CN108579681A - CTAB adulterates Fe3S4Magnetic environment repair materials and its preparation method and application - Google Patents
CTAB adulterates Fe3S4Magnetic environment repair materials and its preparation method and application Download PDFInfo
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- CN108579681A CN108579681A CN201810219311.5A CN201810219311A CN108579681A CN 108579681 A CN108579681 A CN 108579681A CN 201810219311 A CN201810219311 A CN 201810219311A CN 108579681 A CN108579681 A CN 108579681A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Chemical Kinetics & Catalysis (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a kind of CTAB to adulterate Fe3S4Magnetic environment repair materials and its preparation method and application, step is：By FeCl3·6H2O is dissolved in by certain mol proportion in the ethylene glycol of certain volume with thiocarbamide, and magnetic agitation is until form cochineal solution；0.6 ~ 2.4mmol CTAB are added in above-mentioned solution, and stir 10 ~ 30min of ultrasound；By reaction system at 160 ~ 200 DEG C hydro-thermal reaction；It is cooled to room temperature, dry under vacuum, grinding, obtains the magnetic environment repair materials after products therefrom cleaning.Magnetic environment repair materials prepared by the present invention have good magnetic property and stronger adsorption capacity, can adsorb other methods in water and be difficult to the heavy metal removed.
Description
Technical field
The present invention relates to a kind of ecological restoration materials and its preparation method and application of heavy metal in removal water body environment, belong to
In environment remediation field.
Background technology
Currently, the synthesis and application for ferriferrous sulfide are mainly in chemical property, biomedicine, feed addictive
Degradation etc., it is seldom in the research of environmental area application to it, still it is in the Primary Study stage.Kong et al. is by beta-cyclodextrin
For magnetic Fe3S4The stabilisation of nano particle, and it is applied to the removal of heavy metal Pb, removal mechanisms at work is chemical precipitation（Shape
At galena）And adsorption（Kong L, Yan L, Qu Z, et al. β-Cyclodextrin stabilized
magnetic Fe3S4 nanoparticles for efficient removal of Pb(II)[J]. Journal of
Materials Chemistry A, 2015, 3(30):15755-15763.）；Mahamudur Islam et al. pass through hydro-thermal
Method prepares Fe3S4Polypyrrole（GPPy）Nano-complex, and it is applied to the removal of arsenious acid and arsenate（Islam M,
Patel R. Solvothermal synthesis of greigite (Fe3S4)– Conducting polypyrrole
nanocomposite and its application towards arsenic removal[J]. Separation
Science & Technology, 2017.）；Feng Mei etc. are by β-CD and PEG for controlling Fe3S4Crystal form and pattern, with
And by prepared magnetic nano crystal（GMNCs）It is applied in biomedical sector（Feng M, Lu Y, Yang Y, et
al. Bioinspired greigite magnetic nanocrystals: chemical synthesis and
biomedicine applications[J]. Scientific Reports, 2013, 3(10):2994.）.In recent years, positive
Application of the ionic surface active agent in terms of anion heavy metals removal gradually increases, and suitable surfactant can improve
Fe3S4Purity and stability.
But by Fe3S4Reduction adsorption applied to Cr VI rarely has discussion, does not also adulterate Fe about CTAB at present3S4
Remove the report of Cr VI.
Invention content
The object of the present invention is to provide a kind of CTAB to adulterate Fe3S4Magnetic environment repair materials and preparation method thereof, make
Absorption for ecological restoration material for heavy metal in environment, removal capacity is big, thus is with a wide range of applications.
Realizing the technical solution of the object of the invention is：A kind of CTAB doping Fe3S4Magnetic environment repair materials and its
Preparation method, step are：
The first step：By FeCl3·6H2O is mixed with thiocarbamide, and is dissolved in ethylene glycol and is formed mixed liquor；
Second step：Cetyl trimethyl ammonium (CTAB) is added in above-mentioned mixed liquor, and a period of time is stirred by ultrasonic；
Third walks：By second step reaction system at 160 ~ 200 DEG C hydro-thermal reaction；
4th step：It is cooled to room temperature, dry under vacuum, grinding, obtains the magnetic environment after products therefrom cleaning
Repair materials.
Further, in the first step, the FeCl in mixed liquor3·6H2The molar ratio 0.5 ~ 1.0 of O and thiocarbamide.
Further, in second step, the input amount and FeCl of CTAB3·6H2The molar ratio of O is 0.20 ~ 0.80, and ultrasound is stirred
It is 10 ~ 30min to mix the time.
Further, in third step, the hydro-thermal reaction time is 12 ~ 15 hours.
Further, in the 4th step, 3 ~ 5 cleanings are carried out to products therefrom with ethyl alcohol and deionized water；Drying temperature is
60℃。
Compared with prior art, the beneficial effects of the invention are as follows：
（1）Synthesis technology of the present invention is simple, and production cost is low, is conducive to the large-scale production of low cost.
（2）Using magnetic Fe3S4As the adsorbent of heavy metal in solution, there is larger adsorption capacity, and be easy to point
From being conducive to the processing of high concentration heavy metal polluted waste water.
（3）Using CTAB as the dopant in repair materials building-up process, be conducive to improve Fe3S4Purity and stabilization
Property.
Description of the drawings
Fig. 1 is the prepared Fe in comparative example 1 of the present invention and embodiment 1 ~ 43S4And Fe3S4-CTAB0.6~2.4Flied emission
Scanning electron microscope (SEM) photograph（A is Fe3S4, b Fe3S4-CTAB0.6, c Fe3S4-CTAB1.2, d Fe3S4-CTAB1.8, e Fe3S4-
CTAB2.4）.
Fig. 2 is the prepared Fe in comparative example 1 of the present invention and embodiment 1 ~ 43S4And Fe3S4-CTAB0.6~2.4Magnetic hysteresis return
Line chart.
Fig. 3 is the removal efficiency figure of material prepared in comparative example 1 of the present invention and embodiment 1 ~ 4 to Cr (VI).
Specific implementation mode
Comparative example 1
The first step, by FeCl3·6H2O presses 1 with thiocarbamide：2 molar ratios are dissolved in the ethylene glycol of certain volume, and magnetic agitation 20 ~
30min is until form cochineal solution；
First step reaction system is transferred to closed reaction vessel by second step（Autoclave）In；
Third walks, and the autoclave in second step is put into baking oven, and baking oven is warming up to 180 DEG C of reaction temperature, create high temperature,
Reaction under high pressure environment, maintains constant temperature 12 hours；
The reaction system that third walks is cooled to room temperature by the 4th step, and products therefrom is cleaned with ethyl alcohol and deionized water, and in vacuum
Under the conditions of it is dry, magnetic environment repair materials Fe is obtained after grinding3S4, shown in scanning electron microscope (SEM) photograph such as Fig. 1 (a), hysteresis loop
Figure is as shown in Figure 2.
Take the Fe of 15mg3S4With 50mL hexavalent chromium solutions, it is added into 150mL conical flasks, vibrates 1.0 h at room temperature.Six
Valence chromium solution concentration：100mg/L.As shown in figure 3, experiment measures the removal rate about 70% of Cr VI.
Embodiment 1
The first step, by FeCl3·6H2O presses 1 with thiocarbamide：2 molar ratios are dissolved in the ethylene glycol of certain volume, and magnetic agitation 20 ~
30min is until form cochineal solution；
The cetyl trimethyl ammonium (CTAB) of 0.6mmol is added in above-mentioned mixed liquor second step, and is stirred by ultrasonic one section
Time；
Third walks, and second step reaction system is transferred to closed reaction vessel（Autoclave）In；
4th step, the autoclave during third is walked are put into baking oven, and baking oven is warming up to 180 DEG C of reaction temperature, create high temperature,
Reaction under high pressure environment, maintains constant temperature 12 hours；
The reaction system of 4th step is cooled to room temperature by the 5th step, and products therefrom is cleaned with ethyl alcohol and deionized water, and in vacuum
Under the conditions of it is dry, magnetic environment repair materials Fe is obtained after grinding3S4-CTAB0.6, shown in scanning electron microscope (SEM) photograph such as Fig. 1 (b),
Hysteresis loop figure is as shown in Figure 2.
Take the Fe of 15mg3S4-CTAB0.6With 50mL hexavalent chromium solutions, it is added into 150mL conical flasks, vibrates at room temperature
1.0 h.Hexavalent chromium solution concentration：100mg/L.As shown in Fig. 2, experiment measures the removal rate about 84% of Cr VI.
Embodiment 2
The first step, by FeCl3·6H2O presses 1 with thiocarbamide：2 molar ratios are dissolved in the ethylene glycol of certain volume, and magnetic agitation 20 ~
30min is until form cochineal solution；
The cetyl trimethyl ammonium (CTAB) of 1.2mmol is added in above-mentioned mixed liquor second step, and is stirred by ultrasonic one section
Time；
Third walks, and second step reaction system is transferred to closed reaction vessel（Autoclave）In；
4th step, the autoclave during third is walked are put into baking oven, and baking oven is warming up to 180 DEG C of reaction temperature, create high temperature,
Reaction under high pressure environment, maintains constant temperature 12 hours；
The reaction system of 4th step is cooled to room temperature by the 5th step, and products therefrom is cleaned with ethyl alcohol and deionized water, and in vacuum
Under the conditions of it is dry, magnetic environment repair materials Fe is obtained after grinding3S4-CTAB1.2, shown in scanning electron microscope (SEM) photograph such as Fig. 1 (c),
Hysteresis loop figure is as shown in Figure 2.
Take the Fe of 15mg3S4-CTAB1.2With 50mL hexavalent chromium solutions, it is added into 150mL conical flasks, vibrates at room temperature
1.0 h.Hexavalent chromium solution concentration：100mg/L.As shown in figure 3, experiment measures the removal rate about 91% of Cr VI.
Embodiment 3
The first step, by FeCl3·6H2O presses 1 with thiocarbamide：2 molar ratios are dissolved in the ethylene glycol of certain volume, and magnetic agitation 20 ~
30min is until form cochineal solution；
The cetyl trimethyl ammonium (CTAB) of 1.8mmol is added in above-mentioned mixed liquor second step, and is stirred by ultrasonic one section
Time；
Third walks, and second step reaction system is transferred to closed reaction vessel（Autoclave）In；
4th step, the autoclave during third is walked are put into baking oven, and baking oven is warming up to 180 DEG C of reaction temperature, create high temperature,
Reaction under high pressure environment, maintains constant temperature 12 hours；
The reaction system of 4th step is cooled to room temperature by the 5th step, and products therefrom is cleaned with ethyl alcohol and deionized water, and in vacuum
Under the conditions of it is dry, magnetic environment repair materials Fe is obtained after grinding3S4-CTAB1.8, shown in scanning electron microscope (SEM) photograph such as Fig. 1 (d),
Hysteresis loop figure is as shown in Figure 2.
Take the Fe of 15mg3S4-CTAB1.8With 50mL hexavalent chromium solutions, it is added into 150mL conical flasks, vibrates at room temperature
1.0 h.Hexavalent chromium solution concentration：100mg/L.As shown in figure 3, experiment measures the removal rate about 94% of Cr VI.
Embodiment 4
The first step, by FeCl3·6H2O presses 1 with thiocarbamide：2 molar ratios are dissolved in the ethylene glycol of certain volume, and magnetic agitation 20 ~
30min is until form cochineal solution；
The cetyl trimethyl ammonium (CTAB) of 2.4mmol is added in above-mentioned mixed liquor second step, and is stirred by ultrasonic one section
Time；
Third walks, and second step reaction system is transferred to closed reaction vessel（Autoclave）In；
4th step, the autoclave during third is walked are put into baking oven, and baking oven is warming up to 180 DEG C of reaction temperature, create high temperature,
Reaction under high pressure environment, maintains constant temperature 12 hours；
The reaction system of 4th step is cooled to room temperature by the 5th step, and products therefrom is cleaned with ethyl alcohol and deionized water, and in vacuum
Under the conditions of it is dry, magnetic environment repair materials Fe is obtained after grinding3S4-CTAB2.4, shown in scanning electron microscope (SEM) photograph such as Fig. 1 (e),
Hysteresis loop figure is as shown in Figure 2.
Take the Fe of 15mg3S4-CTAB2.4With 50mL hexavalent chromium solutions, it is added into 150mL conical flasks, vibrates at room temperature
1.0 h.Hexavalent chromium solution concentration：100mg/L.As shown in figure 3, experiment measures the removal rate about 84% of Cr VI.
Embodiment 5
The first step, by FeCl3·6H2O presses 1 with thiocarbamide：2 molar ratios are dissolved in the ethylene glycol of certain volume, and magnetic agitation 20 ~
30min is until form cochineal solution；
The cetyl trimethyl ammonium (CTAB) of 1.8mmol is added in above-mentioned mixed liquor second step, and is stirred by ultrasonic one section
Time；
Third walks, and second step reaction system is transferred to closed reaction vessel（Autoclave）In；
4th step, the autoclave during third is walked are put into baking oven, and baking oven is warming up to 180 DEG C of reaction temperature, create high temperature,
Reaction under high pressure environment, maintains constant temperature 12 hours；
The reaction system of 4th step is cooled to room temperature by the 5th step, and products therefrom is cleaned with ethyl alcohol and deionized water, and in vacuum
Under the conditions of it is dry, magnetic environment repair materials Fe is obtained after grinding3S4-CTAB1.8。
Take the Fe of 15mg3S4-CTAB1.8With 50mL hexavalent chromium solutions, it is added into 150mL conical flasks, vibrates at room temperature
1.0 h.Configuring hexavalent chromium solution initial concentration is respectively：100,125,150,200,250,300mg/L.Experimental result meets
Langmuir adsorption isotherms, maximum adsorption capacity 330.03mg/g.
Claims (8)
1.CTAB adulterates Fe3S4Magnetic environment repair materials preparation method, which is characterized in that include the following steps：
The first step：By FeCl3·6H2O is mixed with thiocarbamide, and is dissolved in ethylene glycol and is formed mixed liquor；
Second step：CTAB is added in above-mentioned mixed liquor, and a period of time is stirred by ultrasonic；
Third walks：By second step reaction system at 160 ~ 200 DEG C hydro-thermal reaction；
4th step：It is cooled to room temperature, dry under vacuum, grinding, obtains the magnetic environment after products therefrom cleaning
Repair materials.
2. preparation method as described in claim 1, which is characterized in that in the first step, the FeCl in mixed liquor3·6H2O and sulphur
The molar ratio 0.5 ~ 1.0 of urea.
3. preparation method as described in claim 1, which is characterized in that in second step, the input amount and FeCl of CTAB3·6H2O
Molar ratio be 0.20 ~ 0.80, the ultrasonic agitation time be 10 ~ 30min.
4. preparation method as described in claim 1, which is characterized in that in third step, the hydro-thermal reaction time is 12 ~ 15 hours.
5. preparation method as described in claim 1, which is characterized in that in the 4th step, produced to gained with ethyl alcohol and deionized water
Object carries out 3 ~ 5 cleanings；Drying temperature is 60 DEG C.
6. CTAB prepared by the preparation method as described in claim 1 ~ 5 is any adulterates Fe3S4Magnetic environment repair materials.
7. CTAB prepared by the preparation method as described in claim 1 ~ 5 is any adulterates Fe3S4Magnetic environment repair materials going
Except the application in water body environment on heavy metal.
8. the use as claimed in claim 7, which is characterized in that the heavy metal is Cr VI.
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| CN201810219311.5A CN108579681B (en) | 2018-03-16 | 2018-03-16 | CTAB doped Fe3S4Magnetic environment repairing material and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114870870A (en) * | 2022-04-29 | 2022-08-09 | 成都理工大学 | Magnetic environment purifying material for co-processing MO and Cr (VI) pollution and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874879A (en) * | 2012-10-12 | 2013-01-16 | 中国科学技术大学 | Preparation method for Fe3S4 nanocrystalline material |
| US20160060140A1 (en) * | 2012-10-12 | 2016-03-03 | Advantageous Systems Llc | Immobilization of particles on a matrix |
-
2018
- 2018-03-16 CN CN201810219311.5A patent/CN108579681B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874879A (en) * | 2012-10-12 | 2013-01-16 | 中国科学技术大学 | Preparation method for Fe3S4 nanocrystalline material |
| US20160060140A1 (en) * | 2012-10-12 | 2016-03-03 | Advantageous Systems Llc | Immobilization of particles on a matrix |
Non-Patent Citations (2)
| Title |
|---|
| MAHAMUDUR ISLAM ET AL.: "Solvothermal synthesis of greigite (Fe3S4)-Conducting polypyrrole nanocomposite and its application towards arsenic removal", 《SEPARATION SCIENCE AND TECHNOLOGY》 * |
| 凌丹 等: "羧甲基纤维素钠辅助磁性Fe3S4纳米复合物的合成及其吸附与吸波性质研究", 《化学通报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114870870A (en) * | 2022-04-29 | 2022-08-09 | 成都理工大学 | Magnetic environment purifying material for co-processing MO and Cr (VI) pollution and preparation method thereof |
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