CN104826600A - Preparation method of magnetic kaolin - Google Patents
Preparation method of magnetic kaolin Download PDFInfo
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- CN104826600A CN104826600A CN201510222142.7A CN201510222142A CN104826600A CN 104826600 A CN104826600 A CN 104826600A CN 201510222142 A CN201510222142 A CN 201510222142A CN 104826600 A CN104826600 A CN 104826600A
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Abstract
The invention relates to a preparation method of magnetic kaolin and belongs to the field of water treatment technology and inorganic composite material and technology. The method comprises the following steps: mixing FeCl3.6H2O, NaAc.3H2O, ethanediol, ethidene diamine and kaolin to obtain a tawny suspension, sealing the tawny suspension into a teflon reaction kettle, reacting under the condition of 180-200 DEG C for more than 8 h, taking a black solid, washing, carrying out magnetic separation, drying, grinding, and sieving to obtain magnetic kaolin. 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 kaolin will not be damaged and adsorptive property of kaolin is guaranteed. The kaolin has a good effect of removing phosphate in water, and rapid solid-liquid separation can be realized after adsorption such that an adsorbent is separated from an adsorbent solution so as to be recycled.
Description
Technical field
The present invention relates to a kind of magnetic kleit preparation method, belong to water technology, inorganic composite materials and technical field.
Background technology
Kaolin is that one has layer structure clay mineral, be main component is kaolinic porous material.Kaolinite is dioctahedron 1:1 type layer silicate mineral, exists with atomic little crystallite or cryptocrystal state, and produces with compact massive or earthy aggregate, and chemical composition is: Al [Si
4o
10] (OH)
8, crystal belongs to triclinic layer silicate mineral.
Kaolin has huge specific area, good adsorption properties and ion-exchange performance.Have plasticity, higher fire resistance, good insulating properties and chemical stability, former research mainly concentrates on the fields such as pottery, refractory material, rubber, medicine, cosmetics.Because its particle surface has fine pore, having certain adsorptivity, is the adsorbent of a class high-quality cheapness, has now been widely used in a lot of field such as environmental protection, chemistry, agricultural.
In recent years, its application in field of waste water treatment of kaolinic Study on adsorption properties is utilized to achieve good effect, in order to improve kaolin absorption property further, researcher mainly adopts Physical or chemical method both at home and abroad at present, as the modes such as acidleach, roasting, organic intercalation, polyalcohol intercalation and inorganic-organic hybrid carry out modification to it, molecular sieve is made in the further processing also had, thus its surface nature and interlayer structure are changed, and increases its adsorption capacity.Modified kaolin has the physicochemical properties such as good plasticity, antiacid dissolubility, fire resistance, specific area be large because of it and is widely used.Extensive and good application is had in process phosphorous, heavy metal wastewater thereby, organic wastewater and waste water from dyestuff.
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 kaolin prepares magnetic kaolin material, and the method preparing magnetic kaolin material comprises coprecipitation and the large class of hydro-thermal method two.Wherein coprecipitation refers to that they exist in solution with homogeneous phase, add precipitating reagent in the solution containing two or more cations, after precipitation reaction, the homogeneous precipitation of various composition can be obtained, then precipitation is carried out drying and calcining, thus obtain high purity nanometer powders material.Such as CN103721671A discloses a kind of nano magnetic iron oxide/kaolin particle and its production and use: in the bath solution of polyethylene dissolving pyrrolidones, first add kaolin (NaOH regulates pH), then a certain amount of ferrous salt and molysite is added respectively, generation brownish black precipitates, and constantly adds alkali lye and regulate pH about 10 between the stage of reaction.Reaction final vacuum is dry, finally pulverizes the obtained nano magnetic iron oxide/kaolin particle that sieves.The coreshell type structure of this particle kernel and shell, its kernel is kaolin mineral, and shell is nano magnetic iron oxide (Fe
3o
4), efficiently can remove the polluters such as the arsenic in water body.
The preparation principle of hydro-thermal method refers in the pressure vessel of sealing (autoclave), and under the condition of HTHP, metal ion hydrolysis occurs in alkaline environment and forms metal oxide deposits, and this sediment purity is higher, and particle is thinner.Such as CN103566866A discloses a kind of method utilizing kaolin to prepare magnetic 4A molecular sieve: with Fe
3o
4for magnetic carrier, kaolin is as raw material, and aluminium hydroxide, for supplementing aluminium source, prepares the magnetic 4A molecular sieve of cheapness, high-performance, recoverable by hydrothermal synthesis method.The 4A magnetic zeolite Size of Zeolite of synthesis is thin, magnetic stability good, all has higher clearance to ammonia nitrogen and heavy metal contaminants.
Summary of the invention
The magnetic kleit preparation method that the object of the present invention is to provide that a kind of efficiency is high, technique is simple, there is stronger absorption property, and for removing water pollutant.
Technical scheme
A kind of magnetic kleit preparation method, 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 kaolin, obtain yellowish-brown suspension;
(2) suspension is packaged in polytetrafluoroethylene (PTFE) reactor, under 180-200 DEG C of condition, reacts more than 8h, get black solid;
(3) black solid through washing, Magneto separate, oven dry, grind, sieve, obtain magnetic kaolin.
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 tri-iron tetroxide of the homogeneous nanometer of compound particle size 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。
The ferroferric oxide nano granules of synthesis is combined with kaolin and forms magnetic kaolin.
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 kaolin participate in the kaolinic building-up process of magnetic, and the change of its consumption does not affect the generation of product, but can affect the kaolinic performance of prepared magnetic.Obtain the magnetic kaolin of higher magnetic, FeCl to reduce wastage of material simultaneously
36H
2o, ethylene glycol, NaAc 3H
2o, ethylenediamine and kaolinic usage ratio are preferably: 1.0 g:20 mL:3.0 g:10 mL:0.1-1.0 g; Most preferredly be: 1.0 g:20 mL:3.0 g:10 mL:0.4 g.
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 kaolin 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 of modifying temperature is low, can not destroy kaolinic structure, ensure that its absorption property;
(3) add ethylenediamine in preparation process, absorption property and the superparamagnetism of product can be significantly improved;
(4) to the phosphate in water, there is good removal effect; and the quick separating of solid-liquid can be realized after having adsorbed, adsorbent is separated from adsorbent solution, is recycled; part pollutant also can be recycled, and facilitates the sustainability of resource while protection of the environment.
Accompanying drawing explanation
Fig. 1 is magnetic kaolin of the present invention and kaolin original soil, Fe
3o
4the X-ray diffraction spectrogram of contrast; Wherein, A-E is followed successively by: kaolin original soil, Fe
3o
4, embodiment 2-4 the kaolinic X-ray diffraction spectrogram of magnetic.
Detailed description of the invention
embodiment 1
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, then adds 6.0 g NaAc 3H
2o and 20 mL ethylenediamines, add the kaolin of 0.2 g, stirs 30 min and make it fully disperse;
(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;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding, sieves, obtain magnetic kaolin MK1;
Under room temperature, joined by 0.1 g MK1 in the phosphate solution of 25 mL 20 mg/L, vibrate 120 min, and adsorption rate reaches 91.57%; Under the same terms, kaolin original soil is only 3.18% to phosphatic adsorption rate.
embodiment 2
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, then adds 6.0 g NaAc 3H
2o and 20 mL ethylenediamines, add the kaolin of 0.4 g, stirs 30 min and make it fully disperse;
(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;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding, sieves, obtain magnetic kaolin MK2;
Under room temperature, joined by 0.1 g MK2 in the phosphate solution of 25 mL 20 mg/L, vibrate 120 min, and adsorption rate reaches 91.39%; Under the same terms, kaolin original soil is only 3.18% to phosphatic adsorption rate.
embodiment 3
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, then adds 6.0 g NaAc 3H
2o and 20 mL ethylenediamines, add the kaolin of 0.8 g, stirs 30 min and make it fully disperse;
(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;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding, sieves, obtain magnetic kaolin MK3;
Under room temperature, joined by 0.1 g MK3 in the phosphate solution of 25 mL 20 mg/L, vibrate 120 min, and adsorption rate reaches 92.70%; Under the same terms, kaolin original soil is only 3.18% to phosphatic adsorption rate.
embodiment 4
(1) by 2.0 g FeCl
36H
2o is dissolved in 40mL ethylene glycol, then adds 6.0 g NaAc 3H
2o and 20 mL ethylenediamines, add the kaolin of 2.0 g, stirs 30 min and make it fully disperse;
(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;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding, sieves, obtain magnetic kaolin MK4;
Under room temperature, joined by 0.1 g MK4 in the phosphate solution of 25 mL 20 mg/L, vibrate 120 min, and adsorption rate reaches 89.70%; Under the same terms, kaolin original soil is only 3.18% to phosphatic adsorption rate.
embodiment 5
(1) by 2.0 g FeCl
36H
2o is dissolved in 40 mL ethylene glycol, then adds 6.0 g NaAc 3H
2o, then the kaolin adding 0.8 g, stir 30 min and make it fully disperse;
(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;
(3) the black solid distilled water washing several will obtained, Magneto separate, dries, and grinding, sieves, obtain magnetic kaolin MK5;
Under room temperature, joined by 0.1 g MK5 in the phosphate solution of 25 mL 20 mg/L, vibrate 120 min, and adsorption rate reaches 38.90%.
Comparing embodiment 3 can draw with the experimental data of embodiment 5, when other conditions are identical, the absorption property of magnetic kaolin MK3 prepared by ethylenediamine is added in preparation process, apparently higher than, in preparation process, do not add the absorption property of magnetic kaolin MK5 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 kaolinic amount, Fe and kaolinic ratio (Fe
/kaolin) 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 MK3 is stronger than MK5, and in magnetic history, energy consumption is less; So, add ethylenediamine and can strengthen the kaolinic superparamagnetic performance of magnetic, be reduced in energy loss in remagnetization process.
Claims (4)
1. a magnetic kleit preparation method, 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 kaolin, obtain yellowish-brown suspension;
(2) suspension is packaged in polytetrafluoroethylene (PTFE) reactor, under 180-200 DEG C of condition, reacts more than 8h, get black solid;
(3) black solid through washing, Magneto separate, oven dry, grind, sieve, obtain magnetic kaolin.
2. preparation method according to claim 1, is characterized in that, FeCl
36H
2o, ethylene glycol, NaAc 3H
2o, ethylenediamine and kaolinic usage ratio are: 1.0 g:20 mL:3.0 g:10 mL:0.1-1.0 g.
3. preparation method according to claim 1, is characterized in that, FeCl
36H
2o, ethylene glycol, NaAc 3H
2o, ethylenediamine and kaolinic usage ratio are: 1.0 g:20 mL:3.0 g:10 mL:0.4 g.
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 (7)
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| CN105413630A (en) * | 2016-01-21 | 2016-03-23 | 齐齐哈尔大学 | Magnetic medical stone composite adsorption material and preparing method thereof |
| CN106693886A (en) * | 2016-12-27 | 2017-05-24 | 高州市兆翔新材料有限公司 | Preparation method of magnetic nanometer kaolin for underground water treatment |
| CN110180497A (en) * | 2019-05-27 | 2019-08-30 | 广西壮族自治区农业科学院 | The preparation method of the magnetic material of methyl blue in a kind of absorption effluent |
| CN111389376A (en) * | 2020-03-03 | 2020-07-10 | 苏州科技大学 | Polypyrrole-modified magnetic kaolin nanocomposite and preparation method and application thereof |
| CN111547777A (en) * | 2020-05-22 | 2020-08-18 | 昆明理工大学 | Method for removing arsenic in contaminated acid by ferroferric oxide/kaolin nanocomposite |
| CN114700058A (en) * | 2022-04-29 | 2022-07-05 | 新疆师范大学 | Preparation method of porous magnetic composite adsorbent and application of porous magnetic composite adsorbent in adsorption of dimethylarsinic acid |
| CN116040731A (en) * | 2023-01-31 | 2023-05-02 | 广东名桂环保有限公司 | Composite water treatment agent and preparation method thereof |
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| CN105413630A (en) * | 2016-01-21 | 2016-03-23 | 齐齐哈尔大学 | Magnetic medical stone composite adsorption material and preparing method thereof |
| CN106693886A (en) * | 2016-12-27 | 2017-05-24 | 高州市兆翔新材料有限公司 | Preparation method of magnetic nanometer kaolin for underground water treatment |
| CN110180497A (en) * | 2019-05-27 | 2019-08-30 | 广西壮族自治区农业科学院 | The preparation method of the magnetic material of methyl blue in a kind of absorption effluent |
| CN111389376A (en) * | 2020-03-03 | 2020-07-10 | 苏州科技大学 | Polypyrrole-modified magnetic kaolin nanocomposite and preparation method and application thereof |
| CN111547777A (en) * | 2020-05-22 | 2020-08-18 | 昆明理工大学 | Method for removing arsenic in contaminated acid by ferroferric oxide/kaolin nanocomposite |
| CN111547777B (en) * | 2020-05-22 | 2022-01-28 | 昆明理工大学 | Method for removing arsenic in contaminated acid by ferroferric oxide/kaolin nanocomposite |
| CN114700058A (en) * | 2022-04-29 | 2022-07-05 | 新疆师范大学 | Preparation method of porous magnetic composite adsorbent and application of porous magnetic composite adsorbent in adsorption of dimethylarsinic acid |
| CN114700058B (en) * | 2022-04-29 | 2023-09-19 | 新疆师范大学 | Preparation method of porous magnetic composite adsorbent and application of porous magnetic composite adsorbent in adsorption of dimethyl arsonic acid |
| CN116040731A (en) * | 2023-01-31 | 2023-05-02 | 广东名桂环保有限公司 | Composite water treatment agent and preparation method thereof |
| CN116040731B (en) * | 2023-01-31 | 2023-11-10 | 广东名桂环保有限公司 | Composite water treatment agent and preparation method thereof |
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