CN104826601A - Preparation method of magnetic diatomite - Google Patents
Preparation method of magnetic diatomite Download PDFInfo
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- CN104826601A CN104826601A CN201510222597.9A CN201510222597A CN104826601A CN 104826601 A CN104826601 A CN 104826601A CN 201510222597 A CN201510222597 A CN 201510222597A CN 104826601 A CN104826601 A CN 104826601A
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Abstract
The invention relates to a preparation method of magnetic diatomite and belongs to the field of preparation of an environmental-protection adsorption material. The method comprises the following steps: mixing FeCl3.6H2O, NaAc.3H2O, ethanediol, ethidene diamine and diatomite powers to obtain a diatomite dispersive mixture, sealing the diatomite dispersive mixture into a teflon reaction kettle, reacting at 200 DEG C for more than 8 h, taking a black solid, washing, carrying out magnetic separation, drying, grinding, and sieving to obtain magnetic diatomite. Through a hydro-thermal synthesis technology, kaolin can directly undergo magnetical modification. The method provided by the invention is simple and easy to control. Preparation costs are low; industrial production threshold is low; and the method is easy for industrial popularization. In addition, temperature is low by the method such that the structure of diatomite will not be damaged and adsorptive property of diatomite is guaranteed. The prepared magnetic diatomite has superparamagnetism, is easy for solid-liquid separation and is easy for recovery and reutilization. By the method, the environment is protected and sustainability of resources is promoted.
Description
Technical field
The present invention relates to the diatomaceous preparation method of a kind of magnetic, belong to the preparation field of environmental-protection adsorption material.
Background technology
Diatomite is that the one that ancient times, unicellular rudimentary plant diatom remains were formed through preliminary diagenesis after piling up has porous biological silicalite.Primarily of diatom remains composition in ancient times, mineral composition is opal and mutation thereof mainly, is secondly clay mineral-hydromica, kaolinite and mineral chip; Its chemical analysis mainly SiO
2, containing a small amount of Al
2o
3, Fe
2o
3, CaO, MgO, K
2o, Na
2o, P
2o
5and organic matter.China's diatomite resource enriches, and up to now, national explored reserves 3.2 hundred million tons, prospective reserves can more than 1,000,000,000 tons, and position is at the forefront in the world.
Diatom penus silicolites rock, its essence is moisture noncrystalline SiO
2color is white, canescence, grey and terra brown etc., have fine and smooth, loose, light weight, porous, water imbibition and permeability are strong, specific area is large, chemical inertness and be insoluble to the excellent physicochemical properties such as general acid (except HF), therefore diatomite is widely used in preparing filter aid, adsorbent, catalytic carrier and functional stuffing.
Diatomite, as a kind of adsorbent of excellent economy, is often used to process phosphorous, organic pollution, heavy metal and dyestuff waste water.Natural diatomite multicomponent is impure, and impurity is more, plugs diatomite micropore, reduces specific surface area of diatomite, occupies kieselguhr adsorption point, this greatly limits the performance of kieselguhr adsorption performance.For improving kieselguhr adsorption performance, researcher mainly adopts Typical physical method or chemical method both at home and abroad at present, as washing, acidleach, roasting, microwave, pillared, the mode such as organic intercalation, polyalcohol intercalation and inorganic-organic hybrid carry out modification to it, thus its surface nature and interlayer structure are changed, increase its adsorption capacity.
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.It is combined the interlayer structure that not only can change mineral material with mineral material, and mineral material recovery can also be made to be reused.At present, existing magnetic carrier technology being combined with diatomite prepares magnetic diatomite material, and is applied to the pollutant in process waste water.As diatomite acid solution is carried out pretreatment by a kind of magnetic diatomite base adsorbent and preparation method thereof and application (publication number CN 103432986 A), the pre-modification of physics is carried out with plasma, with ferrous ion, dipping carries out to diatomite modified, adding alkali regulates pH to generate magnetic presoma, and drying, roasting, grinding obtain modification infusorial earth and be used for Adsorption of Nitrobenzene from Aqueous Solution.The diatomite that this present invention is modified, the adsorptivity of p-nitrophenyl significantly improves, and has larger magnetic simultaneously, is easy to the Separation of Solid and Liquid after processing waste water, but prepares the Fe of high-quality based on coprecipitation
3o
4the limitation of itself, make the magnetic diatomite composite material magnetic of preparation lower, and preparation process is comparatively complicated.
Summary of the invention
The object of the invention is to provide to improve the deficiencies in the prior art part the diatomaceous preparation method of magnetic that a kind of efficiency is high, technique is simple, modified effect is good.
Technical scheme
The diatomaceous preparation method of a kind of magnetic, 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 adds diatomite powder mixing, magnetic agitation 30 min, obtains the mixture of diatomite dispersion;
(2) mixture is encapsulated in polytetrafluoroethylene (PTFE) reactor, at 200 DEG C of reaction more than 8h, gets black solid;
(3) washed by black solid, Magneto separate, dry, grinding, sieves, obtains magnetic diatomite.
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 the process of synthetic reaction, nano ferriferrous oxide is combined with diatomite and forms magnetic diatomite.
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 diatomite powder participate in the diatomaceous building-up process of magnetic, and the change of its consumption does not affect the generation of product, but can affect the diatomaceous performance of prepared magnetic.Obtain the magnetic diatomite of higher magnetic, FeCl to reduce wastage of material simultaneously
36H
2o, ethylene glycol, NaAc 3H
2the usage ratio of O, ethylenediamine and diatomite powder is preferably: 2.0g:40mL:6.0g:20mL:0.2-2.0g; Most preferredly be: 2.0g:40mL:6.0g:20mL:0.2g.
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 diatomite by Hydrothermal Synthesis technology, and method is simple and easy to control, and preparation cost is low, and suitability for industrialized production threshold is low, is easy to industrialization promotion;
(2) this method preparation temperature is low, can not destroy diatomaceous structure, ensure that its absorption property;
(3) add ethylenediamine in preparation process, absorption property and the superparamagnetism of product can be significantly improved;
(4) the magnetic diatomite prepared by, possesses superparamagnetism, is convenient to Separation of Solid and Liquid, be easy to recovery and reuse, facilitates the sustainability of resource while protection of the environment; Have good removal effect to the phosphate in water and dyestuff methylene blue, the clearance of phosphorus is high, and in environmental pollution, the improvement of phosphorus in waste water provides new approaches.
Accompanying drawing explanation
Fig. 1 is magnetic diatomite of the present invention and diatomite original soil, Fe
3o
4the X-ray diffraction spectrogram of contrast; Wherein a, b are diatomite, Fe respectively
3o
4x-ray diffraction spectrogram, c, d, e, f are the diatomaceous X-ray diffraction spectrogram of magnetic prepared by embodiment 1,2,3,4 respectively.
Detailed description of the invention
embodiment 1
(1) by 2.0g FeCl
36H
2o is dissolved in 40mL ethylene glycol, then adds 6.0g NaAc 3H
2o, form yellowish-brown clear solution, then add 20mL ethylenediamine, add the diatomite of 0.2g, magnetic agitation 30 min makes diatomite fully disperse, and obtains mixture;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), at 200 DEG C of reaction 8 h, has reacted rear cool to room temperature, got black solid;
(3) black solid distilled water washing several (impurity is washed off) will obtained, (concrete operations are Magneto separate: use magnet, magnetisable material (magnetic diatomite) is separated from the solidliquid mixture after washing, discard the aqueous solution), dry, grinding, crosses 100 mesh sieves, obtains magnetic diatomite MD1;
Under room temperature, joined by 0.1g MD1 in the phosphate solution of 25mL 20mg/L, vibration 120min, adsorption rate reaches 96.29%; Under the same terms, diatomite original soil is only 14.40% to phosphatic adsorption rate.
embodiment 2
(1) by 2.0g FeCl
36H
2o and 6.0g NaAc 3H
2o is dissolved in 40mL ethylene glycol, and form yellowish-brown clear solution, then add 20mL ethylenediamine, add the diatomite of 0.4 g, magnetic agitation 30 min makes diatomite fully disperse, and obtains mixture;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), at 200 DEG C of reaction 8 h, has reacted rear cool to room temperature, got black solid;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding is crossed 100 mesh sieves, obtained magnetic diatomite MD2;
Under room temperature, joined by 0.1g MD2 in the phosphate solution of 25mL 20mg/L, vibration 120min, adsorption rate reaches 93.31%; Under the same terms, diatomite original soil is only 14.40% to phosphatic adsorption rate.
embodiment 3
(1) by 2.0g FeCl
36H
2o is dissolved in 40mL ethylene glycol, then adds 6.0g NaAc 3H
2o, form yellowish-brown clear solution, then add 20mL ethylenediamine, add the diatomite of 0.8g, magnetic agitation 30 min makes diatomite fully disperse, and obtains mixture;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), at 200 DEG C of reaction 8 h, has reacted rear cool to room temperature, got black solid;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding is crossed 100 mesh sieves, obtained magnetic diatomite MD3;
Under room temperature, joined by 0.1g MD3 in the phosphate solution of 25mL 20mg/L, vibration 120min, adsorption rate reaches 91.59%; Under the same terms, diatomite original soil is only 14.40% to phosphatic adsorption rate.Under room temperature, joined by 0.1g MD3 in the methylene blue solution of 25mL 50mg/L, vibration 120min, adsorption rate reaches 94.88%; Under the same terms, the adsorption rate of diatomite original soil to methylene blue is only 4.71%.
embodiment 4
(1) by 2.0g FeCl
36H
2o is dissolved in 40mL ethylene glycol, then adds 6.0g NaAc 3H
2o, form yellowish-brown clear solution, then add 20mL ethylenediamine, add the diatomite of 2.0g, magnetic agitation 30 min makes diatomite fully disperse, and obtains mixture;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), at 200 DEG C of reaction 8 h, has reacted rear cool to room temperature, got black solid;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding is crossed 100 mesh sieves, obtained magnetic diatomite MD4;
Under room temperature, joined by 0.1g MD4 in the phosphate solution of 25mL 20mg/L, vibration 120min, adsorption rate reaches 84.90%; Under the same terms, diatomite original soil is only 14.40% to phosphatic adsorption rate.Under room temperature, joined by 0.1g MD4 in the methylene blue solution of 25mL 50mg/L, vibration 120min, adsorption rate reaches 95.89%; Under the same terms, the adsorption rate of diatomite original soil to methylene blue is only 4.71%.
embodiment 5
(1) by 2.0g FeCl
36H
2o is dissolved in 40mL ethylene glycol, then adds 6.0g NaAc 3H
2o, form yellowish-brown clear solution, add the diatomite of 0.2g, magnetic agitation 30 min makes diatomite fully disperse, and obtains mixture;
(2) said mixture is encapsulated in the reactor of polytetrafluoroethylene (PTFE), at 200 DEG C of reaction 8 h, has reacted rear cool to room temperature, got black solid;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding is crossed 100 mesh sieves, obtained magnetic diatomite MD5;
Under room temperature, joined by 0.1g MD5 in the phosphate solution of 25mL 20mg/L, vibration 120min, adsorption rate reaches 53.72%; Under the same terms, diatomite original soil is only 14.40% to phosphatic adsorption rate.
Comparing embodiment 1 can draw with the experimental data of embodiment 5, when other conditions are identical, the absorption property of magnetic diatomite MD1 prepared by ethylenediamine is added in preparation process, apparently higher than, in preparation process, do not add the absorption property of magnetic diatomite MD5 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 diatomaceous amount, Fe and diatomaceous ratio (Fe
/diatomite) 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 MD1 is stronger than MD5, and in magnetic history, energy consumption is less; So, add ethylenediamine and can strengthen the diatomaceous superparamagnetic performance of magnetic, be reduced in energy loss in remagnetization process.
Claims (4)
1. the diatomaceous preparation method of magnetic, 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 adds diatomite powder mixing, magnetic agitation 30 min, obtains the mixture of diatomite dispersion;
(2) mixture is encapsulated in polytetrafluoroethylene (PTFE) reactor, at 200 DEG C of reaction more than 8h, gets black solid;
(3) washed by black solid, Magneto separate, dry, grinding, sieves, obtains magnetic diatomite.
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 diatomite powder is: 2.0g:40mL:6.0g:20mL:0.2-2.0g.
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 diatomite powder is: 2.0g:40mL:6.0g:20mL:0.2g.
4. the preparation method according to claim 1,2 or 3, is characterized in that, by FeCl
36H
2o is dissolved in ethylene glycol, then adds NaAc 3H
2o.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105413630A (en) * | 2016-01-21 | 2016-03-23 | 齐齐哈尔大学 | Magnetic medical stone composite adsorption material and preparing method thereof |
| CN107262033A (en) * | 2017-06-30 | 2017-10-20 | 安徽工业大学 | The preparation and application of a kind of attapulgite/Fe3O4/ carbon composites |
| CN108393064A (en) * | 2018-01-23 | 2018-08-14 | 吉林化工学院 | A kind of modification infusorial earth material and preparation method thereof of absorption dyestuff direct scarlet 4BS |
| CN109794080A (en) * | 2019-03-07 | 2019-05-24 | 中国科学院兰州化学物理研究所 | It is a kind of can magnetic recovery composite diatomite demulsifying material preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105413630A (en) * | 2016-01-21 | 2016-03-23 | 齐齐哈尔大学 | Magnetic medical stone composite adsorption material and preparing method thereof |
| CN107262033A (en) * | 2017-06-30 | 2017-10-20 | 安徽工业大学 | The preparation and application of a kind of attapulgite/Fe3O4/ carbon composites |
| CN108393064A (en) * | 2018-01-23 | 2018-08-14 | 吉林化工学院 | A kind of modification infusorial earth material and preparation method thereof of absorption dyestuff direct scarlet 4BS |
| CN109794080A (en) * | 2019-03-07 | 2019-05-24 | 中国科学院兰州化学物理研究所 | It is a kind of can magnetic recovery composite diatomite demulsifying material preparation method and application |
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| CN104826601B (en) | 2018-07-31 |
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