CN104815610A - Adsorbent based on ferroferric oxide and nano zinc oxide and preparation method for adsorbent - Google Patents
Adsorbent based on ferroferric oxide and nano zinc oxide and preparation method for adsorbent Download PDFInfo
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- CN104815610A CN104815610A CN201510268939.0A CN201510268939A CN104815610A CN 104815610 A CN104815610 A CN 104815610A CN 201510268939 A CN201510268939 A CN 201510268939A CN 104815610 A CN104815610 A CN 104815610A
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Abstract
The invention discloses an adsorbent based on ferroferric oxide and nano zinc oxide and a preparation method for the adsorbent. The adsorbent based on ferroferric oxide and nano zinc oxide comprises two components, namely nano zinc oxide and ferroferric oxide in a mass ratio of 1:1 to 10:1, wherein ferroferric oxide is powdered. According to the invention, the process is simple, the raw materials are low in price, antibacterial and bacteriostatic, and the product is green, non-toxic and capable of being used for mass production. The adsorbent has high adsorption performance and superparamagnetism, can be used for efficiently adsorbing pollutants such as heavy metal ions, can perform quick separation through control of external magnetic fields, and has a direct application value in purifying heavy metal ions of industrial wastewater, river, sea and the like.
Description
[technical field]
The invention belongs to chemical material field, be specifically related to a kind of adsorbent based on tri-iron tetroxide and nano zine oxide and preparation method thereof.
[background technology]
Along with the development of globalization, heavy metal has caused global extensive concern to the pollution of water body, because their high in water intoxication, easy diffusions bring very large threat to the existence of the mankind.Due to the made rapid progress of industry, many industries are leather manufacture, metallurgy, battery production such as, containing multiple toxic heavy metal ion in a large amount of waste water that plating etc. produce.Adsorb and remove the method for water pollution as a kind of tradition and have some obvious advantages, as wide, easy and simple to handle in low cost, pH value range etc.But traditional ABSORBENTS ABSORPTION adsorption of metal ions effect is unsatisfactory, and separating technology is more complicated, easily introduces secondary pollution, recycles efficiency low.
The outstanding feature of Nano-class zinc oxide is that product pellet is nanoscale, has the double grading of nano material and conventional oxidation zinc simultaneously.Compared with conventional oxidation zinc product, its specific area is large, chemism is high, product fineness, chemical purity and shape of particle can adjust as required, and have Photochemical effects and cover ultraviolet performance preferably, and its UV-preventing rate is up to 98%;
Institute of Analysis of Tsing-Hua University transmission electron microscope is analyzed product, and nano zinc oxide particles is spherical, even particle size distribution, average grain diameter 20 ~ 30 nanometer, and the particle diameter of all particles is all below 50 nanometers.Through F-Sorb 3400 specific surface and the test of pore size determination instrument, the BET specific surface area of nanometer Zinc oxide powder is at more than 35m2/g.In addition, by adjustment preparation technology parameter, rod-like nano-zinc oxide can also be produced.This product is through Institute of Microorganism, Academia Sinica's Testing and appraisal, and result shows, is enriching in bacteria culture media, is adding the nano zine oxide of 0.5% ~ 1%, and can effectively suppress colibacillary growth, bacteriostasis rate reaches more than 99.9%.Meanwhile, it also there is antibacterial bacteriostatic, a series of special performances such as the anti-enzyme of taste of dispelling.
By long-term experimental study, we find, the two-dimensional nano zinc oxide material of extra specific surface area can be adsorbed with organic dye, greasy dirt and heavy metal ion fast and efficiently, but the separation after absorption needs to depend on centrifugal or precipitation, not only complex process, cost is high, very time-consuming.Application magnetic separation technique is the ideal scheme of sewage adsorption cleaning process, but nano zine oxide itself does not possess magnetic, to have ferromagnetic ferroferric oxide nano granules is compound on nano zine oxide, makes it have stable superparamagnetism, is a creationary thinking.The composite magnetic adsorbent that ferroferric oxide nano granules is bundled in surface of nanometer zinc oxide evenly, dispersedly not only has the high absorption property of nano zine oxide, and there is the superparamagnetism of ferroferric oxide nano granules, can either the pollutant such as Adsorption of Heavy Metal Ions efficiently, again can fast response external magnetic field regulation and control be separated, be expected to there is huge application prospect in industrial waste water purifying disposal.But up to the present, do not report the application function that tri-iron tetroxide and the process of nano-zinc oxide composite material heavy metal waste water adsorption cleaning are discussed, the preparation scheme of its composite construction is not also in the news.
Adsorbent that a kind of adsorption efficiency of current shortage is high and preparation method thereof.
[summary of the invention]
Technical problem to be solved by this invention there is provided high adsorbent of a kind of adsorption efficiency and preparation method thereof.
To achieve these goals, the present invention is achieved through the following technical solutions: a kind of adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, adsorbent based on tri-iron tetroxide and nano zine oxide is made up of nano zine oxide and tri-iron tetroxide two kinds of components, wherein, nano zine oxide and tri-iron tetroxide mass ratio are 1:1-10:1, and described tri-iron tetroxide is Powdered.
Further, described nano zine oxide and tri-iron tetroxide mass ratio are 5:1.
Further, described nano zine oxide is 80mg; Described tri-iron tetroxide is 8-80mg.
Prepare the method for the adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, comprise the steps:
(1) nano zine oxide and tri-iron tetroxide is taken respectively according to proportioning; Nano zine oxide is added in deionized water and configures the aqueous solution, and magnetic agitation is even at normal temperatures;
(2) tri-iron tetroxide is added, obtain nano zine oxide respectively and tri-iron tetroxide mass ratio is the mixed solution of 1:1-10:1, after ultrasonic abundant mixing dispersion, pour in reactor and react, progressively heat up, being heated to temperature is 250-300 DEG C, keeps temperature stabilization, reaction 1-3h, obtains product;
(3) product deionized water is obtained and alcohol washs, when temperature is 60-80 DEG C, vacuum drying 10-15h, the obtained adsorbent based on tri-iron tetroxide and nano zine oxide.
Further, in step (1), weigh nano zine oxide 80mg and add in deionized water and configure the 40ml aqueous solution, and magnetic agitation 2-3h at normal temperatures; In step (2), add 8-80mg tri-iron tetroxide, after the ultrasonic abundant mixing dispersion of 1-2h, heating rate is 8-20 DEG C/min.
Further, in step (1), the equipment that described magnetic agitation uses is six magnetic stirring apparatus; Described ultrasonic equipment used in combination is numerical control ultrasonic cleaner.
Adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention is as the application of Adsorption of Heavy Metal Ions.
Further, described heavy metal ion is mercury ion or cadmium ion or chromium ion.
Beneficial effect: present invention process is simple and easy, low in raw material price, antibacterial bacteriostatic, and Product Green is nontoxic, can be mass.The present invention not only has high absorption property but also have superparamagnetism, can the pollutant such as Adsorption of Heavy Metal Ions efficiently, and quick separating can be carried out by external magnetic field manipulation, in the purified treatment of the heavy metal ion of industrial wastewater, rivers, ocean etc., there is direct using value.Tool of the present invention has the following advantages:
(1) the separable adsorbent of the magnetic of tri-iron tetroxide and nano zine oxide compound has very strong Adsorption of Heavy Metal Ions and the ability of organic dyestuff, and can it be separated from water body by external magnetic field fast.It has potential application in many aspects: replace traditional adsorbent can have better adsorption effect with this compound.
(2) the present invention uses hydro-thermal method, and it is simple that hydro-thermal method has technique, can mass, and condition is easy to control, the advantage that repeatability is high.In the process of hydrothermal reduction nano zine oxide, achieve being incorporated to of tri-iron tetroxide, simultaneously by the control of component, achieve the single dispersing ground embedded compound of tri-iron tetroxide in nano zine oxide, such structure can stop oxidation and the corrosion of tri-iron tetroxide effectively, add specific area simultaneously, be more conducive to adsorption fouling thing molecule.
[accompanying drawing explanation]
Fig. 1 is the stereoscan photograph of tri-iron tetroxide of the present invention and nano zine oxide compound Magneto separate adsorbent;
Fig. 2 is the digital photograph mixed with adsorbent before Adsorption of Heavy Metals mercury ion of the present invention;
Fig. 3 is the digital photograph after Adsorption of Heavy Metals mercury ion Magneto separate of the present invention.
[detailed description of the invention]
Further specific descriptions will be done with specific embodiment to the present invention in conjunction with the drawings below, but can not be interpreted as it is limiting the scope of the present invention.
Embodiment 1
As shown in Figure 1, for stereoscan photograph display ferriferrous oxide nano sphere be dispersed on nano zine oxide, pattern and size more homogeneous, define composite construction.Fig. 2 is the digital photograph mixed with adsorbent before Adsorption of Heavy Metals mercury ion of the present invention; Fig. 3 is the digital photograph after Adsorption of Heavy Metals mercury ion Magneto separate of the present invention.As Fig. 2 and Fig. 3 is known, the adsorption effect of adsorbent of the present invention is obvious, and adsorption efficiency is high.
A kind of adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, adsorbent based on tri-iron tetroxide and nano zine oxide is made up of nano zine oxide and tri-iron tetroxide two kinds of components, wherein, nano zine oxide and tri-iron tetroxide mass ratio are 1:1, and described tri-iron tetroxide is Powdered.
Described nano zine oxide is 80mg; Described tri-iron tetroxide is 80mg.
Prepare the ferroferric oxide nano granules that pattern is homogeneous.Obtain black ferroferric oxide nanosphere powder preparation nano zine oxide.
Prepare the method for the adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, comprise the steps:
(1) nano zine oxide and tri-iron tetroxide is taken respectively according to proportioning; Nano zine oxide is added in deionized water and configures the aqueous solution, and magnetic agitation is even at normal temperatures; Weigh nano zine oxide 80mg to add in deionized water and configure the 40ml aqueous solution, and magnetic agitation 2h at normal temperatures; The equipment that described magnetic agitation uses is six magnetic stirring apparatus; Described ultrasonic equipment used in combination is numerical control ultrasonic cleaner.Want evenly when nano zine oxide mixes with tri-iron tetroxide; heating rate can not be too fast; material proportion will strictly control; so just can obtain Embedded composite construction; instead of bulk deposition is on surface; embedded composite construction could really protect tri-iron tetroxide not easily oxidized effectively, and can effectively stop tri-iron tetroxide to corrode in acid condition.
(2) tri-iron tetroxide is added, obtain nano zine oxide respectively and tri-iron tetroxide mass ratio is the mixed solution of 1:1, after ultrasonic abundant mixing dispersion, pour in reactor and react, progressively heat up, being heated to temperature is 250-300 DEG C, keeps temperature stabilization, reaction 1h, obtains product; Add 80mg tri-iron tetroxide, after the ultrasonic abundant mixing dispersion of 1h, heating rate is 8 DEG C/min.
(3) product deionized water is obtained and alcohol washs, when temperature is 60 DEG C, vacuum drying 10h, the obtained adsorbent based on tri-iron tetroxide and nano zine oxide.
Adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention is as the application of Adsorption of Heavy Metal Ions.
Described heavy metal ion is mercury ion.
The size of tri-iron tetroxide of the present invention, tamped density and uniformity directly affect absorption property and the magnetic of composite, and therefore in above-mentioned production process, the experiment condition such as reaction temperature, reaction time, material molar ratio needs strict control.
Present invention process is simple and easy, low in raw material price, antibacterial bacteriostatic, and Product Green is nontoxic, can be mass.The present invention not only has high absorption property but also have superparamagnetism, can the pollutant such as Adsorption of Heavy Metal Ions efficiently, and quick separating can be carried out by external magnetic field manipulation, in the purified treatment of the heavy metal ion of industrial wastewater, rivers, ocean etc., there is direct using value.Tool of the present invention has the following advantages:
(1) the separable adsorbent of the magnetic of tri-iron tetroxide and nano zine oxide compound has very strong Adsorption of Heavy Metal Ions and the ability of organic dyestuff, and can it be separated from water body by external magnetic field fast.It has potential application in many aspects: replace traditional adsorbent can have better adsorption effect with this compound.
(2) the present invention uses hydro-thermal method, and it is simple that hydro-thermal method has technique, can mass, and condition is easy to control, the advantage that repeatability is high.In the process of hydrothermal reduction nano zine oxide, achieve being incorporated to of tri-iron tetroxide, simultaneously by the control of component, achieve the single dispersing ground embedded compound of tri-iron tetroxide in nano zine oxide, such structure can stop oxidation and the corrosion of tri-iron tetroxide effectively, add specific area simultaneously, be more conducive to adsorption fouling thing molecule.
Embodiment 2
Embodiment 2 is with the difference of embodiment 1: a kind of adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, adsorbent based on tri-iron tetroxide and nano zine oxide is made up of nano zine oxide and tri-iron tetroxide two kinds of components, wherein, described tri-iron tetroxide is Powdered.
Described nano zine oxide and tri-iron tetroxide mass ratio are 5:1.Now the present invention has best adsorption capacity, also has larger magnetic, is beneficial to Magnetic Isolation.
Described nano zine oxide is 80mg; Described tri-iron tetroxide is 16mg.
Prepare the method for the adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, comprise the steps:
(1) nano zine oxide and tri-iron tetroxide is taken respectively according to proportioning; Nano zine oxide is added in deionized water and configures the aqueous solution, and magnetic agitation is even at normal temperatures; Weigh nano zine oxide 80mg to add in deionized water and configure the 40ml aqueous solution, and magnetic agitation 2.5h at normal temperatures; The equipment that described magnetic agitation uses is six magnetic stirring apparatus; Described ultrasonic equipment used in combination is numerical control ultrasonic cleaner.Want evenly when nano zine oxide mixes with tri-iron tetroxide; heating rate can not be too fast; material proportion will strictly control; so just can obtain Embedded composite construction; instead of bulk deposition is on surface; embedded composite construction could really protect tri-iron tetroxide not easily oxidized effectively, and can effectively stop tri-iron tetroxide to corrode in acid condition.
(2) add tri-iron tetroxide, obtain nano zine oxide respectively and tri-iron tetroxide mass ratio is the mixed solution of 5:1, after ultrasonic abundant mixing dispersion, pour in reactor and react, progressively heat up, being heated to temperature is 280 DEG C, keep temperature stabilization, reaction 2h, obtains product; Add 16mg tri-iron tetroxide, after the ultrasonic abundant mixing dispersion of 1.5h, heating rate is 16 DEG C/min.
(3) product deionized water is obtained and alcohol washs, when temperature is 70 DEG C, vacuum drying 13h, the obtained adsorbent based on tri-iron tetroxide and nano zine oxide.
Embodiment 3
Embodiment 3 is with the difference of embodiment 1: a kind of adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, adsorbent based on tri-iron tetroxide and nano zine oxide is made up of nano zine oxide and tri-iron tetroxide two kinds of components, wherein, nano zine oxide and tri-iron tetroxide mass ratio are 10:1, and described tri-iron tetroxide is Powdered.
Described nano zine oxide is 80mg; Described tri-iron tetroxide is 8mg.
Prepare the method for the adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, comprise the steps:
(1) nano zine oxide and tri-iron tetroxide is taken respectively according to proportioning; Nano zine oxide is added in deionized water and configures the aqueous solution, and magnetic agitation is even at normal temperatures; Weigh nano zine oxide 80mg to add in deionized water and configure the 40ml aqueous solution, and magnetic agitation 3h at normal temperatures; The equipment that described magnetic agitation uses is six magnetic stirring apparatus; Described ultrasonic equipment used in combination is numerical control ultrasonic cleaner.Want evenly when nano zine oxide mixes with tri-iron tetroxide; heating rate can not be too fast; material proportion will strictly control; so just can obtain Embedded composite construction; instead of bulk deposition is on surface; embedded composite construction could really protect tri-iron tetroxide not easily oxidized effectively, and can effectively stop tri-iron tetroxide to corrode in acid condition.
(2) add tri-iron tetroxide, obtain nano zine oxide respectively and tri-iron tetroxide mass ratio is the mixed solution of 10:1, after ultrasonic abundant mixing dispersion, pour in reactor and react, progressively heat up, being heated to temperature is 300 DEG C, keep temperature stabilization, reaction 3h, obtains product; Add 8mg tri-iron tetroxide, after the ultrasonic abundant mixing dispersion of 1-2h, heating rate is 20 DEG C/min.
(3) product deionized water is obtained and alcohol washs, when temperature is 80 DEG C, vacuum drying 15h, the obtained adsorbent based on tri-iron tetroxide and nano zine oxide.
Embodiment 4
Embodiment 4 is with the difference of embodiment 1: described heavy metal ion is cadmium ion.
Embodiment 5
Embodiment 5 is with the difference of embodiment 1: described heavy metal ion is chromium ion.
Test 1
Be used in experiment 1 by embodiment 1 based on the adsorbent of tri-iron tetroxide and nano zine oxide, in lecture experiment, we have prepared the aqueous solution of 0.142mol/l mercury ion, namely Hg2+ ion concentration is 30mg/l, the nano zine oxide adopting above scheme to obtain and tri-iron tetroxide compound adsorbent 100mg add in the Hg2+ deionized water solution of preparation, wherein nano zine oxide and tri-iron tetroxide mass ratio are that the sample of 5:1 represents best adsorption effect, Hg2+ ion remaval rate reaches 96%, and it has stable magnetic, the Magneto separate of express delivery can be realized under the effect of one block of magnet.
As shown in Figures 2 and 3, be that before absorption, potassium bichromate solution is yellow, becomes the turbid solution of brown after adding adsorbent; After absorption Magneto separate completes, become the aqueous solution of clear.
Can prove according to above test, with the adsorbent based on tri-iron tetroxide and nano zine oxide of the present invention, the present invention not only has high absorption property but also have superparamagnetism, can the heavy-metal pollution thing such as the aqueous solution of Adsorption of Mercury ion efficiently, and quick separating can be carried out by external magnetic field manipulation.
More than show and describe general principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and application claims protection domain is defined by appending claims, description and equivalent thereof.
Claims (8)
1. the adsorbent based on tri-iron tetroxide and nano zine oxide, it is characterized in that: the adsorbent based on tri-iron tetroxide and nano zine oxide is made up of nano zine oxide and tri-iron tetroxide two kinds of components, wherein, nano zine oxide and tri-iron tetroxide mass ratio are 1:1-10:1, and described tri-iron tetroxide is Powdered.
2. the adsorbent based on tri-iron tetroxide and nano zine oxide according to claim 1, is characterized in that: described nano zine oxide and tri-iron tetroxide mass ratio are 5:1.
3. the adsorbent based on tri-iron tetroxide and nano zine oxide according to claim 2, is characterized in that: described nano zine oxide is 80mg; Described tri-iron tetroxide is 8-80mg.
4. the method for the preparation adsorbent based on tri-iron tetroxide and nano zine oxide according to claim 1, is characterized in that comprising the steps:
(1) nano zine oxide and tri-iron tetroxide is taken respectively according to proportioning; Nano zine oxide is added in deionized water and configures the aqueous solution, and magnetic agitation is even at normal temperatures;
(2) tri-iron tetroxide is added, obtain nano zine oxide respectively and tri-iron tetroxide mass ratio is the mixed solution of 1:1-10:1, after ultrasonic abundant mixing dispersion, pour in reactor and react, progressively heat up, being heated to temperature is 250-300 DEG C, keeps temperature stabilization, reaction 1-3h, obtains product;
(3) product deionized water is obtained and alcohol washs, when temperature is 60-80 DEG C, vacuum drying 10-15h, the obtained adsorbent based on tri-iron tetroxide and nano zine oxide.
5. the method for the adsorbent based on tri-iron tetroxide and nano zine oxide according to claim 4, is characterized in that:
In step (1), weigh nano zine oxide 80mg and add in deionized water and configure the 40ml aqueous solution, and magnetic agitation 2-3h at normal temperatures; In step (2), add 8-80mg tri-iron tetroxide, after the ultrasonic abundant mixing dispersion of 1-2h, heating rate is 8-20 DEG C/min.
6. the method for the adsorbent based on tri-iron tetroxide and nano zine oxide according to claim 5, is characterized in that: in step (1), and the equipment that described magnetic agitation uses is six magnetic stirring apparatus; Described ultrasonic equipment used in combination is numerical control ultrasonic cleaner.
7. the adsorbent based on tri-iron tetroxide and nano zine oxide according to any one of claim 1-6 is as the application of Adsorption of Heavy Metal Ions.
8. application according to claim 7, is characterized in that: described heavy metal ion is mercury ion or cadmium ion or chromium ion.
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| CN109468837A (en) * | 2018-11-01 | 2019-03-15 | 深圳市润海源通科技有限公司 | Deodorization antibiotic agent and its application |
| JP2020116501A (en) * | 2019-01-22 | 2020-08-06 | 三井金属鉱業株式会社 | Method of removing mercury in smoke effluent |
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| CN101680120A (en) * | 2007-04-11 | 2010-03-24 | 新加坡国立大学 | fibers for decontamination of chemical and biological agents |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109468837A (en) * | 2018-11-01 | 2019-03-15 | 深圳市润海源通科技有限公司 | Deodorization antibiotic agent and its application |
| JP2020116501A (en) * | 2019-01-22 | 2020-08-06 | 三井金属鉱業株式会社 | Method of removing mercury in smoke effluent |
| JP7110128B2 (en) | 2019-01-22 | 2022-08-01 | 三井金属鉱業株式会社 | Method for removing mercury in smoke washing wastewater |
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