CN113398883B - Preparation method and application of iron carbide/manganese crosslinked sodium alginate composite material - Google Patents
Preparation method and application of iron carbide/manganese crosslinked sodium alginate composite material Download PDFInfo
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Abstract
The invention discloses a preparation method and application of an iron carbide/manganese crosslinked sodium alginate composite material, wherein the preparation method comprises the following steps: s1, dropwise adding an iron (II) salt solution and/or a manganese (II) salt solution into a 2wt% sodium alginate aqueous solution, generating iron/manganese crosslinked sodium alginate through a crosslinking reaction, washing, collecting microspherical particles, and drying; and S2, sintering and carbonizing the dried sodium alginate in the step S1 at the temperature of 300-900 ℃ for 1-4h under protective gas, washing, drying, grinding and sieving to obtain the iron carbide/manganese crosslinked sodium alginate composite material. The iron carbide/manganese crosslinked sodium alginate composite material can simultaneously realize the reduction and removal of heavy metal toxicity, phosphorus retention and photocatalytic reduction adsorption of heavy metals.
Description
Technical Field
The invention relates to the field of environmental management, in particular to a preparation method and application of an iron carbide/manganese crosslinked sodium alginate composite material.
Background
With the advance of industrialization, heavy metal pollution in water environment and soil environment is increasingly serious, and the health and ecological development of human beings are seriously threatened. The rapid and efficient heavy metal adsorbent is researched and developed to adsorb heavy metal ions, so that the heavy metal ions are efficiently and rapidly adsorbed, the heavy metal ions in the water body are reduced to the national relevant water quality standard limit value (for example, as is 0.05 mg/L), and the method is very important for the sustainable development of the water environment and the soil environment.
The existing composite material for adsorption is not easy to realize the defects of complicated preparation process, low adsorption performance, high price and the like by effectively combining with heavy metal ions, so that the application of the composite material in the field of heavy metal adsorption is limited.
Disclosure of Invention
The invention mainly aims to provide a preparation method and application of an iron carbide/manganese crosslinked sodium alginate composite material.
The technical problem of the invention is solved by the following technical scheme:
a preparation method of an iron carbide/manganese crosslinked sodium alginate composite material comprises the following steps:
s1, dropwise adding an iron (II) salt solution and/or a manganese (II) salt solution into a 2wt% sodium alginate aqueous solution, generating iron/manganese crosslinked sodium alginate through a crosslinking reaction, washing, collecting microspherical particles, and drying;
s2, sintering and carbonizing the dried sodium alginate in the step S1 at the temperature of 300-900 ℃ for 1-4h under protective gas, cooling, washing, drying, grinding and sieving to obtain the iron/manganese carbide crosslinked sodium alginate composite material.
Preferably, the iron (II) salt solution is an iron (II) sulfate solution.
Preferably, the manganese (II) salt solution is at least one of a manganese sulfate solution and a manganese chloride solution, and preferably, the manganese (II) salt solution is a manganese sulfate solution.
Preferably, the step S2 is performed by sintering and carbonizing at 600 ℃ for 2h.
Preferably, said sieving in said step S2 means sieving with a 60 mesh sieve.
Preferably, when an iron (II) salt solution or a manganese (II) salt solution is dropwise added in the step S1, the volume ratio of the sodium alginate aqueous solution to the iron (II) salt solution or the manganese (II) salt solution is 1:1, the molar concentration of iron (II) ions in the iron (II) salt solution is 0.67mol/L, and the molar concentration of manganese (II) ions in the manganese (II) salt solution is 0.67mol/L; when a mixed solution of an iron (II) salt solution and a manganese (II) salt solution is dropwise added in the step S1, the volume ratio of the sodium alginate aqueous solution to the mixed solution is 1:2, the molar concentration of iron (II) ions in the mixed solution is 0.33mol/L, and the molar concentration of manganese (II) ions in the mixed solution is 0.33mol/L.
Preferably, the shielding gas is at least one of helium, neon, argon and nitrogen; the dripping in the step S1 is carried out by adopting a peristaltic pump with the rotating speed of 3 mL/min.
An iron carbide/manganese crosslinked sodium alginate composite material prepared by the preparation method.
The application of the iron carbide/manganese crosslinked sodium alginate composite material in treating heavy metal ions and/or phosphorus is provided.
Preferably, the heavy metal ions are at least one of As (III) ions, as (V) ions and Cr (VI) ions.
The beneficial effects of the invention include: according to the preparation method, the specific surface area of the composite material can be increased, the porosity of the composite material can be increased, the composite material can be effectively contacted with heavy metal ions and/or phosphorus, the heavy metal ions and the phosphorus can be quickly and efficiently adsorbed, the heavy metal ions can be synchronously oxidized or reduced, and the toxicity of the metal ions is reduced.
Drawings
Fig. 1 is an XRD pattern of the composite materials prepared in examples 1 and 2 of the present invention.
FIG. 2 is a FT-IR plot of composites prepared in examples 1 and 2 of the present invention.
FIG. 3 is an SEM image of composite materials prepared in examples 1 and 2 of the present invention.
FIG. 4 is a graph showing the As (III), as (V), and Cr (VI) adsorption kinetics of the composite material prepared in example 1 of the present invention.
FIG. 5 is a graph showing the kinetics of phosphorus retention of a composite material prepared in example 1 of the present invention.
FIG. 6 is a Barrett-Emmett-Teller analysis (Barrett-Emmett-Teller) chart of a composite material prepared in example 1 of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings and preferred embodiments. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The embodiment of the invention provides a preparation method of an iron carbide/manganese crosslinked sodium alginate composite material, which comprises the following steps:
s1, dropwise adding an iron (II) salt solution and/or a manganese (II) salt solution into a 2wt% sodium alginate aqueous solution, generating iron/manganese crosslinked sodium alginate through a crosslinking reaction, washing, collecting microspherical particles, and drying;
and S2, sintering and carbonizing the dried sodium alginate in the step S1 at the temperature of 300-900 ℃ for 1-4h under protective gas, cooling, washing, drying, grinding and sieving to obtain the iron carbide/manganese crosslinked sodium alginate composite material.
In the technical scheme, the iron/manganese crosslinked sodium alginate prepared in the step S1 is in the form of microspherical particles, and is not beneficial to effective combination with heavy metal ions and the like due to smooth surface, the iron/manganese crosslinked sodium alginate is subjected to sintering carbonization treatment in the step S2, so that the specific surface area of the composite material can be improved, the porosity of the composite material can be increased, the composite material can be effectively contacted with the heavy metal ions and/or phosphorus, the heavy metal ions and the phosphorus can be quickly and efficiently adsorbed, oxidation or reduction of the heavy metal ions (such As reduction of hexavalent chromium (Cr (VI)) and oxidation of trivalent arsenic (As (III)) can be synchronously realized, and the toxicity of the metal ions is reduced.
In a preferred embodiment, the iron (II) salt solution is an iron (II) sulfate solution.
In a preferred embodiment, the manganese (II) salt solution is at least one of a manganese sulfate solution and a manganese chloride solution, and preferably, the manganese (II) salt solution is a manganese sulfate solution.
In a preferred embodiment, the step S2 is sintering carbonization at 600 ℃ for 2h.
In a preferred embodiment, said sieving in said step S2 is 60 mesh sieving.
In a preferred embodiment, when an iron (II) salt solution or a manganese (II) salt solution is dropwise added in the step S1, the volume ratio of the sodium alginate aqueous solution to the iron (II) salt solution or the manganese (II) salt solution is 1:1, the molar concentration of iron (II) ions in the iron (II) salt solution is 0.67mol/L, and the molar concentration of manganese (II) ions in the manganese (II) salt solution is 0.67mol/L; when a mixed solution of an iron (II) salt solution and a manganese (II) salt solution is dropwise added in the step S1, the volume ratio of the sodium alginate aqueous solution to the mixed solution is 1:2, the molar concentration of iron (II) ions in the mixed solution is 0.33mol/L, and the molar concentration of manganese (II) ions in the mixed solution is 0.33mol/L.
In a preferred embodiment, the dropping of step S1 refers to dropping by using a peristaltic pump with a rotation speed of 3 mL/min.
In a preferred embodiment, the shielding gas is at least one of helium, neon, argon and nitrogen.
The embodiment of the invention also provides the iron carbide/manganese cross-linked sodium alginate composite material prepared by the preparation method.
The embodiment of the invention also provides application of the iron carbide/manganese crosslinked sodium alginate composite material in treatment of heavy metal ions and/or phosphorus.
In a preferred embodiment, the heavy metal ions are at least one of As (III) ions, as (V) ions and Cr (VI) ions.
The present invention is further illustrated by the following specific examples.
Example 1
3g of sodium alginate was dissolved in 150mL of distilled water at 60 deg.C (a drop of acetic acid solution may be added dropwise during the dissolution to aid in the dissolution of sodium alginate). Simultaneously preparing 100mmol 150mL MnSO 4 The solution is fully stirred for 2 hours, and the prepared sodium alginate solution with the concentration of 2 weight percent is dripped into MnSO through a peristaltic pump (the rotating speed is 3 mL/min) 4 Solutions ofIn (2), micro-spherical particles are rapidly formed. Washing the prepared microspherical particles with deionized water for three times, drying in an oven at 80 ℃, and collecting the microspherical particles.
Placing the obtained microspherical particles in a ceramic crucible, reacting for 2 hours at 600 ℃ in a vacuum muffle furnace with introduced nitrogen, cooling to room temperature, grinding the microspherical composite carbonized particles by using an agate mortar, ball-milling for 15 minutes at the rotating speed of 220rpm by using a ball mill, recovering the powder, and sieving by using a 60-mesh sieve to obtain the manganese carbide crosslinked sodium alginate composite material, wherein a sample is named as Mn/SA-C2 for storage.
Example 2
3g of sodium alginate was dissolved in 150mL of distilled water at 60 deg.C (a drop of acetic acid solution may be added dropwise during the dissolution process to aid in the dissolution of sodium alginate). Simultaneously preparing 100mmol 150mL MnCl 2 The solution is fully stirred for 2 hours, and the prepared sodium alginate solution with the concentration of 2 weight percent is dripped into MnCl through a peristaltic pump (the rotating speed is 3 mL/min) 2 In solution and rapidly form micro-spherical particles. Washing the prepared microspherical particles with deionized water for three times, drying in an oven at 80 ℃, and collecting the microspherical particles.
Placing the obtained microspherical particles in a ceramic crucible, reacting for 2 hours at 600 ℃ in a vacuum muffle furnace filled with nitrogen, cooling to room temperature, grinding the microspherical composite carbonized particles by using an agate mortar, performing ball milling for 15 minutes at the rotating speed of 220rpm by using a ball mill, recovering powder, and sieving by using a 60-mesh sieve to obtain a manganese carbide crosslinked sodium alginate composite material, wherein a sample is named as Mn/SA-C1 for storage.
Example 3
3g of sodium alginate is dissolved in 150mL of distilled water at 60 ℃ (one drop of acetic acid solution can be added dropwise during the dissolution process to assist the dissolution of sodium alginate). While preparing 100mmol 150mL FeSO 4 The solution is fully stirred for 2h, and the prepared sodium alginate solution with the concentration of 2wt% is dripped into the solution through a peristaltic pump (the rotating speed is 3 mL/min), and micro-spherical particles are rapidly formed. Washing the prepared microspherical particles with deionized water for three times, drying in an oven at 80 ℃, and collecting the microspherical particles.
Placing the obtained microspherical particles in a ceramic crucible, reacting for 2h at 600 ℃ in a vacuum muffle furnace with introduced nitrogen, cooling to room temperature, grinding the microspherical composite carbonized particles by using an agate mortar, ball-milling for 15min at the rotating speed of 220rpm by using a ball mill, recovering the powder, and sieving with a 60-mesh sieve to obtain the manganese carbide crosslinked sodium alginate composite material, wherein a sample is named as Fe/SA-C for storage.
Example 4
3g of sodium alginate was dissolved in 150mL of distilled water at 60 deg.C (a drop of acetic acid solution may be added dropwise during the dissolution process to aid in the dissolution of sodium alginate). Simultaneously 100mmol of MnSO is prepared 4 With 100mmol of FeSO 4 300mL of the mixed solution is fully stirred for 2h, and the prepared sodium alginate solution with the concentration of 2wt% is dripped into the solution through a peristaltic pump (the rotating speed is 3 mL/min) and micro-spherical particles are rapidly formed. Washing the prepared microspherical particles with deionized water for three times, drying in an oven at 80 ℃, and collecting the microspherical particles.
Placing the obtained microspherical particles in a ceramic crucible, reacting for 2 hours at 600 ℃ in a vacuum muffle furnace with introduced nitrogen, cooling to room temperature, grinding the microspherical composite carbonized particles by using an agate mortar, ball-milling for 15 minutes at the rotating speed of 220rpm by using a ball mill, recovering the powder, and sieving with a 60-mesh sieve to obtain the manganese iron carbide crosslinked sodium alginate composite material, wherein a sample is named as Mn @ Fe/SA-C for storage.
XRD characterization was performed on the composites prepared in examples 1 and 2, as shown in fig. 1. From the XRD pattern, it can be found that sodium alginate, before being crosslinked with Mn or Fe, generates sodium carbonate as the main material after carbonization, while Mn/SA-C1 composite material obtained after crosslinking, after carbonization, mainly comprises a carbon skeleton (in the embodiment of the present application, referred to as SA-C, the same applies hereinafter) and MnO attached to the carbon skeleton, and Mn/SA-C2 composite material obtained after crosslinking, after carbonization, mainly comprises the carbon skeleton and MnO and MnS attached to the carbon skeleton 2 . From the viewpoint of crystallinity, the Mn/SA-C1 composite material has better crystallinity than Mn/SA-C2, whereas the Mn/SA-C2 composite material generates MnO and MnS during carbonization 2 Can form sulfide precipitate with heavy metal, and has better effects of reducing hexavalent chromium, oxidizing trivalent arsenic and complexing phosphorus.
For examples 1 and2 FT-IR characterization was performed on the composite material prepared as shown in figure 2. From FT-IR spectrum, it can be found that the intensity of the light is from 400 to 1000cm -1 The absorption peak wavelength is Mn-O and-COONa stretching vibration, whereby it is sufficiently confirmed that MnO was generated by carbonization. At 1134cm -1 The stretching vibration of Mn-OH as the absorption wavelength in (B) can be inferred from the MnSO by carbonization in example 2 4 Crosslinking sodium alginate produces MnO and MnS 2 。
SEM powder characterization of the composites prepared in examples 1 and 2, as shown in FIG. 3, can be found by carbonizing MnCl 2 The cross-linked sodium alginate forms a good network lattice, and MnSO is carbonized 4 The crosslinked sodium alginate forms fine nano particles, provides a large specific surface area for the composite material, and provides attachment sites for heavy metal adsorption.
FIG. 4 is a graph showing the kinetics of adsorption of heavy metals As (III), as (V) and Cr (VI) by the composite material prepared in example 1. The reaction conditions are as follows: 30mL of a solution containing 15mg of the composite material and 10mg/L of heavy metal ions. Shows that: the Mn/SA-C2 composite material of example 1 can efficiently and rapidly adsorb As, and the adsorption kinetic curve shows that the As concentration can reach the surface water quality standard within 20min, but the adsorption time of Cr (VI) is obviously prolonged, which may be MnS 2 The content is lower.
FIG. 5 is a graph of the kinetics of phosphorus retention of the composite of example 1. The reaction conditions are as follows: 30mL of a solution containing 15mg of the composite material and 20mg/L of phosphorus. Shows that: the Mn/SA-C2 composite material has higher adsorption capacity to the phosphorus and can achieve the purpose of phosphorus retention.
FIG. 6 shows that the specific surface area and the porosity of the composite material can be obviously increased by crosslinking sodium alginate through manganese carbide element through BET analysis of the composite material, and the specific surface area of the Mn/SA-C2 composite material is 77.02m 2 A specific surface area of 3.67m for SA-C alone 2 And/g, deducing that the cross-linking carbonization forms porous microspheres, obviously enhancing the specific surface area of the composite material, further fully exposing the metal oxide in the composite material, providing a carbon skeleton carrier for the metal oxide, and realizing the high-efficiency adsorption of heavy metal and phosphorus.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several equivalent substitutions or obvious modifications can be made without departing from the spirit of the invention, and all the properties or uses are considered to be within the scope of the invention.
Claims (4)
1. The application of the manganese carbide crosslinked sodium alginate composite material in treating at least one of As (III) ions and As (V) ions is characterized in that the preparation method of the manganese carbide crosslinked sodium alginate composite material comprises the following steps:
s1, dropwise adding 2wt% sodium alginate aqueous solution into a manganese (II) salt solution, generating manganese cross-linked sodium alginate through a cross-linking reaction, washing, collecting microspherical particles, and drying, wherein the manganese (II) salt solution is a manganese sulfate solution;
s2, sintering and carbonizing the dried manganese crosslinked sodium alginate in the step S1 at 600 ℃ for 2h under protective gas, cooling, washing, drying, grinding and sieving to obtain the manganese carbide crosslinked sodium alginate composite material, wherein the manganese carbide crosslinked sodium alginate composite material mainly comprises a carbon skeleton, mnO and MnS attached to the carbon skeleton 2 Capable of forming sulfide precipitates with As (III) ions or As (V) ions.
2. The use of claim 1, wherein: the sieving in the step S2 is to pass through a 60-mesh sieve.
3. The use of claim 1, wherein:
the volume ratio of the sodium alginate aqueous solution to the manganese (II) salt solution is 1:1, and the molar concentration of manganese (II) ions in the manganese (II) salt solution is 0.67 mol/L.
4. The use of claim 1, wherein: the protective gas is at least one of helium, neon, argon and nitrogen; the dripping in the step S1 is carried out by adopting a peristaltic pump with the rotating speed of 3 mL/min.
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| KR20160136572A (en) * | 2015-05-20 | 2016-11-30 | 한국화학연구원 | Double crosslinked sodium alginate/polyvinyl alcohol composite nanofiltration membrane and preparation method thereof |
| CN108554385B (en) * | 2018-01-17 | 2021-02-19 | 湖南农业大学 | Preparation method of magnetic ferric alginate mesoporous carbon microspheres capable of adsorbing heavy metal elements |
| CN111146424B (en) * | 2019-12-30 | 2023-06-06 | 上海交通大学 | Metal sulfide/carbon composite material, and preparation method and application thereof |
| CN112221477A (en) * | 2020-09-28 | 2021-01-15 | 湖北富邦科技股份有限公司 | Polyacrylamide modified Fe-Mn-S/sodium alginate composite microsphere and preparation method thereof |
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