CN102674469A - Nanometer magnetic iron oxide and preparation method and application thereof - Google Patents

Nanometer magnetic iron oxide and preparation method and application thereof Download PDF

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Publication number
CN102674469A
CN102674469A CN2012101411327A CN201210141132A CN102674469A CN 102674469 A CN102674469 A CN 102674469A CN 2012101411327 A CN2012101411327 A CN 2012101411327A CN 201210141132 A CN201210141132 A CN 201210141132A CN 102674469 A CN102674469 A CN 102674469A
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arsenic
fecl
water
ferriferous oxide
sorbent material
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CN102674469B (en
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林森
卢滇楠
刘铮
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Tsinghua University
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Tsinghua University
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Abstract

The invention discloses nanometer magnetic iron oxide and a preparation method and application thereof. The method comprises the following steps of: uniformly mixing FeCl3, FeCl2 and a pH value mutagen in a solvent for reaction, and thus obtaining the iron oxide after the reaction. According to the method, an adsorbent can be quickly prepared at normal temperature under a high-speed stirring condition by a method for quickly changing the pH value of the prepared liquor by using 25 percent ammonia water. An arsenic adsorbent prepared by the method has a series of advantages of simple preparation process, low cost, high adsorption quantity, high adsorption speed, low influences of aqueous environments, recycling simplicity and the like which contribute to industrial application.

Description

Nano magnetic ferrite thing and preparation method thereof and application
Technical field
The invention belongs to the Environmental Water process field, relate to a kind of nano magnetic ferrite thing and preparation method thereof and application.
Background technology
Arsenic element has storage effect in animal and plant body, and the people is had the serious harm of " carcinogenic, teratogenesis shape, mutagenesis ".Even a spot of arsenic accumulates, also can cause skin ulceration, hypertension, various diseases such as keratinization in human body.Total arsenic content can not surpass 0.01mg/L in World Health Organization's regulation tap water, and total arsenic content can not surpass 0.5mg/L in the industrial discharge waste water.According to this standard, the many geographic people in the whole world are suffering by the murder by poisoning of the water of arsenic contamination, such as; Bangladesh, Vietnam, Mongolia; India, Chile etc., wherein serious with Bangladesh; Because the region, almost the content of arsenic all exceeds standard in the waters of whole country, and the population above 8,000 ten thousand is suffering the murder by poisoning of arsenic contamination.And the situation of China also allows of no optimist, owing to open a mine, and arsenic content overproof in the water in many zones, ground such as Shanxi, the highest even up to 4.8mg/L, the value of being above standard hundreds of times.Therefore, the improvement for arsenic contamination is very urgent.
The method of administering arsenic contamination in the water at present mainly can be divided into six big types: chemical precipitation method, electrolytic process, membrane separation process, ion exchange method, living body biological method, absorption method.In these methods, be most widely used with absorption method.But the various sorbent materials to water arsenic have the subsequent recovery difficulty at present, are prone to cause secondary pollution, and the not high defective of adsorptive capacity is unfavorable for industriallization and extensive waste water treatment.
Summary of the invention
The purpose of this invention is to provide a kind of nano magnetic ferrite thing and preparation method thereof and application.
The method for preparing ferriferous oxide provided by the invention comprises the steps: FeCl 3, FeCl 2Prominent with the pH value
Become agent mixing in solvent and react, reaction finishes and obtains said ferriferous oxide.
In the aforesaid method, said FeCl 3With FeCl 2Molar ratio be 2 ~ 2.4: 1;
The consumption of said solvent is for making said FeCl 2Concentration be 25 ~ 40mmol/L;
Agent of said pH value mutation and FeCl 2Amount ratio be 6.5 ~ 8ml:1mmol, be specially 7.5ml: 1mmol or 7.7ml: 1mmol;
The agent of said pH value mutation is an ammoniacal liquor; The mass percentage concentration of said ammoniacal liquor is 25-35%, preferred 25%.
Said solvent is a water;
In the said mixing step, blending manner is a stirring and evenly mixing.
In the said stirring and evenly mixing, rotating speed is 500-2000rmp, preferred 1000rmp; In the said reactions step, temperature is a room temperature, and the time is 20-30 minute.
The said method for preparing ferriferous oxide also comprises the steps: after said reaction finishes, products therefrom to be adsorbed with magnet, makes itself and liquid phase separation, uses water washing again;
In the said washing step, the consumption of water is the said FeCl of 1mmol 2The said water of corresponding 100 ~ 150ml, washing times is 3-5 time.
The colloidal solution that ferriferous oxide that the method for utilizing the invention described above to provide prepares or the ferriferous oxide that is obtained by method for preparing and water are formed also belongs to protection scope of the present invention.Wherein, the particle diameter of said ferriferous oxide is 8-12nm.
In addition, ferriferous oxide that the invention described above provides or colloidal solution also belong to protection scope of the present invention at application and the arsenic sorbent material that contains this ferriferous oxide or colloidal solution of absorption in the arsenic compound.Wherein, the valence state of arsenic is trivalent or pentavalent in the said arsenic compound; The valence state that said arsenic sorbent material is an arsenic-adsorbing is the arsenic compound of trivalent or pentavalent; In the said adsorption step, medium is a water, is specially sewage; The working medium of said arsenic sorbent material is a water, is specially sewage.In the said adsorption step, the pH value that contains the system of arsenic compound is 1-14, is specially 2.5-12.
The present invention reaches the purpose of purifying waste water with the arsenic element of nano-scale magnetic iron oxide particle as different valence state (trivalent and pentavalent) in the sorbent material removal sewage.This arsenic sorbent material has preparation simply, and adsorptive capacity is big, and rate of adsorption is fast, and it is little influenced by aqueous environment, is easy to series of advantages such as recovery, extremely is fit to the processing of extensive water arsenic contamination, and the utmost point is beneficial to industrial applications, has important use and is worth.
Description of drawings
The transmission electron microscope picture of the nano-scale magnetic iron oxide particle sorbent material that Fig. 1 makes for embodiment 1.
Fig. 2 is the photo of the nano-scale magnetic iron oxide particle that uses magnet recovery embodiment 1 and make.
The X-ray diffractogram (XRD) of the nano-scale magnetic iron oxide particle sorbent material that Fig. 3 makes for embodiment 1.
The hysteresis curve of the nano-scale magnetic iron oxide particle sorbent material that Fig. 4 makes for embodiment 1.
Embodiment
Below in conjunction with specific embodiment the present invention is done further elaboration, but the present invention is not limited to following examples.Said method is ordinary method if no special instructions.Said starting material all can get from open commercial sources if no special instructions.The concentration of said ammoniacal liquor is mass percentage concentration.
Embodiment 1
FeCl with 2mmol 3With 1mmol FeCl 2Add in the distilled water of 30ml, under the stirring of 1000rpm, add the ammoniacal liquor of 7.5ml 25% fast, stirring at room reaction 20min uses magnet that reaction product is adsorbed, and with liquid phase separation, with deionized water wash 3 times, the products therefrom yield is 98.4%.
The particle diameter of this product is between 8-12nm; Accompanying drawing 1 is the transmission electron microscope picture (TEM) of the nano-scale magnetic iron oxide particle that makes; Accompanying drawing 2 reclaims the photo of the nano-scale magnetic iron oxide particle that makes for using magneticstrength as the permanent magnet of 0.5T; Accompanying drawing 3 is the X-ray diffractogram (XRD) of the nano-scale magnetic iron oxide particle sorbent material that makes, and accompanying drawing 4 is the hysteresis curve of the nano-scale magnetic iron oxide particle sorbent material that makes.By on can know that this product structure is correct, be the nano-scale magnetic ferriferous oxide.
Embodiment 2
FeCl with 10mmol 3With 5mmol FeCl 2Add in the distilled water of 150ml, under the stirring of 1000rpm, add the ammoniacal liquor of 38.5ml 25% fast; Stirring at room reaction 20min uses magnet that reaction product is adsorbed, with liquid phase separation; With deionized water wash 3 times, the products therefrom yield is 98.9%, and the particle diameter of this product is 8-12nm.
Embodiment 3
FeCl with 20mmol 3With 10mmol FeCl 2Add in the distilled water of 300ml, under the stirring of 1000rpm, add the ammoniacal liquor of 77ml 25% fast; Stirring at room reaction 20min uses magnet that reaction product is adsorbed, with liquid phase separation; With deionized water wash 3 times, the products therefrom yield is 96.8%, and the particle diameter of this product is 8-12nm.
Embodiment 4
FeCl with 50mmol 3With 25mmol FeCl 2Add in the distilled water of 750ml, under the stirring of 1000rpm, add the ammoniacal liquor of 192.5ml 25% fast; Stirring reaction 20min uses magnet that reaction product is adsorbed, with liquid phase separation; With deionized water wash 3 times, the products therefrom yield is 97.4%, and the particle diameter of this product is 8-12nm.
Embodiment 5
FeCl with 2.2mmol 3With 1mmol FeCl 2Add in the distilled water of 30ml, under the stirring of 1000rpm, add the ammoniacal liquor of 7.5ml 25% fast; Stirring at room reaction 20min uses magnet that reaction product is adsorbed, with liquid phase separation; With deionized water wash 3 times, the products therefrom yield is 94.2%, and the particle diameter of this product is 8-12nm.
Embodiment 6
FeCl with 2.4mmol 3With 1mmol FeCl 2Add in the distilled water of 30ml, under the stirring of 1000rpm, add the ammoniacal liquor of 7.5ml 25% fast; Stirring reaction 20min uses magnet that reaction product is adsorbed, with liquid phase separation; With deionized water wash 3 times, the products therefrom yield is 93.1%, and the particle diameter of this product is 8-12nm.
Embodiment 7
FeCl with 20mmol 3With 10mmol FeCl 2Add in the distilled water of 300ml, under the stirring of 1000rpm, add the ammoniacal liquor of 77ml 25% fast; Stirring at room reaction 20min uses magnet that reaction product is adsorbed, with liquid phase separation; With deionized water wash 3 times, the products therefrom yield is 96.8%, and the particle diameter of this product is 8-12nm.
Embodiment 8
1mmol embodiment 1 preparation gained sorbent material is added 100ml, pH value=4 ~ 9, the starting point concentration of As is the NaH of 100ppm 2AsO 3In the solution, 30 ℃, behind the reaction 60min, arsenious clearance is higher than 99.61% in the solution under the concussion condition of 175rpm, and residual concentration is lower than 0.39ppm, is limited to the arsenic content emission standard of 0.5ppm on meeting in the national waste water.
Embodiment 9
0.5mmol embodiment 1 preparation gained sorbent material is added 100ml, pH value=4 ~ 9, the starting point concentration of As is the NaH of 100ppm 2AsO 3In the solution, 30 ℃, behind the reaction 60min, arsenious clearance is higher than 75.51% in the solution under the concussion condition of 175rpm, and residual concentration is lower than 24.49ppm.
Embodiment 10
0.5mmol embodiment 1 preparation gained sorbent material is added 100ml, pH value=2.5 ~ 7.0, the starting point concentration of As is the NaH of 100ppm 2AsO 4In the solution, 30 ℃, behind the reaction 60min, arsenious clearance is higher than 97.41% in the solution under the concussion condition of 175rpm, and residual concentration is lower than 2.59ppm.
Embodiment 11
1mmol embodiment 1 preparation gained sorbent material is added 100ml, pH value=2.5 ~ 7.0, the starting point concentration of As is the NaH of 100ppm 2AsO 4In the solution, 30 ℃, behind the reaction 60min, arsenious clearance is higher than 99.81% in the solution under the concussion condition of 175rpm, and residual concentration is lower than 0.19ppm, is limited to the arsenic content emission standard of 0.5ppm on meeting in the national waste water.
Embodiment 12
Respectively 0.5mmol embodiment 1 preparation gained sorbent material is added the SO that contains 50mmol/L respectively 4 2-, NO 3 -, Cl -100ml, pH value=7.5, the As starting point concentration is 100ppmNaH 2AsO 4In the solution, at 30 ℃, behind the reaction 60min, arsenious concentration is respectively 18.01ppm in the solution, 17.14ppm and 19.44ppm under the concussion condition of 175rpm.
Embodiment 13
Respectively 0.5mmol embodiment 1 preparation gained sorbent material is added the SO that contains 50mmol/L respectively 4 2-, NO 3 -, Cl -100ml, pH value=3.2, the As starting point concentration is 100ppmNaH 2AsO 4In the solution, at 30 ℃, behind the reaction 60min, arsenious concentration is respectively 0.11ppm in the solution, 0.04ppm and 0.19ppm under the concussion condition of 175rpm.
Embodiment 14
1mmol embodiment 1 preparation gained sorbent material is added 100ml; Total arsenic content is 110.4ppm, and original pH value value is 12.7, and COD is in the actual waste water of 1165mg/L from certain army; At 30 ℃; Behind the reaction 60min, the residual concentration of arsenic is 33.42ppm in the solution under the concussion condition of 175rpm, and clearance reaches 66.58%.
Embodiment 15
1mmol embodiment 1 preparation gained sorbent material is added 100ml, and the pH value is adjusted to 5.0, and total arsenic content is 110.4ppm; COD is in the actual waste water of 1165mg/L from certain army; At 30 ℃, behind the reaction 60min, the clearance of arsenic reaches 99.64% in the solution under the concussion condition of 175rpm; Residual concentration is 0.36ppm, is limited to the arsenic content emission standard of 0.5ppm on meeting in the national waste water.

Claims (10)

1. a method for preparing ferriferous oxide comprises the steps: FeCl 3, FeCl 2React with pH value mutation agent mixing in solvent, reaction finishes and obtains said ferriferous oxide.
2. method according to claim 1 is characterized in that: said FeCl 3With FeCl 2Molar ratio be 2 ~ 2.4: 1;
Agent of said pH value mutation and FeCl 2Amount ratio be 6.5 ~ 8ml: 1mmol;
The consumption of said solvent is for making said FeCl 2Concentration be 25 ~ 40mmol/L;
In the said mixing step, blending manner is a stirring and evenly mixing.
3. method according to claim 2 is characterized in that: in the said stirring and evenly mixing, rotating speed is 500-2000rmp, preferred 1000rmp;
In the said reactions step, temperature is a room temperature, and the time is 20-30 minute.
4. according to the arbitrary described method of claim 2-3, it is characterized in that: said solvent is a water;
The agent of said pH value mutation is an ammoniacal liquor;
The mass percentage concentration of said ammoniacal liquor is 25-35%, preferred 25%.
5. according to the arbitrary described method of claim 1-4, it is characterized in that: the said method for preparing ferriferous oxide also comprises the steps: after said reaction finishes, products therefrom to be adsorbed with magnet, makes itself and liquid phase separation, uses water washing again;
In the said washing step, the consumption of water is the said FeCl of 1mmol 2The said water of corresponding 100 ~ 150ml, washing times is 3-5 time.
6. the colloidal solution formed of the ferriferous oxide for preparing of the arbitrary said method of claim 1-5 or the ferriferous oxide for preparing by the arbitrary said method of claim 1-5 and water.
7. ferriferous oxide according to claim 6 or colloidal solution is characterized in that: the particle diameter of said ferriferous oxide is 8-12nm.
8. claim 6 or 7 said ferriferous oxides or the colloidal solution application in the absorption arsenic compound.
9. the arsenic sorbent material that contains claim 6 or 7 said ferriferous oxides or colloidal solution.
10. the described arsenic sorbent material of application according to claim 8 or claim 9 is characterized in that: the valence state of arsenic is trivalent or pentavalent in the said arsenic compound; The valence state that said arsenic sorbent material is an arsenic-adsorbing is the arsenic compound of trivalent or pentavalent;
In the said adsorption step, medium is a water, is specially sewage;
The working medium of said arsenic sorbent material is a water, is specially sewage;
In the said adsorption step, the pH value that contains the system of arsenic compound is 1-14, is specially 2.5-12.
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CN103464089A (en) * 2013-09-11 2013-12-25 清华大学 Magnetic arsenic adsorbent as well as preparation method and application thereof
CN103933928A (en) * 2014-04-04 2014-07-23 无锡普爱德环保科技有限公司 Dehumidification adsorbent and preparation method thereof
CN104341010A (en) * 2013-07-25 2015-02-11 同济大学 Method for synthesizing superparamagnetic ferroferric oxide nano-sheets
CN108620034A (en) * 2018-05-22 2018-10-09 华东理工大学 A kind of preparation method of gel embedding type effectively removing arsenic material
CN110102264A (en) * 2019-06-04 2019-08-09 太原理工大学 A kind of preparation of superelevation magnetic responsiveness nanocluster microballoon and wastewater treatment method

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104341010A (en) * 2013-07-25 2015-02-11 同济大学 Method for synthesizing superparamagnetic ferroferric oxide nano-sheets
CN104341010B (en) * 2013-07-25 2016-05-18 同济大学 A kind of method of synthetic SPIO nanometer sheet
CN103464089A (en) * 2013-09-11 2013-12-25 清华大学 Magnetic arsenic adsorbent as well as preparation method and application thereof
CN103464089B (en) * 2013-09-11 2015-10-28 清华大学 Magnetic arsenic adsorbent and preparation method thereof and application
CN103933928A (en) * 2014-04-04 2014-07-23 无锡普爱德环保科技有限公司 Dehumidification adsorbent and preparation method thereof
CN108620034A (en) * 2018-05-22 2018-10-09 华东理工大学 A kind of preparation method of gel embedding type effectively removing arsenic material
CN110102264A (en) * 2019-06-04 2019-08-09 太原理工大学 A kind of preparation of superelevation magnetic responsiveness nanocluster microballoon and wastewater treatment method
CN110102264B (en) * 2019-06-04 2021-03-02 太原理工大学 Preparation of ultra-high magnetic responsiveness nanocluster microspheres and wastewater treatment method

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