at the nano zero-valence iron surface.Referring to Fig. 2.
(2) test result of XRD
The test result of XRD shows that prepared nano zero valence iron is a fe, deposits not occur iron oxide impurity after two months in air.Referring to Fig. 3.
(3) utilize TG-DTA that the stability of nano zero valence iron is further analyzed, from about room temperature to 220 ℃, the TG curve is steady, illustrates to be coated with the basic no change of nano zero valence iron quality of shitosan this moment; From about 220-about 340 ℃, quality occurs and reduce step, corresponding to the thermal decomposition of coating shitosan in the material; After about 340 ℃, the nano zero-valence weight of iron begins to increase, and promptly the clad material shitosan begins to decompose in system this moment, and the residue nanometer nulvalent iron particle by dioxygen oxidation, thereby causes quality obviously to increase under air atmosphere.The nano zero valence iron of the preparation of the present invention as seen from the above analysis has good heat endurance below 340 ℃.Referring to Fig. 4.
Claims (4)
- One kind can existence stable in the air nanometer nulvalent iron particle, it is characterized in that: the nanometer nulvalent iron particle that this can existence stable in the air is to be core with the nanometer nulvalent iron particle, is coated with the Nano chitosan particle on its surface.
- 2. nanometer nulvalent iron particle that can existence stable in the air according to claim 1, it is characterized in that: the molecular weight of described shitosan is 50000-100000.
- 3. the preparation method of a nanometer nulvalent iron particle that can existence stable in the air as claimed in claim 1, it is characterized in that: the preparation method may further comprise the steps:(1). preparation shitosan salpeter solution:With molecular weight is that the shitosan of 50000-100000 is dissolved in 0.05mol/L HNO 3In the solution, obtaining the quality percentage composition is the shitosan salpeter solution of 0.3-0.8%;(2). deoxygenation:In the above-mentioned shitosan salpeter solution of 3ml, add and contain FeSO 47H 2The aqueous solution of O, the molar concentration that makes iron ion is 0.01-1.0mol/L, feeds nitrogen deoxygenation 20-40min then, mechanical agitation 9-11min obtains mixed solution so that mix fully then;(3). preparation nanometer ferrous solution:Under mechanical agitation to the freshly prepd KBH of mixed solution and dripping 4Solution or NaBH 4Solution reacts 80-100min, obtains the nanometer ferrous solution of black;(4). the preparation nanometer nulvalent iron particle:The nanometer ferrous solution is isolated nanometer nulvalent iron particle through magnetic method, fully wash three times with distilled water, vacuum drying promptly obtain can existence stable in the air nanometer nulvalent iron particle.
- 4. the preparation method of nanometer nulvalent iron particle that can existence stable in the air according to claim 3 is characterized in that: described to the freshly prepd KBH of mixed solution and dripping 4Solution or NaBH 4The molar concentration of solution is 5-8 a times of iron ion molar concentration.
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| CN102205419A (en) * | 2011-03-28 | 2011-10-05 | 北京师范大学 | Novel method for preparing load nano zero valent iron |
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| CN108555010A (en) * | 2018-01-31 | 2018-09-21 | 中冶华天南京工程技术有限公司 | Application and method of the nano zero valence iron of Chitosan-coated in removal heavy-metal contaminated soil antimony |
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Application publication date: 20090923 |