CN112427028A - Cetyl trimethyl ammonium bromide modified nano iron lanthanum material, preparation method and application - Google Patents

Cetyl trimethyl ammonium bromide modified nano iron lanthanum material, preparation method and application Download PDF

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CN112427028A
CN112427028A CN202011304563.1A CN202011304563A CN112427028A CN 112427028 A CN112427028 A CN 112427028A CN 202011304563 A CN202011304563 A CN 202011304563A CN 112427028 A CN112427028 A CN 112427028A
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trimethyl ammonium
ammonium bromide
solution
hexadecyl trimethyl
iron lanthanum
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谢燕华
姜飞
罗婷
吴桐
唐勇
王波
韩学威
陈浪
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Chengdu Univeristy of Technology
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Abstract

The invention relates to a hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material, a preparation method and application thereof, and the preparation method comprises the following steps: a. respectively weighing LaCl3·nH2O and Fe (NO)3)3·7H2O is put in deionized water and is stirred and mixed fully by magnetic force; b. adding a hexadecyl trimethyl ammonium bromide solution, magnetically stirring for 2 hours, then adjusting the pH value of the mixed solution to 6 by using a NaOH solution to obtain iron lanthanum hydroxide precipitate, and magnetically stirring for 24 hours; c. centrifuging the solution, and washing with deionized water until the filtrate contains no chlorine and nitrate; d. drying at 60 deg.C for 12 hr, taking out, cooling to room temperature, placing into ceramic grinding bowlAnd grinding the mixture into powder particles to obtain the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material. The underground water defluorination method provided by the invention has the advantages of low cost, simple preparation process, simple and convenient operation, good defluorination effect, recyclability and better popularization and application prospects.

Description

Cetyl trimethyl ammonium bromide modified nano iron lanthanum material, preparation method and application
Technical Field
The invention relates to the field of preparation of inorganic metal oxide nano composite materials, in particular to a hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material, a preparation method and application thereof.
Technical Field
For a long time, the pollution of fluorine in water has been of great concern because the concentration of fluoride in water is too high to cause various body diseases such as dental fluorosis, fluoroossium, brain injury and thyroid disease. Therefore, the national health organization strictly regulates that the maximum allowable concentration of fluoride in drinking water is 1.5 mg/L. However, it is statistical that the fluoride content of drinking water in many countries and regions of the world exceeds the standards set by the world health organization, and poses a serious threat to the health of animals and plants, as well as humans, particularly in some parts of india, china, the middle of africa, and south america. Therefore, the fluoride is quickly and effectively removed, and the method is very important for guaranteeing the safety of drinking water and the sustainable development of water resources.
At present, the commonly used defluorination methods mainly include precipitation, adsorption, electrocoagulation, ion exchange, reverse osmosis, electrodialysis, and the like. Among them, the adsorption method is considered to be a promising fluorine removal technology due to its advantages of stable water discharge, simple process, good selectivity, low maintenance cost, etc. The feasibility of this technique depends to a large extent on the development of suitable adsorbent materials, such as aluminium-based oxide adsorbents, iron-based adsorbents, and carbon-based adsorbents. However, many limitations of water adsorption capacity have hindered their practical application in fluoride removal. Therefore, the development of an efficient and expandable adsorbent for improving the removal rate of fluorine from drinking water is urgent.
In recent years, nano iron oxide or hydroxide thereof has received much attention as a material for removing fluorine in water. Meanwhile, rare earth metal adsorbents such as lanthanide adsorbents have strong chemical attraction of fluoride ions. Therefore, it is feasible to select the nano iron lanthanum oxide as the fluoride adsorbing material, but the shape, size and dispersion of the bimetallic oxide particles are uneven, which may cause unstable fluorine adsorbing efficiency and poor adsorbing capacity. The surfactant-assisted precipitation method can simultaneously adjust the dispersibility and the particle size of the particles. Cetyl Trimethyl Ammonium Bromide (CTAB) is a cationic surfactant and has wide application prospect in the aspect of preparing homogeneous nanorods or particles. Therefore, by using CTAB as the surfactant of the lanthanum-doped mixed phase iron oxide nanoparticles, the obtained material has high fluorine removal efficiency and more uniform adsorption.
Disclosure of Invention
The invention provides a hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material, a preparation method and application thereof, and the modified nano iron lanthanum material prepared by the invention is used as an inorganic nano composite material adsorbent and has excellent adsorption performance on fluorine, such as large adsorption capacity; the adsorption rate is high; is not sensitive to pH; the application range is wide; NaOH solution can be used as regeneration liquid, so that the regeneration performance is good, and the regeneration liquid can be repeatedly used; has the characteristics of simple preparation process and good dispersibility.
The invention is realized by the following technical scheme:
the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material is prepared by the following preparation method, and comprises the following steps:
a. respectively weighing LaCl according to a certain mass ratio3·nH2O and Fe (NO)3)3·7H2O is put in deionized water and is stirred and mixed fully by magnetic force;
b. adding 5ml of Cetyl Trimethyl Ammonium Bromide (CTAB) solution, magnetically stirring for 2h, adjusting the pH value of the mixed solution to 6 by using NaOH solution to obtain iron lanthanum hydroxide mixed precipitate, and magnetically stirring for 24 h;
c. the solution was centrifuged, and the supernatant was removed and washed with deionized water.
d. Drying at 60 ℃ for 12h, taking out the material, cooling to room temperature, grinding in a ceramic grinding bowl to obtain granular hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material.
In the step a, LaCl3·nH2O and Fe (NO)3)3·7H2Selecting O with the mass ratio of 0.4: 1-0.5: 1, and weighing LaCl with corresponding mass3·nH2O and Fe (NO)3)3·7H2Dissolving O in deionized water by ultrasonic wave, and stirring for 5min on a magnetic stirrer at 25 deg.C.
In the step b, the concentration of a Cetyl Trimethyl Ammonium Bromide (CTAB) solution is 0.1 mol/L.
In the step b, the concentration of the NaOH solution is 4mol/L, the stirring speed is increased, and the stirring is carried out for 24 hours.
In the step c, the filtrate is washed by deionized water until the filtrate does not contain chlorine (0.01 mol/L AgNO is used)3Solution detection) and nitrate (nitrate qualitative loop experimental detection).
The application of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material is used for removing fluoride in water.
And (2) regenerating the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material, adding the modified nano iron lanthanum material adsorbing fluorine ions into an alkaline solution, oscillating for 120min, filtering and separating to obtain a fluorine ion-containing recovery solution, cleaning the separated material with deionized water, and drying to obtain the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material.
The alkaline solution is 0.01mol/L NaOH aqueous solution.
The beneficial effects of the invention are mainly embodied in the following aspects:
1. the hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material prepared by the invention selects hexadecyl trimethyl ammonium bromide as a surfactant, and the size and the dispersibility of the material can be controlled. The composite material has a synergistic effect and is rich in hydroxyl functional groups, so that the adsorption capacity of the material is effectively improved;
2. the invention has large exchange capacity for fluorine, simple process, large-scale production, stable water outlet, higher adsorption capacity after regeneration and cyclic utilization. Is suitable for areas drinking high-fluorine underground water for a long time, and is expected to be widely applied to underground water pollution remediation engineering.
3. The material prepared by the invention can be desorbed and regenerated by NaOH solution, has good regeneration performance, can be repeatedly utilized, and has good economic effect.
Drawings
FIG. 1(a) is La of an example3+With Fe3+Influence relation between concentration ratio and CTAB volume on fluorine adsorption quantity;
FIG. 1(b) is La of an example3+With Fe3+The concentration ratio and the pH value influence the fluorine removal rate;
FIG. 1(c) is a graph showing the effect of pH on the fluorine adsorption amount in examples;
FIG. 2 is a graph of the reusability of the cetyltrimethylammonium bromide modified nano iron lanthanum material of the embodiment (material addition amount is 1 g/L).
Detailed Description
For better understanding of the present invention, the following examples are provided to further illustrate the present invention, but the present invention is not limited to the following examples.
Example 1:
a preparation method of a hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material comprises the following steps:
a. respectively weighing LaCl according to a certain mass ratio3·nH2O and Fe (NO)3)3·7H2O is put into 100ml deionized water and is stirred and mixed fully by magnetic force;
b. adding 5ml of Cetyl Trimethyl Ammonium Bromide (CTAB) solution, magnetically stirring for 2h, adjusting the pH value of the mixed solution to 6 by using NaOH solution to obtain iron lanthanum hydroxide mixed precipitate, and magnetically stirring for 24 h;
c. the solution was centrifuged, and the supernatant was removed and washed with deionized water.
d. Drying at 60 ℃ for 12h, taking out the material, cooling to room temperature, grinding in a ceramic grinding bowl to obtain granular hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material.
In the step a, LaCl3·nH2O and Fe (NO)3)3·7H2Selecting O with the mass ratio of 0.01:1, 0.05:1, 0.1:1, 0.2:1, 0.4:1, 0.6:1 and 0.8:1 respectively, and weighing LaCl with corresponding mass3·nH2O and Fe (NO)3)3·7H2Dissolving O in deionized water with a certain volume by ultrasonic wave, and stirring for 5min on a magnetic stirrer at the mixing temperature of 25 ℃.
In the step b, the concentration of a Cetyl Trimethyl Ammonium Bromide (CTAB) solution is 0.1 mol/L.
In the step b, the concentration of the NaOH solution is 4mol/L, the stirring speed is increased, and the stirring is carried out for 24 hours.
In the step c, the filtrate is washed by deionized water until the filtrate does not contain chlorine (0.01 mol/L AgNO is used)3Solution detection) and nitrate (nitrate qualitative loop experimental detection).
The application of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material comprises the steps of respectively adding different prepared modified nano iron lanthanum materials into a solution which contains 10mg/L of fluorine and has the pH value of 6-7 to carry out an adsorption experiment, wherein the adding amount of the materials is 1g/L, reacting in a gas bath constant temperature oscillation box at the temperature of 25 +/-1 ℃ and the rpm of 200 to reach adsorption balance, and then, monitoring and analyzing experimental data to select the optimal preparation factor.
Example 2:
a. respectively weighing LaCl according to a certain mass ratio3·nH2O and Fe (NO)3)3·7H2O is put into 100ml deionized water and is stirred and mixed fully by magnetic force;
b. respectively adding 1ml, 3ml, 5ml, 10ml and 20ml of Cetyl Trimethyl Ammonium Bromide (CTAB) solution, magnetically stirring for 2h, adjusting the pH value of the mixed solution to 6 by using NaOH solution to obtain iron lanthanum hydroxide mixed precipitate, and magnetically stirring for 24 h;
c. the solution was centrifuged, and the supernatant was removed and washed with deionized water.
d. Drying at 60 ℃ for 12h, taking out the material, cooling to room temperature, grinding in a ceramic grinding bowl to obtain granular hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material.
In the step a, LaCl3·nH2O and Fe (NO)3)3·7H2Selecting O with the mass ratio of 0.4:1 respectively, and weighing LaCl with corresponding mass3·nH2O and Fe (NO)3)3·7H2Dissolving O in 100ml deionized water by ultrasonic, and stirring for 5min on a magnetic stirrer at 25 ℃.
In the step b, the concentration of a Cetyl Trimethyl Ammonium Bromide (CTAB) solution is 0.1 mol/L.
In the step b, the concentration of the NaOH solution is 4mol/L, the stirring speed is increased, and the stirring is carried out for 24 hours.
In the step c, the filtrate is washed by deionized water until the filtrate does not contain chlorine (0.01 mol/L AgNO is used)3Solution detection) and nitrate (nitrate qualitative loop experimental detection).
The application of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material comprises the steps of respectively adding different prepared modified nano iron lanthanum materials into a solution which contains 10mg/L of fluorine and has the pH value of 6-7 to carry out an adsorption experiment, wherein the adding amount of the materials is 1g/L, reacting in a gas bath constant temperature oscillation box at the temperature of 25 +/-1 ℃ and the rpm of 200 to reach adsorption balance, and then, monitoring and analyzing experimental data to select the optimal preparation factor.
Example 3:
a. respectively weighing LaCl according to a certain mass ratio3·nH2O and Fe (NO)3)3·7H2O is put into 100ml deionized water and is stirred and mixed fully by magnetic force;
b. adding 5ml of Cetyl Trimethyl Ammonium Bromide (CTAB) solution, magnetically stirring for 2h, adjusting the pH value of the mixed solution to 4, 6, 7, 8, 9, 10, 11 and 12 respectively by using NaOH solution to obtain iron lanthanum hydroxide mixed precipitate, and magnetically stirring for 24 h;
c. the solution was centrifuged, and the supernatant was removed and washed with deionized water.
d. Drying at 60 ℃ for 12h, taking out the material, cooling to room temperature, grinding in a ceramic grinding bowl to obtain granular hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material.
In the step a, LaCl3·nH2O and Fe (NO)3)3·7H2Selecting O with the mass ratio of 0.4:1 respectively, and weighing LaCl with corresponding mass3·nH2O and Fe (NO)3)3·7H2Dissolving O in 100ml deionized water by ultrasonic, and stirring for 5min on a magnetic stirrer at 25 ℃.
In the step b, the concentration of a Cetyl Trimethyl Ammonium Bromide (CTAB) solution is 0.1 mol/L.
In the step b, the concentration of the NaOH solution is 4mol/L, the stirring speed is increased, and the stirring is carried out for 24 hours.
In the step c, the filtrate is washed by deionized water until the filtrate does not contain chlorine (0.01 mol/L AgNO is used)3Solution detection) and nitrate (nitrate qualitative loop experimental detection).
The application of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material comprises the steps of respectively adding different prepared modified nano iron lanthanum materials into a solution which contains 10mg/L of fluorine and has the pH value of 6-7 to carry out an adsorption experiment, wherein the adding amount of the materials is 1g/L, reacting in a gas bath constant temperature oscillation box at the temperature of 25 +/-1 ℃ and the rpm of 200 to reach adsorption balance, and then, monitoring and analyzing experimental data to select the optimal preparation factor.
Example 4:
a. respectively weighing LaCl according to a certain mass ratio3·nH2O and Fe (NO)3)3·7H2O is put into 100ml deionized water and is stirred and mixed fully by magnetic force;
b. adding 5ml of Cetyl Trimethyl Ammonium Bromide (CTAB) solution, magnetically stirring for 2h, adjusting the pH value of the mixed solution to 6 by using NaOH solution to obtain iron lanthanum hydroxide mixed precipitate, and magnetically stirring for 24 h;
c. the solution was centrifuged, and the supernatant was removed and washed with deionized water.
d. Drying at 60 ℃ for 12h, taking out the material, cooling to room temperature, grinding in a ceramic grinding bowl to obtain granular hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material.
In the step a, LaCl3·nH2O and Fe (NO)3)3·7H2Selecting O with the mass ratio of 0.4:1 respectively, and weighing LaCl with corresponding mass3·nH2O and Fe (NO)3)3·7H2Dissolving O in 100ml deionized water by ultrasonic, and stirring for 5min on a magnetic stirrer at 25 ℃.
In the step b, the concentration of a Cetyl Trimethyl Ammonium Bromide (CTAB) solution is 0.1 mol/L.
In the step b, the concentration of the NaOH solution is 4mol/L, the stirring speed is increased, and the stirring is carried out for 24 hours.
In the step c, the filtrate is washed by deionized water until the filtrate does not contain chlorine (0.01 mol/L AgNO is used)3Solution detection) and nitrate (nitrate qualitative loop experimental detection).
The application of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material comprises the steps of adding the modified nano iron lanthanum material into a fluorine-containing solution, oscillating, centrifugally filtering, and carrying out solid-liquid separation to obtain the modified nano iron lanthanum material for adsorbing fluorine ions, wherein the fluoride in water is removed.
And (2) regenerating the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material, adding the modified nano iron lanthanum material adsorbing fluorine ions into a NaOH solution, oscillating for 120min, filtering and separating to obtain a fluorine ion-containing recovery solution, washing the separated material with deionized water, and drying to obtain the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material.
The following comparison of desorption experiments of the defluorinated hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material in NaOH solutions with different concentrations through specific experiments shows that:
taking 0.1g of hexadecylAdding trimethyl ammonium bromide modified nano iron lanthanum material into 100mL of fluorine solution with initial concentration of 10mg/L, oscillating at 200rpm for 120min, filtering and separating to obtain hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material adsorbing fluorine ions, and then respectively adding 100mL of 10-concentration nano iron lanthanum material-6、10-5、10-4、10-3、10-2、10-1And shaking the mol/L NaOH solution at 200rpm at room temperature for 120min to desorb the adsorbed fluorine, wherein the desorption result is shown in Table 1.
TABLE 1 Desorption results
Desorption conditions Fluorine desorption rate (%)
10-6mol/L NaOH 3.89
10-5mol/L NaOH 6.03
10-4mol/L NaOH 42.39
10-3mol/L NaOH 71.11
10-2mol/L NaOH 97.77
10-1mol/L NaOH 98.93
As can be seen from Table 1, the specific application 10-2The mol/L NaOH solution can not only ensure the fluorine desorption rate, but also save resources.
Regeneration experiment of hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material:
adding 100mL, 10 percent of hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material adsorbing fluorinion- 2And (2) shaking the solution of NaOH in mol/L at the room temperature of 200rpm for 120min, filtering and separating to obtain a recovered solution containing fluorine ions, washing the separated material with deionized water, and drying to obtain the desorbed hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material. And then adding the desorbed hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material into 100mL of fluorine solution with the initial concentration of 10mg/L, oscillating at room temperature at 200rpm for 120min, filtering and separating, and measuring the fluorine concentration in the solution by using a fluorine ion selective electrode, wherein the result is shown in Table 2.
TABLE 2 adsorption Rate
Number of cycles Adsorption rate
1 91.76％
2 90.13％
3 88.43％
4 85.69％
5 83.17％
6 81.89％
As can be seen from Table 2, the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material is subjected to centrifugal separation, is easy to separate solid from liquid, has the defluorination rate reduced by about 10 percent after being recycled for six times, has good regeneration performance, and can be repeatedly utilized.
As can be seen from fig. 1(a) to 1(c), in the preparation of the CTAB-LIN composite material by optimizing the synthesis conditions by the response surface method, the synthesis parameters are optimized by a three-variable three-level design method based on the research results of the single-factor synthesis experiment: la3+With Fe3+The concentration ratio of (3) was 0.4:1, the amount of CTAB was 5.5mL, and the synthesis pH was 6.
As can be seen from FIG. 1(a), with La3+With Fe3+The concentration ratio and the volume of CTAB are increased, and the adsorption amount of CTAB-LIN to fluorine is gradually increased. With La3+The defluorination tendency is obvious due to the increase of the concentration, which is caused by La3+Has affinity for fluoride ion greater than that of Fe3+. As can be seen from FIG. 1(b), with La3+With Fe3+The concentration ratio is increased and the pH value is reduced, and the removal rate of fluorine by CTAB-LIN is increased, which is mainly because of La3+F is easier to adsorb in acid environment-. At the same time, La3+The increase of the concentration is more beneficial to the adsorption of fluorine by the material. From FIG. 1(c), it can be seen that, when the volume of CTAB is constant, as the pH value is increased, the adsorption amount of CTAB-LIN to fluorine is increased; however, when the volume of CTAB is increased at a certain pH, there is no significant change in the defluorination of CTAB-LIN, probably because CTAB is positively charged on its surface and is more readily electrostatically adsorbed in an alkaline environment.
As can be seen from fig. 2, the defluorination effect of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material after six times of recycling is still good, and the surface hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material has good regeneration performance.

Claims (9)

1. The preparation method of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material is characterized by comprising the following steps of:
a. respectively weighing LaCl according to a certain mass ratio3·nH2O and Fe (NO)3)3·7H2O is put in deionized water and is stirred and mixed fully by magnetic force;
b. adding cetyl trimethyl ammonium bromide and the solution, magnetically stirring for 2h, adjusting the pH value of the mixed solution to 6 by using NaOH solution to obtain iron lanthanum hydroxide mixed precipitate, and magnetically stirring for 24 h;
c. centrifuging the solution obtained in the step b, removing supernatant, and washing with deionized water;
d. drying at 60 ℃ for 12h, taking out the material, cooling to room temperature, grinding in a ceramic grinding bowl to obtain granular hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material.
2. The method for preparing hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material according to claim 1, which is characterized in that: in the step a, LaCl3·nH2O and Fe (NO)3)3·7H2Selecting O with the mass ratio of 0.4: 1-0.5: 1, and weighing LaCl with corresponding mass3·nH2O and Fe (NO)3)3·7H2Dissolving O in deionized water by ultrasonic wave, and stirring for 5min on a magnetic stirrer at 25 deg.C.
3. The method for preparing hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material according to claim 1, which is characterized in that: in the step b, the concentration of the hexadecyl trimethyl ammonium bromide solution is 0.1 mol/L.
4. The method for preparing hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material according to claim 1, which is characterized in that: in the step b, the concentration of the NaOH solution is 4 mol/L.
5. The method for preparing hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material according to claim 1, which is characterized in that: and in the step c, washing with deionized water until the filtrate does not contain chlorine and nitrate.
6. The hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material is characterized in that: the method according to claims 1 to 5.
7. The application of the hexadecyl trimethyl ammonium bromide modified nanometer iron lanthanum material according to claim 6, wherein the application comprises the following steps: for removing fluoride from water.
8. The regeneration of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material is characterized in that: adding the modified nano iron lanthanum material adsorbing fluorine ions into an alkaline solution, oscillating for 120min, filtering and separating to obtain a recovery solution containing fluorine ions, cleaning the separated material with deionized water, and drying to obtain the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material.
9. The regeneration of the hexadecyl trimethyl ammonium bromide modified nano iron lanthanum material according to claim 8, wherein: the alkaline solution is 0.01mol/L NaOH aqueous solution.
CN202011304563.1A 2020-11-19 2020-11-19 Cetyl trimethyl ammonium bromide modified nano iron lanthanum material, preparation method and application Pending CN112427028A (en)

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