CN104874382A - Preparation method of vermiculite loaded with magnetic nano-materials - Google Patents
Preparation method of vermiculite loaded with magnetic nano-materials Download PDFInfo
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- CN104874382A CN104874382A CN201510222656.2A CN201510222656A CN104874382A CN 104874382 A CN104874382 A CN 104874382A CN 201510222656 A CN201510222656 A CN 201510222656A CN 104874382 A CN104874382 A CN 104874382A
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Abstract
The invention particularly relates to a preparation method of vermiculite loaded with magnetic nano-materials, and belongs to the technical field of water treatment of inorganic materials. The method comprises the following steps: mixing FeCl3.6H2O, NaAc.3H2O, glycol, ethylenediamine and industrial vermiculite powder to obtain yellowish-brown turbid liquid, encapsulating the yellowish-brown turbid liquid in a polytetrafluoroethylene reaction kettle, reacting for 8h and more at 180-200 DEG C, taking black solid, washing, magnetically separating, drying and grinding to obtain vermiculite loaded with magnetic nano-materials. The magnetization modification is directly performed in the industrial vermiculite through a thermosynthesis technology, the operation flow is simple and easy to control, the preparation cost is low, the industrial production threshold is low, and the method is easy for the industrial large-scale production; the prepared loaded magnetic vermiculite not only has the feature diffraction peak of the vermiculite and has the superparamagnetism of the magnetic nanoparticles; the prepared loaded magnetic vermiculite has good effect on partial dye pollutant in the water.
Description
Technical field
The present invention is specifically related to the preparation method that vermiculite loads magnetic Nano material, belongs to inorganic material water-treatment technology field.
Background technology
Vermiculite belongs to layered magnesium (or aluminium) silicate mineral of 2: 1 types, by two silicon-oxy tetrahedrons and an octahedra construction unit layer forming vermiculite of magnesium (or aluminium) oxygen (or hydrogen-oxygen).In the forming process of vermiculite, because isomorphous substitution phenomenon is as Al in tetrahedron
3+, Fe
3+to Si
4+displacement, make to produce permanent negative electrical charge between vermiculite crystal layer, these negative electrical charges by the tradable cation of interlayer as Na
+, K
+, Ca
2+, Mg
2+etc. balancing, due to the interchangeability of interlayer ion, there is larger specific area and higher ion exchange capacity, making vermiculite have stronger cation exchange capacity (CEC).
Vermiculite is special, the widely used nonmetallic ore of a kind of character, all can obtain remarkable benefit because of application vermiculite in the department such as heat insulation, insulation, light building material, waste liquid disposal, gardening, agricultural, feed, the vermiculite through chemical modification and specially treated even also can display application prospect in high-tech sector.
Usually said vermiculite refers to Industrial Vermiculite, it comprises the vermiculite of mineralogical significance and the rule of vermiculite and mica or irregular interstratified minerals, vermiculite has good adsorptivity, ion-exchange performance etc., in industry, agricultural, gardening, animal husbandry etc., have wide range of application.But Industrial Vermiculite sample is generally impure, affect its reactivity, its surface hydrophilicity affects again its application in the composite, and vermiculite has expansile shortcoming, is very important so carry out modification to Industrial Vermiculite.Conventional method of modifying has sour modification, heat modification, organically-modified etc.
Magnetic carrier technology, be evenly to be introduced in the particle of non magnetic or weak magnetic thus the magnetic susceptibility of matrix material is strengthened by the ferromagnetic substance that has of dispersion, use magnetic separation technique allows saturated magnetic compound be separated fast from effect system then.Therefore, the magnetic material of easily collecting under external magnetic field, is being separated and is having unique advantage in removal process.But, have no the document that vermiculite loads the preparation method of magnetic Nano material.
Summary of the invention
This patent provides a kind of technological process simple, and removal efficiency is high, and cost-saving vermiculite of preparing loads the large method of magnetic Nano material, better to remove water pollutant.
Technical scheme
Vermiculite loads a preparation method for magnetic Nano material, comprises the following steps:
(1) by FeCl
36H
2o, NaAc 3H
2o is dissolved in ethylene glycol, then adds ethylenediamine and forms clear solution, then add Industrial Vermiculite powder, obtain yellowish-brown suspension;
(2) suspension is packaged in polytetrafluoroethylene (PTFE) reactor, under 180-200 DEG C of condition, reacts 8 more than h, get black solid;
(3) black solid is through washing, Magneto separate, oven dry, grinding, obtains the vermiculite loading magnetic Nano material.
Preparation method of the present invention, using iron chloride as source of iron, adopts ethylene glycol as solvent and carries out partial solvent thermal reduction to ferric ion, successfully synthesizing ferroferric oxide nano granules; Sodium acetate is adopted to be coating agent as reflection auxiliary agent, ethylenediamine, can the uniform tri-iron tetroxide of synthesizing nano-particle by the ratio controlling ethylenediamine and ferric trichloride.By two step key reactions in the reaction of synthesis ferroferric oxide nano granules, possible reaction is as follows:
2Fe
3++OHCH
2CH
2OH+2H
+→2Fe
2++CH
3CHO+2H
2O；
2Fe
3++Fe
2++8OH
- →Fe
3O
4+4H
2O。
In synthetic reaction process, nano ferriferrous oxide is combined with Industrial Vermiculite powder and forms magnetic vermiculite.
In addition, ethylenediamine will be planted after reagent adds at first three and be added; Otherwise iron chloride and sodium acetate cannot dissolve.
In said method, FeCl
36H
2o, ethylene glycol, NaAc 3H
2o, ethylenediamine and Industrial Vermiculite powder participate in magnetic vermiculite building-up process, and the change of its consumption does not affect the generation of product, but can affect the performance of prepared magnetic vermiculite.Obtain the magnetic vermiculite of higher magnetic, FeCl to reduce wastage of material simultaneously
36H
2o, ethylene glycol, NaAc 3H
2the usage ratio of O, ethylenediamine and Industrial Vermiculite powder is preferably: 1.0g:20mL:3.0g:10mL:0.04-1.0g; Most preferredly be: 1.0g:20mL:3.0g:10mL:1.0g.
In order to shorten mixing time, said method, preferably by FeCl
36H
2o is dissolved in ethylene glycol, then adds NaAc 3H
2o.
beneficial effect
(1) the present invention directly adds magnetic modification to Industrial Vermiculite by Hydrothermal Synthesis technology, and operating process is simple and easy to control, and preparation cost is low, and suitability for industrialized production threshold is low, is easy to industrial mass production;
(2) do not need in preparation process to use water, only need a small amount of organic solvent;
(3) the loading magnetic vermiculite prepared by not only possesses the characteristic diffraction peak of vermiculite, have the advantage of the superparamagnetism of magnetic nano-particle, and operating process is convenient and simple, and save material cost, combined coefficient is high;
(4) the loading magnetic vermiculite prepared is to the some dyes pollutant in water, and the adsorption effect as basic fuchsin, alkaline royal blue dyestuff etc. is good, and can realize the quick separating of solid-liquid after having adsorbed, and adsorbent is recycled;
(5) add ethylenediamine in preparation process, absorption property and the superparamagnetism of product can be significantly improved.
Accompanying drawing explanation
Fig. 1 is magnetic vermiculite of the present invention and Industrial Vermiculite, Fe
3o
4the X-ray diffraction spectrogram of contrast; Wherein, A-D is followed successively by: the vermiculite of Fe3O4, Industrial Vermiculite, embodiment 4-5 loads the X-ray diffraction spectrogram of magnetic Nano material.
Detailed description of the invention
embodiment 1
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, adds 6.0 g NaAc 3H
2o forms clear solution, then adds 20 mL ethylenediamines, adds the Industrial Vermiculite powder of 0.08g, stirs 30 minutes, obtains well-mixed yellowish-brown suspension (Industrial Vermiculite powder fully disperses);
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), adds thermal response 8 h at 180 DEG C, reacted rear cool to room temperature;
(3) black solid distilled water washing several (washing away impurity) will obtained, Magneto separate, dries, and 100 mesh sieves are crossed in grinding, obtains loading magnetic vermiculite MV1;
Under room temperature, add 0.04g MV1 in the Basic Fuchsin in Aqueous Solution of 25mL 20mg/l, vibration 360min, adsorption rate reaches 81.2%; In the alkaline royal blue solution of 25mL 20mg/l, add 0.04g MV1, vibration 360min, adsorption rate reaches 78.76%.
embodiment 2
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, adds 6.0 g NaAc 3H
2o forms clear solution, then adds 20 mL ethylenediamines, adds the Industrial Vermiculite powder of 0.2g, stirs 30 minutes, obtains well-mixed yellowish-brown suspension;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), adds thermal response 8 h at 190 DEG C, reacted rear cool to room temperature;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and 100 mesh sieves are crossed in grinding, obtains loading magnetic vermiculite MV2;
Under room temperature, add 0.04g MV2 in the Basic Fuchsin in Aqueous Solution of 25mL 20mg/l, vibration 360min, adsorption rate reaches 83.9%; In the alkaline royal blue solution of 25mL 20mg/l, add 0.04g MV2, vibration 360min, adsorption rate reaches 85.1%.
embodiment 3
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, adds 6.0 g NaAc 3H
2o forms clear solution, then adds 20 mL ethylenediamines, adds 0.4g Industrial Vermiculite powder, stirs 30 minutes, obtains well-mixed yellowish-brown suspension;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), adds thermal response 8 h at 200 DEG C, reacted rear cool to room temperature;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and 200 mesh sieves are crossed in grinding, obtains loading magnetic vermiculite MV3;
Under room temperature, add 0.04g MV3 in the Basic Fuchsin in Aqueous Solution of 25mL 20mg/l, vibration 360min, adsorption rate reaches 87.84%; In the alkaline royal blue solution of 25mL 20mg/l, add 0.04g MV3, vibration 360min, adsorption rate reaches 92.41%.
embodiment 4
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, adds 6.0 g NaAc 3H
2o forms clear solution, then adds 20 mL ethylenediamines, adds 0.8g sodium base vermiculite powder, stirs 30 minutes; Obtain well-mixed yellowish-brown suspension;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), adds thermal response 8 h at 200 DEG C, reacted rear cool to room temperature;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and 200 mesh sieves are crossed in grinding, obtains loading magnetic vermiculite MV4;
Under room temperature, add 0.04g MV4 in the Basic Fuchsin in Aqueous Solution of 25mL 20mg/l, vibration 150min, adsorption rate reaches 90.3%; In the alkaline royal blue solution of 25mL 100mg/l, add 0.04g MV4, vibration 240min, adsorption rate reaches 92.8%
embodiment 5
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, adds 6.0 g NaAc 3H
2o forms clear solution, then adds 20 mL ethylenediamines, adds 2.0g sodium base vermiculite powder, stirs 30 minutes; Obtain well-mixed yellowish-brown suspension;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), adds thermal response 8 h at 200 DEG C, reacted rear cool to room temperature;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and 200 mesh sieves are crossed in grinding, obtains loading magnetic vermiculite MV5;
Under room temperature, add 0.04g MV5 in the Basic Fuchsin in Aqueous Solution of 25mL 20mg/l, vibration 360min, adsorption rate reaches 90.3%; In the alkaline royal blue solution of 25mL 20mg/l, add 0.04g MV5, vibration 360min, adsorption rate reaches 95.6%.
embodiment 6
(1) 2.0gFeCl3 6H2O is dissolved in 40mL ethylene glycol, adds 6.0gNaAc 3H2O and form clear solution, add 0.4g Industrial Vermiculite powder, stir 30 minutes, obtain well-mixed yellowish-brown suspension;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), adds thermal response 8h at 200 DEG C, reacted rear cool to room temperature;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and 200 mesh sieves are crossed in grinding, obtains loading magnetic vermiculite MV6;
Under room temperature, add 0.04g MV6 in the Basic Fuchsin in Aqueous Solution of 25mL 20mg/l, vibration 360min, adsorption rate reaches 76.43%; In the alkaline royal blue solution of 25mL 20mg/l, add 0.04g MV6, vibration 360min, adsorption rate reaches 81.29%.
Comparing embodiment 3 can draw with the experimental data of embodiment 6, when other conditions are identical, the absorption property of loading magnetic vermiculite MV3 prepared by ethylenediamine is added in preparation process, apparently higher than, in preparation process, do not add the absorption property of loading magnetic vermiculite MV6 prepared by ethylenediamine.As can be seen here, ethylenediamine serves the effect improving product absorption property in the preparation process in accordance with the present invention.
The present invention finds in experimentation: along with the increase of the amount of vermiculite, the ratio (Fe of Fe and vermiculite
/vermiculite) less, the magnetism of material of synthesis is more weak.The superparamagnetic performance (along with the increase of externally-applied magnetic field, the performance that magnetic increases) of MV3 is stronger than MV6, and in magnetic history, energy consumption is less; So, add ethylenediamine and can strengthen the superparamagnetic performance that vermiculite loads magnetic Nano material, be reduced in energy loss in remagnetization process.
Claims (4)
1. vermiculite loads a preparation method for magnetic Nano material, comprises the following steps:
(1) by FeCl
36H
2o, NaAc 3H
2o is dissolved in ethylene glycol, then adds ethylenediamine and forms clear solution, then add Industrial Vermiculite powder, obtain yellowish-brown suspension;
(2) suspension is packaged in polytetrafluoroethylene (PTFE) reactor, under 180-200 DEG C of condition, reacts 8 more than h, get black solid;
(3) black solid is through washing, Magneto separate, oven dry, grinding, obtains the vermiculite loading magnetic Nano material.
2. preparation method according to claim 1, is characterized in that, FeCl
36H
2o, ethylene glycol, NaAc 3H
2the usage ratio of O, ethylenediamine and Industrial Vermiculite powder is: 1.0g:20mL:3.0g:10mL:0.04-1.0g.
3. preparation method according to claim 2, is characterized in that, FeCl
36H
2o, ethylene glycol, NaAc 3H
2the usage ratio of O, ethylenediamine and Industrial Vermiculite powder is 1.0g:20mL:3.0g:10mL:1.0g.
4., according to the preparation method of claim 1,2 or 3, it is characterized in that, by FeCl
36H
2o is dissolved in ethylene glycol, then adds NaAc 3H
2o.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110655089A (en) * | 2018-06-29 | 2020-01-07 | 中国地质大学（北京） | Dispersion liquid with adjustable optical property and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0380986A (en) * | 1989-08-23 | 1991-04-05 | Shizen:Kk | Triiron tetroxide-containing water treatment agent |
| CN101417822A (en) * | 2008-11-24 | 2009-04-29 | 中国科学院长春应用化学研究所 | Method for preparing super paramagnetic mesoporous ferriferrous oxide nano particle |
| CN101647780A (en) * | 2009-09-23 | 2010-02-17 | 北京化工大学 | Core-shell type magnetic nano-composite particle based on Fe3O4 and houghite and preparation method thereof |
-
2015
- 2015-05-05 CN CN201510222656.2A patent/CN104874382A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0380986A (en) * | 1989-08-23 | 1991-04-05 | Shizen:Kk | Triiron tetroxide-containing water treatment agent |
| CN101417822A (en) * | 2008-11-24 | 2009-04-29 | 中国科学院长春应用化学研究所 | Method for preparing super paramagnetic mesoporous ferriferrous oxide nano particle |
| CN101647780A (en) * | 2009-09-23 | 2010-02-17 | 北京化工大学 | Core-shell type magnetic nano-composite particle based on Fe3O4 and houghite and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| L.C.R.MACHADO ET AL.: "Polymer coated vermiculite–iron composites:Novel floatable magnetic adsorbents for water spilled contaminants", 《APPLIED CLAY SCIENCE》 * |
| RAN-RAN SHAN ET AL.: "Magnetic Fe3O4/MgAl-LDH composite for effectiveremoval of three red dyes from aqueous solution", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 郑易安等: "不同方式处理蛭石对磷吸附性能研究", 《应用化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110655089A (en) * | 2018-06-29 | 2020-01-07 | 中国地质大学（北京） | Dispersion liquid with adjustable optical property and preparation method thereof |
| CN110655089B (en) * | 2018-06-29 | 2021-08-24 | 中国地质大学（北京） | Dispersion liquid with adjustable optical property and preparation method thereof |
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Application publication date: 20150902 |
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