CN103480323A - Method for realizing one-step synthesis of ferroferric oxide microspheres having hierarchical structure and application method of product thereof - Google Patents
Method for realizing one-step synthesis of ferroferric oxide microspheres having hierarchical structure and application method of product thereof Download PDFInfo
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- CN103480323A CN103480323A CN201310396313.9A CN201310396313A CN103480323A CN 103480323 A CN103480323 A CN 103480323A CN 201310396313 A CN201310396313 A CN 201310396313A CN 103480323 A CN103480323 A CN 103480323A
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Abstract
The invention relates to a method for realizing one-step synthesis of ferroferric oxide microspheres having a hierarchical structure and an application method of a product thereof. The method comprises the following steps: dissolving ferric salt and sodium acetate trihydrate in a certain amount of ethylene glycol, adding 10 milliliters of dodecanethiol into the mixed solution, and stirring to obtain a suspension; and heating at 180 DEG C for 8 hours, cooling, and washing. Compared with the prior art, the dodecanethiol can be effectively attached to the surface of ferroferric oxide, thereby preventing the ferroferric oxide nanoparticles from further growing; and meanwhile, the mutual aggregation of the ferroferric oxide nanoparticles can be accelerated, thereby generating the ferroferric oxide microspheres having a hierarchical structure through self assembling. By adopting the one-step liquid-phase method, the method is simple to operate, low in raw material cost and easy to control. The product has remarkable selective adsorption effect on lead ions in a water solution, and can be recycled.
Description
Technical field
A kind of method that the present invention relates to one-step synthesis hierarchy tri-iron tetroxide microballoon with and products thereof application process, be specifically related to a kind of synthetic method of hierarchy tri-iron tetroxide microballoon that can the selective absorption lead ion.
Background technology
In recent years, the micro Nano material that there is hierarchy because of its have good character and widely application prospect receive much concern.The micro Nano material size of hierarchy is larger, but by size, less nano material unit self assembly forms, and has high specific area.This class material has function and the advantageous property of nanometer and micrometer structure simultaneously, by the form of hierarchy, has brought into play to greatest extent advantage separately of micron, nano material and has suppressed its deficiency.
The method of the synthetic hierarchy micro Nano material of having reported at present has template, multistep reaction method, vapour deposition process and liquid phase method etc.Template finally need to be removed template by methods such as calcining, chemical attacks, and the operation of removing template may exert an influence to final product.The multistep reaction method is due to the reaction that relates to a plurality of steps, operates comparatively loaded down with trivial detailsly, is not easy to control.One step liquid phase method has simple to operate, is easy to control, and reaction unit is required to the advantages such as low, is the Perfected process for preparing the hierarchy micro Nano material.
The tri-iron tetroxide micro Nano material has unique ferromagnetism, thereby has been subject to paying close attention to widely, at aspects such as magnetic recording, magnetic fluid, magnetic resonance imaging and target medicine carriers, all has wide practical use.In recent years, existing a large amount of synthetic report about the tri-iron tetroxide micro Nano material, comprise nanometer rods, nano wire, microballoon etc.In addition, also a lot of about the research of ferriferrous oxide nano composite.
Effluent containing heavy metal ions pollutes has become a global problem.Heavy metal ion is hypertoxic, and has been found that aspect a lot of and had influence on people's health, even still can be influential when its concentration is very low.In heavy-metal pollution, the pollution of lead ion is modal.Lead ion can hinder the biosynthesis of heme, suppresses several synthetic containing zinc element enzyme, with nucleic acid and t-RNA effect and then affect synthesizing of protein, and can in bone, assemble.
Traditional method of removing heavy metal ions in wastewater has: chemical precipitation method, coagulation-flocculence, ion-exchange, membrane filter method, electroosmose process and absorption method etc.The characteristics such as in these technology, absorption method is low because of the cost that it has, and efficiency height and secondary pollution are less, be considered to technology the most easily.Adsorbent commonly used is mainly active carbon at present, porous silica etc.These adsorbents can adsorb poisonous heavy metal ion at short notice, and have higher adsorption efficiency.Yet but have the following disadvantages: poisonous heavy metal ion is present in a large amount of waste water, after adsorbent has adsorbed heavy metal ion, usually adopt the methods such as sedimentation, filtration and centrifugation that adsorbent is separated from water, but the speed that these methods are processed is slow, wastes time and energy.
Recently, magnetic composite has obtained widely and has paid close attention in field of waste water treatment.Magnetic composite is gathered around magnetic component, has good external magnetic field response characteristic, is easy to be attracted by external magnetic field.The effect magnetic composite of outside magnetic field can be collected and separate easily, and other functional components in magnetic composite can provide the adsorption function to heavy metal ion, for example: the Fe with nucleocapsid structure
3o
4@SiO
2and Fe
3o
4siO in@shitosan magnetic composite
2there is superior heavy metal ion adsorbed ability with shitosan, so these magnetic composites can be used as adsorbent and remove the heavy metal ion in waste water.In these magnetic composites, Fe
3o
4only play the effect of a response external magnetic field, to removing heavy metal ion, do not play what effect.
The shortcoming of prior art: 1. synthetic employing multistep reaction or the template synthesis of hierarchy, step is more complicated.2. nonmagnetic adsorbent is deposited and is had in use separation difficulty, the shortcoming such as time-consuming.
Summary of the invention
A kind of method that the object of the present invention is to provide one-step synthesis hierarchy tri-iron tetroxide microballoon with and products thereof application process, a step liquid phase method of employing, simple to operate, raw material is cheap, be easy to control.Product is remarkable to the selective absorption effect of lead ion in the aqueous solution, and can recycle.
Concrete technical scheme is as follows:
The method of one-step synthesis hierarchy tri-iron tetroxide microballoon adopts following steps: ferric salt, sodium acetate trihydrate are dissolved in a certain amount of ethylene glycol, then add lauryl mercaptan in mixed solution, and stir as emulsion, heated, cooling and washing.
Further, specifically comprise the steps:
(1) ferric salt, sodium acetate trihydrate are dissolved in a certain amount of ethylene glycol;
(2) be stirred to dissolving and obtain mixed solution;
(3) add a certain amount of lauryl mercaptan in mixed solution obtained above, fully stir into emulsion;
(4) solution is packed into container;
(5) heating;
(6) cooling;
(7) collect product;
(8) washing;
(9) drying.
Described in step (1), ferric salt is ferric chloride hexahydrate, and/or Fe(NO3)39H2O.
At room temperature carry out step (1) and (2).
In step (4), the mixed liquor of gained is packed in the autoclave of inner liner polytetrafluoroethylene inner bag.
In step (5), under 180～200 ℃, heat 8～48 hours.
Step naturally cools to room temperature in (6).
Step is collected product with externally-applied magnetic field in (7).
Use acetone and absolute ethanol washing in step (8) for several times.
In step (9) in vacuum drying chamber 60 ℃ of dryings approximately 2 hours.
The application process of the product of the method for above-mentioned one-step synthesis hierarchy tri-iron tetroxide microballoon, be applied to the heavy metal ion in adsorption aqueous solution, comprises the steps:
Under a, room temperature, by 0.2g hierarchy Fe
3o
4microballoon joins the Pb that 50mL concentration is 10mg/L
2+(or Cd
2+, Cu
2+) in the aqueous solution of ion and stir with mechanical stirring device, make Fe
3o
4microballoon and Pb
2+ion fully contacts, and then every 10 minutes, gets 3mL solution, with externally-applied magnetic field, removes Fe
3o
4, more remaining Pb in analytical solution
2+the concentration of ion.
B, to hierarchy Fe
3o
4microballoon recycle research as follows: get 0.2gFe
3o
4be distributed to the Pb that 50mL concentration is 10mg/L
2+in solution and constantly, stir, after the absorption of 40 minutes, under the effect of externally-applied magnetic field, by Fe
3o
4microballoon is collected fully, by weak acid solution desorption under ultrasonic effect of 100mL, then use the distilled water washes clean, adsorbent again joins in identical solution and carries out the next one circulation, repeat aforesaid operations and recycle altogether 5 times, each absorption is later to remaining Pb in solution
2+concentration is detected.
The present invention compares with the technology of existing Liquid preparation methods tri-iron tetroxide micro Nano material, lauryl mercaptan can be attached to the surface of tri-iron tetroxide effectively, stop ferriferrous oxide nano-particle further to be grown up, can promote ferriferrous oxide nano-particle reunion each other, thereby self assembly generates the tri-iron tetroxide microballoon with hierarchy simultaneously.This synthetic method one step can obtain target product, simple to operate, raw material is cheap, be easy to control.
The accompanying drawing explanation
The hierarchy Fe that Fig. 1 is embodiment 1 preparation
3o
4the X-ray diffraction pattern of microballoon.
The hierarchy Fe that Fig. 2 is embodiment 1 preparation
3o
4the stereoscan photograph of microballoon.
The hierarchy Fe that Fig. 3 is embodiment 1 preparation
3o
4the transmission electron microscope photo of microballoon.
The hierarchy Fe that Fig. 4 is embodiment 2 preparations
3o
4the stereoscan photograph of microballoon.
The hierarchy Fe that Fig. 5 is embodiment 3 preparations
3o
4the stereoscan photograph of microballoon.
The hierarchy Fe that Fig. 6 is embodiment 4 preparations
3o
4the stereoscan photograph of microballoon.
The hierarchy Fe that Fig. 7 is embodiment 5 preparations
3o
4the stereoscan photograph of microballoon.
The hierarchy Fe that Fig. 8 is embodiment 6 preparations
3o
4the stereoscan photograph of microballoon.
The hierarchy Fe that Fig. 9 is embodiment 7 preparations
3o
4the stereoscan photograph of microballoon.
Figure 10 is for being used the hierarchy Fe of embodiment 1 preparation
3o
4the kinetic curve of lead, cadmium and copper ion in the microballoon adsorption aqueous solution.
Figure 11 is the hierarchy Fe that recycles embodiment 1 preparation
3o
4in the microballoon adsorption aqueous solution, lead ion removes efficiency change figure.
The specific embodiment
Below describe the present invention with reference to the accompanying drawings, it is a kind of preferred embodiment in numerous embodiments of the present invention.
The method of one-step synthesis hierarchy tri-iron tetroxide microballoon, a, at room temperature, ferric salt, sodium acetate trihydrate are dissolved in a certain amount of ethylene glycol, under room temperature, be stirred to dissolve and obtain mixed solution, add a certain amount of lauryl mercaptan in mixed solution obtained above, fully stir into emulsion; B, the mixed liquor of gained in step a is packed in the autoclave of inner liner polytetrafluoroethylene inner bag, heat 8～48 hours under 180～200 ℃, naturally cool to subsequently room temperature.Collect product with externally-applied magnetic field, with acetone and absolute ethanol washing for several times, last 60 ℃ of dryings approximately 2 hours in vacuum drying chamber, described ferric salt is ferric chloride hexahydrate, Fe(NO3)39H2O.In this reaction, ferric salt is as source of iron, and sodium acetate is as alkali source, and ethylene glycol is as the solvent reducing agent of holding concurrently, and lauryl mercaptan is as emulsifying agent and surfactant, and end reaction generates the tri-iron tetroxide microballoon of hierarchy.Lauryl mercaptan is attached on the surface of product, utilizes the organic solvents such as acetone and ethanol that the lauryl mercaptan molecule on product surface is washed away, the impact caused while reducing organic molecule on Characterization of The Products.
Embodiment 1:
A, at room temperature, 1.34 gram ferric chloride hexahydrates and 3.4 gram sodium acetate trihydrates are dissolved in the ethylene glycol of 30 milliliters, under room temperature, are stirred to fully and dissolve and obtain mixed solution, lauryl mercaptan to adding 10 milliliters in mixed solution obtained above, fully stir into emulsion;
B, the emulsion of gained in step a is packed in the autoclave of inner liner polytetrafluoroethylene inner bag, heating is 8 hours under 180 ℃, naturally cools to subsequently room temperature.Collect product with externally-applied magnetic field, use respectively acetone and absolute ethanol washing for several times, last 60 ℃ of dryings approximately 2 hours in vacuum drying chamber, characterize waiting.
Its result is as shown in accompanying drawing 1～3: the explanation of the X-ray diffraction pattern of Fig. 1 obtains by the method is the Fe of pure quadrature phase
3o
4.The scanning electron microscope (SEM) photograph of Fig. 2 shows that this product is the microballoon of the hierarchy that formed by a large amount of self-assemblies.The favorable dispersibility of these microballoons, particle diameter is than homogeneous, and average grain diameter is 400 nanometers approximately.The particle diameter that forms the nano particle of microballoon is 10～20 nanometers.Fig. 3 is the transmission electron microscope picture of product, shows that equally these microballoons are to be formed by less self-assembly, and is solid structure.
Embodiment 2:
A, at room temperature, 1.34 gram ferric chloride hexahydrates and 3.4 gram sodium acetate trihydrates are dissolved in the ethylene glycol of 35 milliliters, under room temperature, are stirred to fully and dissolve and obtain mixed solution, lauryl mercaptan to adding 5 milliliters in mixed solution obtained above, fully stir into emulsion;
B, the mixed liquor of gained in step a is packed in the autoclave of inner liner polytetrafluoroethylene inner bag, heating is 8 hours under 180 ℃, naturally cools to subsequently room temperature.Collect product with externally-applied magnetic field, use respectively acetone and absolute ethanol washing for several times, last 60 ℃ of dryings approximately 2 hours in vacuum drying chamber, characterize waiting.
Its result is as shown in Figure 4.
The ESEM picture of Fig. 4 has shown to obtain the microballoon of tri-iron tetroxide, but the uniformity of these microballoons is poor, and wherein some is assembled by granule, and some is only formed by several particle assembling, and some also presents the characteristic of monocrystalline even.Illustrate and can not effectively stop growing up of ferriferrous oxide particles if the consumption of lauryl mercaptan is very few, thereby be difficult to obtain the tri-iron tetroxide microballoon of hierarchy.
Embodiment 3:
A, at room temperature, 1.34 gram ferric chloride hexahydrates and 3.4 gram sodium acetate trihydrates are dissolved in the ethylene glycol of 20 milliliters, under room temperature, are stirred to fully and dissolve and obtain mixed solution, lauryl mercaptan to adding 20 milliliters in mixed solution obtained above, fully stir into emulsion;
B, the mixed liquor of gained in step a is packed in the autoclave of inner liner polytetrafluoroethylene inner bag, heating is 8 hours under 180 ℃, naturally cools to subsequently room temperature.Collect product with externally-applied magnetic field, use respectively acetone and absolute ethanol washing for several times, last 60 ℃ of dryings approximately 2 hours in vacuum drying chamber, characterize waiting.
Its result as shown in Figure 5.
The ESEM picture of Fig. 5 shows that obtained product is the tri-iron tetroxide microballoon with hierarchy, and result is similar to example 2, and the particle diameter that still forms the nano particle of microballoon slightly reduces.Illustrate that the consumption that increases lauryl mercaptan can further suppress the growth of ferriferrous oxide nano-particle.
Embodiment 4:
A, at room temperature, 1.34 gram ferric chloride hexahydrates and 3.4 gram sodium acetate trihydrates are dissolved in the ethylene glycol of 30 milliliters, under room temperature, are stirred to fully and dissolve and obtain mixed solution, lauryl mercaptan to adding 10 milliliters in mixed solution obtained above, fully stir into emulsion;
B, the mixed liquor of gained in step a is packed in the autoclave of inner liner polytetrafluoroethylene inner bag, heating is 19 hours under 180 ℃, naturally cools to subsequently room temperature.Collect product with externally-applied magnetic field, use respectively acetone and absolute ethanol washing for several times, last 60 ℃ of dryings approximately 2 hours in vacuum drying chamber, characterize waiting.
Its result as shown in Figure 6.
The ESEM picture of Fig. 6 shows that the microballoon pattern of this hierarchy is similar to the product pattern of example 2,3, but a small amount of larger nano particle has wherein appearred, explanation is along with the prolongation in reaction time, and ferriferrous oxide nano-particle has the trend of growing up gradually.
Embodiment 5:
A, at room temperature, 1.34 gram ferric chloride hexahydrates and 3.4 gram sodium acetate trihydrates are dissolved in the ethylene glycol of 30 milliliters, under room temperature, are stirred to fully and dissolve and obtain mixed solution, lauryl mercaptan to adding 10 milliliters in mixed solution obtained above, fully stir into emulsion;
B, the mixed liquor of gained in step a is packed in the autoclave of inner liner polytetrafluoroethylene inner bag, heating is 48 hours under 180 ℃, naturally cools to subsequently room temperature.Collect product with externally-applied magnetic field, use respectively acetone and absolute ethanol washing for several times, last 60 ℃ of dryings approximately 2 hours in vacuum drying chamber, characterize waiting.
Its result as shown in Figure 7.
The ESEM picture of Fig. 7 shows that the microballoon pattern of this hierarchy is similar to the product pattern of example 5, wherein the shared ratio of larger nano particle is larger, further illustrate the prolongation along with the reaction time, ferriferrous oxide nano-particle has the trend of growing up gradually.
Embodiment 6:
A, at room temperature, 1.34 gram ferric chloride hexahydrates and 3.4 gram sodium acetate trihydrates are dissolved in the ethylene glycol of 30 milliliters, under room temperature, are stirred to fully and dissolve and obtain mixed solution, lauryl mercaptan to adding 10 milliliters in mixed solution obtained above, fully stir into emulsion;
B, the mixed liquor of gained in step a is packed in the autoclave of inner liner polytetrafluoroethylene inner bag, heating is 8 hours under 200 ℃, naturally cools to subsequently room temperature.Collect product with externally-applied magnetic field, use respectively acetone and absolute ethanol washing for several times, last 60 ℃ of dryings approximately 2 hours in vacuum drying chamber, characterize waiting.
Its result as shown in Figure 8.
The ESEM picture of Fig. 8 shows that obtained product is the tri-iron tetroxide microballoon with hierarchy, and result is similar to example 2, and the particle diameter that still forms the nano particle of microballoon slightly has increase.Explanation is along with the rising of reaction temperature, and ferriferrous oxide nano-particle can be grown up.
Embodiment 7:
A, at room temperature, 2.02 gram Fe(NO3)39H2Os and 3.4 gram sodium acetate trihydrates are dissolved in the ethylene glycol of 30 milliliters, under room temperature, are stirred to fully and dissolve and obtain mixed solution, lauryl mercaptan to adding 10 milliliters in mixed solution obtained above, fully stir into emulsion;
B, the mixed liquor of gained in step a is packed in the autoclave of inner liner polytetrafluoroethylene inner bag, heating is 8 hours under 180 ℃, naturally cools to subsequently room temperature.Collect product with externally-applied magnetic field, use respectively acetone and absolute ethanol washing for several times, last 60 ℃ of dryings approximately 2 hours in vacuum drying chamber, characterize waiting.
Its result as shown in Figure 9.
Although it is the tri-iron tetroxide microballoon with hierarchy that the ESEM picture of Fig. 9 shows the product obtained, particle size were is inhomogeneous, and the size of the ferriferrous oxide nano-particle of formation microballoon is also very inhomogeneous.
The embodiment of the heavy metal ion in adsorption aqueous solution:
Under a, room temperature, by the hierarchy Fe of 0.2g example 1 synthesized
3o
4microballoon joins the Pb that 50mL concentration is 10mg/L
2+(or Cd
2+, Cu
2+) in the aqueous solution of ion and stir with mechanical stirring device, make Fe
3o
4microballoon and Pb
2+ion fully contacts, and then every 10 minutes, gets 3mL solution, with externally-applied magnetic field, removes Fe
3o
4, more remaining Pb in analytical solution
2+the concentration of ion.
B, to hierarchy Fe
3o
4microballoon recycle research as follows: get 0.2g Fe
3o
4be distributed to the Pb that 50mL concentration is 10mg/L
2+in solution and constantly, stir, after the absorption of 40 minutes, under the effect of externally-applied magnetic field, by Fe
3o
4microballoon is collected fully, by weak acid solution desorption under ultrasonic effect of 100mL, then uses the distilled water washes clean, and adsorbent again joins in identical solution and carries out the next one circulation, repeats aforesaid operations and recycles altogether 5 times.Each absorption is later to remaining Pb in solution
2+concentration is detected.
The result of test is as Fig. 9, shown in 10:
Figure 9 shows that the hierarchy Fe that example 1 is prepared
3o
4microballoon removes respectively the Pb in the aqueous solution
2+, Cu
2+and Cd
2+removal efficiency chart etc. heavy metal ion.C wherein
0pb
2+initial concentration (C
0=10mgL
– 1), C is the concentration after absorption.
The initial concentration of these heavy metal ion is 10mgL
– 1.Can find out Pb
2+concentration just promptly reduces within initial 10 minutes, and Cu
2+and Cd
2+there is no great variation, subsequently Pb
2+concentration with also have reducing but the speed reduced obviously slow down, after 30 minutes, Pb
2+concentration almost no longer changes, and shows that this adsorbent has now reached saturated, by calculating known hierarchy Fe
3o
4microballoon is to Pb
2+removal rate can reach 97%.Above experimental result shows the Fe of hierarchy
3o
4microballoon can be optionally by Pb
2+from rare aqueous solution, absorption is fallen effectively.
As can be seen from Figure 10 Fe in recycling process
3o
4the adsorption efficiency of adsorbent does not significantly change, and this has absolutely proved the Fe of hierarchy
3o
4microballoon has good desorption ability and recycles ability.
The above is exemplarily described the present invention by reference to the accompanying drawings; obviously specific implementation of the present invention is not subject to the restrictions described above; as long as the various improvement that adopted method design of the present invention and technical scheme to carry out; or directly apply to other occasion without improvement, all within protection scope of the present invention.
Claims (10)
1. the method for one-step synthesis hierarchy tri-iron tetroxide microballoon, is characterized in that, adopts following steps: ferric salt, sodium acetate trihydrate are dissolved in a certain amount of ethylene glycol, add lauryl mercaptan again in mixed solution, and stir as emulsion, heated cooling and washing.
2. the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as claimed in claim 1, is characterized in that, specifically comprises the steps:
(1) ferric salt, sodium acetate trihydrate are dissolved in a certain amount of ethylene glycol;
(2) be stirred to dissolving and obtain mixed solution;
(3) add a certain amount of lauryl mercaptan in mixed solution obtained above, fully stir into emulsion;
(4) solution is packed into container;
(5) heating;
(6) cooling;
(7) collect product;
(8) washing;
(9) drying.
3. the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as claimed in claim 2, is characterized in that, described in step (1), ferric salt is ferric chloride hexahydrate, and/or Fe(NO3)39H2O, and/or at room temperature carry out step (1) and (2).
4. as the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as described in claim 2 or 3, it is characterized in that, in the autoclave of the inner liner polytetrafluoroethylene inner bag of in step (4), the mixed liquor of gained being packed into.
5. as the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as described in any one in claim 2-4, it is characterized in that, heat under 180～200 ℃ 8～48 hours in step (5).
6. as the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as described in any one in claim 2-5, it is characterized in that, step naturally cools to room temperature in (6).
7. as the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as described in any one in claim 2-6, it is characterized in that, step is collected product with externally-applied magnetic field in (7).
8. as the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as described in any one in claim 2-7, it is characterized in that, in step (8) with acetone and absolute ethanol washing for several times.
9. as the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as described in any one in claim 2-8, it is characterized in that, in step (9) in vacuum drying chamber 60 ℃ of dryings approximately 2 hours.
10. as the application process of the product of the method for one-step synthesis hierarchy tri-iron tetroxide microballoon as described in claim 1-9, it is characterized in that, be applied to the heavy metal ion in adsorption aqueous solution, comprise the steps:
Under a, room temperature, by 0.2g hierarchy Fe
3o
4microballoon joins the Pb that 50mL concentration is 10mg/L
2+(or Cd
2+, Cu
2+) in the aqueous solution of ion and stir with mechanical stirring device, make Fe
3o
4microballoon and Pb
2+ion fully contacts, and then every 10 minutes, gets 3mL solution, with externally-applied magnetic field, removes Fe
3o
4, more remaining Pb in analytical solution
2+the concentration of ion.
B, to hierarchy Fe
3o
4microballoon recycle research as follows: get 0.2g Fe
3o
4be distributed to the Pb that 50mL concentration is 10mg/L
2+in solution and constantly, stir, after the absorption of 40 minutes, under the effect of externally-applied magnetic field, by Fe
3o
4microballoon is collected fully, by weak acid solution desorption under ultrasonic effect of 100mL, then use the distilled water washes clean, adsorbent again joins in identical solution and carries out the next one circulation, repeat aforesaid operations and recycle altogether 5 times, each absorption is later to remaining Pb in solution
2+concentration is detected.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105883934A (en) * | 2016-04-18 | 2016-08-24 | 吉林师范大学 | Method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres |
| CN106596501A (en) * | 2016-11-23 | 2017-04-26 | 深圳先进技术研究院 | Magnetic movable Raman enhanced chip, and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011086567A1 (en) * | 2010-01-12 | 2011-07-21 | Council Of Scientific & Industrial Research | Magnetic dye-adsorbent catalyst |
| CN103263886A (en) * | 2013-06-06 | 2013-08-28 | 湖北大学 | Hydrothermal preparation method and application of magnetic ferroferric oxide nanochain |
-
2013
- 2013-09-03 CN CN201310396313.9A patent/CN103480323B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011086567A1 (en) * | 2010-01-12 | 2011-07-21 | Council Of Scientific & Industrial Research | Magnetic dye-adsorbent catalyst |
| CN103263886A (en) * | 2013-06-06 | 2013-08-28 | 湖北大学 | Hydrothermal preparation method and application of magnetic ferroferric oxide nanochain |
Non-Patent Citations (3)
| Title |
|---|
| 余响林 等: "可循环利用的重金属离子吸附剂的制备与性能研究", 《长江大学学报（自然科学版）》, vol. 8, no. 4, 30 April 2011 (2011-04-30), pages 14 - 17 * |
| 王萌 等: "巯基修饰和胡敏酸包裹纳米 Fe3O4颗粒的制备及其对溶液中Pb2+Cd2+Cu2+的吸附效果研究", 《农业环境科学学报》, vol. 30, no. 8, 31 August 2011 (2011-08-31), pages 1669 - 1674 * |
| 路苹 等: "单分散Fe3O4亚微米球的合成与表征", 《无机化学学报》, vol. 26, no. 7, 31 July 2010 (2010-07-31), pages 1177 - 1182 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105883934A (en) * | 2016-04-18 | 2016-08-24 | 吉林师范大学 | Method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres |
| CN106596501A (en) * | 2016-11-23 | 2017-04-26 | 深圳先进技术研究院 | Magnetic movable Raman enhanced chip, and preparation method and application thereof |
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