CN101306862A - Method for preparing nano-level Fe<0>/Fe3O4 and uses thereof - Google Patents
Method for preparing nano-level Fe<0>/Fe3O4 and uses thereof Download PDFInfo
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- CN101306862A CN101306862A CNA2008100627417A CN200810062741A CN101306862A CN 101306862 A CN101306862 A CN 101306862A CN A2008100627417 A CNA2008100627417 A CN A2008100627417A CN 200810062741 A CN200810062741 A CN 200810062741A CN 101306862 A CN101306862 A CN 101306862A
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Abstract
The invention discloses a method for preparing nanoscale Fe0F3O4 and an application thereof. The method comprises the steps of: adding 0.5 to 1 mmol of FeSO4.7H2O into 400 ml of water, then inletting nitrogen for 0.5 to 1 hour to remove and dissolve oxygen, and then adding 0.5 to 1.5g Fe3O4 and adding 100 ml of NaBH4 water solution drop by drop under the condition of uninterruptedly inletting N2 and stirring continuously, so as to obtain the Nanoscale Fe0F3O4, wherein the initial molar concentration of the NaBH4 water solution is eight times the FeSO4.7H2O solution. The Nanoscale Fe0Fe3O4 can be used in the reduction restoration of Cr (VI) in water. The preparation method of the Nanoscale Fe0/Fe3O4 is simple, quick to react, overcomes the defect that the Nanoscale Fe0 is easy to congregate and be oxidized due to the affect of the globe magnetic field and the static magnetic force among granules, thereby reducing the defect of reaction activity, but makes use of the weak magnetism of the magnetite to have the Nanoscale Fe0 highly dispersed on the surface of a magnetite and form a highly efficient Fe2+-Fe3+ electronic circulation and Fe0-Fe3O4 electronic transporting reduction system solving the problem that Fe0 is hard to transport electrons due to the inactive surface, improving the reduction capability and effectively removing the Cr(VI) in water.
Description
Technical field
The present invention relates to a kind of nanoscale Fe
0/ Fe
3O
4Preparation method and its usage.
Background technology
Produce and life process in all contaminations that discharges enter environment by all means, severe contamination atmosphere, soil, underground water and surface water system, serious threat human beings'health and is lived.Wherein Cr (VI) is one of ubiquitous priority pollutant in underground water, soil and the surface water body.
Cr (VI), total chromium are " integrated wastewater discharge standard " first kind pollutent in (GB8978-1996), and its highest permission discharge quality concentration is respectively 0.5mg/L and 1.5mg/L.Cr (VI) is the carcinogens that international anticancer research center and U.S.'s toxicology tissue are announced, has tangible carcinogenesis, often contacts heavy dose of Cr (VI) and can cause the ulcer of contact site or cause untoward reaction.The Cr of excess intake (VI) can cause kidney and liver damage, feels sick, GI irritation, stomach ulcer, spasm even death.Cr (VI) also can enter DNA and entail the next generation.According to test, when containing chromium 1mg/L in the water, can stimulate plant growth, can make plant growth slow during 1～10mg/L, crop stops growing during to 100mg/L, is on the verge of death.When containing chromium cpd in the waste water, can reduce the efficient of biological wastewater treatment.
Discover Fe
0Almost can remove pollutent main in the polluted underground water, comprise the dechlorination of chlorinated organics in the underground water, the denitrogenation of nitrate, reach the reparation of Cr heavy metals such as (VI) in the underground water etc., and the ferric oxide (ironic hydroxide, iron carbonate etc.) that the oxidized back of iron forms can adsorb multiple pollutent, as As (II).Utilizing ferrous metal to handle phreatic system, can be ground, also can mix with sand grains as the reaction wall directly to be embedded in the waterbearing stratum.
Though metallic iron can make chlorinated organics and nitrate dechlorination, denitrogenation effectively, can reduce repairing heavy metal pollution, but still be faced with following challenge:
(1) along with the carrying out of reaction, the metallic iron surface forms metal hydroxides or carbonate passivation layer gradually, makes the reactive behavior of iron reduce.
(2) nano level Fe
0Though can improve reactive behavior, because particle is less, under the influence of magnetostatic power between terrestrial magnetic field and particle, assemble agglomeratingly easily, and be exposed to oxidation easily takes place in the air, thereby influence the performance of reactive behavior.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of nanoscale Fe is provided
0/ Fe
3O
4Preparation method and its usage.
Nanoscale Fe
0/ Fe
3O
4The preparation method be FeSO with 0.5～1mmol
47H
2O adds in the 400ml water, and logical nitrogen 0.5～1h removes dissolved oxygen then, adds 0.5～1.5g Fe again
3O
4, constantly passing into N
2And under the condition of continuous stirring, splash into 100ml NaBH
4The aqueous solution, NaBH
4The initial molar concentration of the aqueous solution is FeSO
47H
28 times of O solution obtain nanoscale Fe
0/ Fe
3O
4
Nanoscale Fe
0/ Fe
3O
4Be used for underground water and the chromic removal of waste water and reparation.
The beneficial effect that the present invention compared with prior art has:
1) nanoscale Fe
0/ Fe
3O
4System preparation method is simple, and reaction speed is fast.Only need three kinds of chemical reagent in the preparation process, namely at first make NaBH
4And FeSO
47H
2O reacts, and has added stabilisation and dispersing nanometer level Fe again
0The Fe of effect
3O
4, reaction can be finished in 0.5-1h, and the time is short;
2) nanoscale Fe
0/ Fe
3O
4Nanoscale Fe in the system
0Diameter is all below 100nm, at Fe
3O
4Faint magnetic action under, can be dispersed in Fe
3O
4The surface, the specific area of whole system is significantly increased (as shown in Figure 2), reaction rate improves greatly;
3) at nano level Fe
0/ Fe
3O
4In the system, utilize Fe
3O
4Faint magnetic, make nano level Fe
0High dispersing is at Fe
3O
4Particle surface has overcome nano level Fe
0Easy shortcoming of reuniting; Simultaneously, using this system to remove in the reaction of Cr (VI) in the water Fe
2+Behind the reduction Cr (VI), generate Fe
3+, electronics is from being positioned at Fe
3O
4The Fe on surface
0In transfer to Fe
3O
4On, the Fe that generates
3+Reduction becomes Fe
2+Thereby, form a reduction system efficiently, solved Fe
0Owing to surface passivation causes the problem of electron transport difficulty, make reducing power increase substantially,
4) nanoscale Fe
0/ Fe
3O
4In nanoscale Fe
0Good dispersion, the reactivity height.As Fe
3O
4When existing, only add 0.05g/L nanoscale Fe
0, can make initial concentration be 20mg/L Cr (VI) the reaction 15 minutes after, reach 100% Cr (VI) clearance.In contrast to this, there be not Fe
3O
4Exist, when other conditions are identical, the removal efficient of Cr (VI) only is about 50%.
Description of drawings
Fig. 1 is common nano level Fe
0Transmission electron microscope picture;
Fig. 2 is nanoscale Fe
0/ Fe
3O
4The transmission electron microscope picture of system.
Embodiment
Nanoscale Fe
0/ Fe
3O
4The preparation method be FeSO with 0.5～1mmol
47H
2O adds in the 400ml water, and logical nitrogen 0.5～1h removes dissolved oxygen then, adds 0.5～1.5g Fe again
3O
4, constantly passing into N
2And under the condition of continuous stirring, splash into 100ml NaBH
4The aqueous solution, NaBH
4The initial molar concentration of the aqueous solution is FeSO
47H
28 times of O solution obtain nanoscale Fe
0/ Fe
3O
4
Nanoscale Fe
0/ Fe
3O
4Be used for underground water and the chromic removal of waste water and reparation.
Nanoscale Fe
0/ Fe
3O
4Preparation method's reaction equation as follows:
Fe(H
2O)
6 2++2BH
4 -→Fe↓+2B(OH)
3+7H
2↑
Foundation of the present invention is nano level Fe
0Have bigger specific surface area, have dispersiveness preferably on the magnetite surface, can effectively stop nano level Fe
0Gathering.
Nanoscale Fe proposed by the invention
0/ Fe
3O
4Purposes, its technical characterstic is: adopt senior reduction technique synchronously, the water body contain Cr (VI) is repaired in reduction rapidly, passes into continuously nitrogen in the whole course of reaction to keep good anaerobic environment.For the preparation of nanoscale Fe
0/ Fe
3O
4Water before reaction, need pass into nitrogen, aeration 2 hours is with except the dissolved oxygen in anhydrating.
Of the present invention being further characterized in that, nanoscale Fe
0/ Fe
3O
4Under the reducing environment of anaerobism, the reaction that namely have fast, efficient reparation contains the effect of Cr (VI) water body.In the common scope of 0～40 ℃ of occurring in nature water temperature, general preferred temperature value is 25 ℃ (being normal temperature); The pH value of water is neutral, need not to regulate; The concentration range that is fit to common underground water pollutant is 0.05～200ppm.
Nanoscale Fe
0/ Fe
3O
4Be used for containing the reparation of Cr (VI) polluted-water.Concrete steps are as follows:
Pass into continuously nitrogen, keeping in the situation of good anaerobic environment, in containing Cr (VI) contaminant water, adding nanoscale Fe
0/ Fe
3O
4, pollutant and nanoscale Fe
0Usage ratio be about 1: 2, contain Cr (VI) polluted-water and nanoscale Fe
0/ Fe
3O
4Fully contact is after 15 minutes, and water body obtains repairing, purifying.
Embodiment 1:
FeSO with 0.5mmol
47H
2O adds in the 400ml water, and passes into nitrogen removal dissolved oxygen, and duration of ventilation is 0.5h, adds then 1.5g Fe
3O
4, constantly passing into N
2And under the condition of continuous stirring, splash into 100mlNaBH
4The aqueous solution, NaBH
4The molar concentration of the aqueous solution is FeSO
47H
28 times of O solution obtain nanoscale Fe
0/ Fe
3O
4
In initial pH value is 5.5, and temperature of reaction is under 30 ℃ the condition, and to wherein adding 10mg Cr (VI), Cr (VI) clearance is 100% behind the reaction 15min.Under the equal conditions, if there is not Fe
3O
4Exist, removing efficient only is about 50%.
Embodiment 2:
FeSO with 1mmol
47H
2O adds in the 400ml water, and passes into nitrogen removal dissolved oxygen, and duration of ventilation is 0.5h, adds then 0.5g Fe
3O
4, constantly passing into N
2And under the condition of continuous stirring, splash into 100mlNaBH
4The aqueous solution, NaBH
4The molar concentration of the aqueous solution is FeSO
47H
28 times of O solution obtain nanoscale Fe
0/ Fe
3O
4
In initial pH value is 6.0, and temperature of reaction is under 25 ℃ the condition, and to wherein adding 5mg Cr (VI), Cr (VI) clearance is 100% behind the reaction 5min.
Embodiment 3:
FeSO with 0.5mmol
47H
2O adds in the 400ml water, and passes into nitrogen removal dissolved oxygen, and duration of ventilation is 0.5h, adds then 0.5g Fe
3O
4, constantly passing into N
2And under the condition of continuous stirring, splash into 100mlNaBH
4The aqueous solution, NaBH
4The molar concentration of the aqueous solution is FeSO
47H
28 times of O solution obtain nanoscale Fe
0/ Fe
3O
4
In initial pH value is 6.0, and temperature of reaction is under 35 ℃ the condition, and to wherein adding 10mg Cr (VI), Cr (VI) clearance is 80% behind the reaction 120min.
Embodiment 4:
FeSO with 0.5mmol
47H
2O adds in the 400ml water, and passes into nitrogen removal dissolved oxygen, and duration of ventilation is 0.5h, adds then 0.75g Fe
3O
4, constantly passing into N
2And under the condition of continuous stirring, splash into 100mlNaBH
4The aqueous solution, NaBH
4The molar concentration of the aqueous solution is FeSO
47H
28 times of O solution obtain nanoscale Fe
0/ Fe
3O
4
In initial pH value is 6.0, and temperature of reaction is under 35 ℃ the condition, and to wherein adding 10mg Cr (VI), Cr (VI) clearance is 100% behind the reaction 120min.
Claims (2)
1. nanoscale Fe °/Fe
3O
4The preparation method, it is characterized in that: with the FeSO of 0.5～1mmol
47H
2O adds in the 400ml water, and logical nitrogen 0.5～1h removes dissolved oxygen then, adds 0.5～1.5gFe again
3O
4, constantly passing into N
2And under the condition of continuous stirring, splash into 100ml NaBH
4The aqueous solution, NaBH
4The initial molar concentration of the aqueous solution is FeSO
47H
28 times of O solution obtain nanoscale Fe °/Fe
3O
4
2. nanoscale Fe °/Fe of method preparation as claimed in claim 1
3O
4Purposes, it is characterized in that: be used for underground water and the chromic removal of waste water and reparation.
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|---|---|---|---|
| CNA2008100627417A CN101306862A (en) | 2008-07-01 | 2008-07-01 | Method for preparing nano-level Fe<0>/Fe3O4 and uses thereof |
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|---|---|---|---|
| CNA2008100627417A CN101306862A (en) | 2008-07-01 | 2008-07-01 | Method for preparing nano-level Fe<0>/Fe3O4 and uses thereof |
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|---|---|
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198314A (en) * | 2011-05-05 | 2011-09-28 | 中国地质大学（武汉） | Method for detoxifying and curing Cr(VI) by utilizing metakaolin-based geopolymer added with FeSO4.7H2O |
| CN102633345A (en) * | 2012-04-28 | 2012-08-15 | 常州亚环环保科技有限公司 | Method for treating high-concentration ammonia nitrogen in coal chemical wastewater |
| CN104827049A (en) * | 2015-02-11 | 2015-08-12 | 北京建筑大学 | Preparation method of zero-valent iron ball |
| CN105148915A (en) * | 2015-08-07 | 2015-12-16 | 武汉科技大学 | Fe3O4/Fe<0>/coke biomimetic catalyst capable of degrading POPs (persistent organic pollutants) and preparation method of catalyst |
| CN105197973A (en) * | 2015-09-09 | 2015-12-30 | 洛阳国兴矿业科技有限公司 | Method of utilizing low-quality bauxite to prepare aluminum oxide |
| CN105728426A (en) * | 2016-01-29 | 2016-07-06 | 厦门大学 | Method for promoting reduction of Cr(VI) in chromium core deposits by utilizing nano-material |
| CN105771148A (en) * | 2016-03-04 | 2016-07-20 | 华南师范大学 | Nanometer Fe<0>@Fe3O4 composite material and preparation method and application thereof |
| CN106669677A (en) * | 2017-01-05 | 2017-05-17 | 中国科学院新疆理化技术研究所 | Preparation method of magnetic iron-based heterogeneous Fenton catalyst taking graphene as carrier and application |
| CN109851144A (en) * | 2019-04-03 | 2019-06-07 | 南京大学 | It is a kind of to magnetize powder reinforced nitrate nitrogen and Phos minimizing technology |
| CN111453875A (en) * | 2020-02-28 | 2020-07-28 | 浙江工业大学 | Water treatment method for N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduction water |
| CN112279466A (en) * | 2020-10-28 | 2021-01-29 | 山西农业大学 | Method for treating acid mine wastewater by combining chemistry and microorganisms |
| CN114618493A (en) * | 2022-03-31 | 2022-06-14 | 中国科学院城市环境研究所 | Nano Fe0@Fe3O4Core-shell structure material and preparation method and application thereof |
-
2008
- 2008-07-01 CN CNA2008100627417A patent/CN101306862A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198314A (en) * | 2011-05-05 | 2011-09-28 | 中国地质大学（武汉） | Method for detoxifying and curing Cr(VI) by utilizing metakaolin-based geopolymer added with FeSO4.7H2O |
| CN102198314B (en) * | 2011-05-05 | 2012-05-30 | 中国地质大学（武汉） | Method for detoxifying and curing Cr(VI) by utilizing metakaolin-based geopolymer added with FeSO4.7H2O |
| CN102633345A (en) * | 2012-04-28 | 2012-08-15 | 常州亚环环保科技有限公司 | Method for treating high-concentration ammonia nitrogen in coal chemical wastewater |
| CN104827049A (en) * | 2015-02-11 | 2015-08-12 | 北京建筑大学 | Preparation method of zero-valent iron ball |
| CN105148915A (en) * | 2015-08-07 | 2015-12-16 | 武汉科技大学 | Fe3O4/Fe<0>/coke biomimetic catalyst capable of degrading POPs (persistent organic pollutants) and preparation method of catalyst |
| CN105197973A (en) * | 2015-09-09 | 2015-12-30 | 洛阳国兴矿业科技有限公司 | Method of utilizing low-quality bauxite to prepare aluminum oxide |
| CN105728426A (en) * | 2016-01-29 | 2016-07-06 | 厦门大学 | Method for promoting reduction of Cr(VI) in chromium core deposits by utilizing nano-material |
| CN105771148A (en) * | 2016-03-04 | 2016-07-20 | 华南师范大学 | Nanometer Fe<0>@Fe3O4 composite material and preparation method and application thereof |
| CN105771148B (en) * | 2016-03-04 | 2019-05-28 | 华南师范大学 | A kind of nanometer Fe0@Fe3O4Composite material and preparation method and application |
| CN106669677A (en) * | 2017-01-05 | 2017-05-17 | 中国科学院新疆理化技术研究所 | Preparation method of magnetic iron-based heterogeneous Fenton catalyst taking graphene as carrier and application |
| CN109851144A (en) * | 2019-04-03 | 2019-06-07 | 南京大学 | It is a kind of to magnetize powder reinforced nitrate nitrogen and Phos minimizing technology |
| CN109851144B (en) * | 2019-04-03 | 2021-09-28 | 南京大学 | Method for removing nitrate nitrogen and inorganic phosphorus strengthened by magnetized powder |
| CN111453875A (en) * | 2020-02-28 | 2020-07-28 | 浙江工业大学 | Water treatment method for N-nitrosodimethylamine in ferroferric oxide reinforced zero-valent iron reduction water |
| CN112279466A (en) * | 2020-10-28 | 2021-01-29 | 山西农业大学 | Method for treating acid mine wastewater by combining chemistry and microorganisms |
| CN114618493A (en) * | 2022-03-31 | 2022-06-14 | 中国科学院城市环境研究所 | Nano Fe0@Fe3O4Core-shell structure material and preparation method and application thereof |
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Open date: 20081119 |