Polyacid complex, nanocomposite material containing same, and application of nanocomposite material in dye adsorption

Abstract

The invention relates to a polyacid complex. The chemical formula of the polyacid complex is [Ni(HL)2]2H2[P2Mo5O23].2H2O, wherein HL is 2-acetylpyrazine thiosemicarbazone. The polyacid complex belongsto the monoclinic crystal system, and has a C2 / c space group, and cell parameters are as follows: a = 3.0575(7) nm, b = 1.3276(3) nm, c = 1.7009(4) nm, alpha = 90 DEG, beta = 113.837 (5) DEG, and gamma = 90 DEG. The invention also provides a nanocomposite material containing the polyacid complex. The polyacid complex POMs with a good adsorption function is combined with magnetic Fe3O4 nanoparticles to form the magnetic nanocomposite material. The combination of the POMs and Fe3O4 nanoparticles makes the material have an increased adsorption efficiency and well achieve recycling under the action of an external magnetic field.

Description

technical field

[0001] The invention belongs to the technical field of functionalized polyacids, in particular to a polyacid complex, a nanocomposite material containing it (that is, a polyacid complex of a POMs compound with good adsorption function, and a magnetic Fe complex) 3 o 4 Nanoparticles combine to form magnetic nanocomposite materials), synthetic methods, and applications in the selective adsorption of cationic dyes. The nanocomposite material combines polyacid complexes POMs with Fe 3 o 4 The combination of nanoparticles not only improves the adsorption efficiency, but also can achieve good recycling under the action of an external magnetic field. Background technique

[0002] With the continuous development of human society, the discharge of numerous industrial dye wastewaters poses a serious threat to the water environment and human health. At present, there are mainly two strategies for dye treatment, one is photocatalytic degradation, which is mainly unde...

Examples

Embodiment 1

[0031] A preparation method of a nanocomposite material containing polyacid complexes, specifically comprising the steps of:

[0032] 1) Preparation of Fe 3 o 4 Nanoparticles can be synthesized with reference to literature methods (Liu HongLing., Wu JunHua., MinJi Hyun, Zhang XiaoYan, Kim Young Keun. Tunable synthesis and multifunctionalities of Fe 3 o 4 -ZnO hybrid core-shell nanocrystals. Mater. Res. Bull. 2013, 48 , 551–558).

[0033] 2) Preparation of polyacid complexes:

[0034] 2-Acetylpyrazine thiosemicarbazone (0.097 g, 0.5 mmol), Ni(ClO 4 ) 2 ·6H 2 O (0.091 g, 0.25 mmol) was added to a small beaker containing a mixed solution of 15 mL distilled water and 10 mL methanol, stirred at 60°C for 30 min to fully dissolve it, then the solution was cooled to room temperature, and molybdic acid was added Sodium solution (0.24 g, by 1 mmolNa 2 MoO 24 4H 2 O dissolved in 10 mL of water), followed by concentrated H 3 PO 4 Adjust the pH value of the solution so tha...

Embodiment 2

[0041] 2 mg, 4 mg, 6 mg, 8 mg, 10 mg, 12 mg and 14 mg of magnetic adsorbent Fe 3 o 4 The @multi-acid complex was added to 10 mL and 15 mg / L methylene blue solutions respectively, and reacted at room temperature for 3 h. The result is as image 3 As shown in a, when 12 mg of magnetic adsorbent is used, the adsorption efficiency of methylene blue is the highest, which can reach 97.84%. Therefore, for this adsorption process, 12 mg / 10 mL was considered to be the optimal dosage / volume ratio, and this ratio was also used as the implementation of the next investigation.

Embodiment 3

[0043] 12 mg of magnetic adsorbent Fe 3 o 4 Add the polyacid complex to 10 mL methylene blue solution containing 5 mg / L, 10 mg / L, 15 mg / L, 20 mg / L, 25 mg / L and 30 mg / L, and react at room temperature for 3 h . The result is as image 3 As shown in b, as the concentration of methylene blue increases, the adsorption rates of the magnetic adsorbent to methylene blue are 95.02%, 97.53%, 97.84%, 97.76%, 95.81% and 94.70% ( image 3 b). Therefore, 15 mg / L is the optimum adsorption concentration for this process.

technical field

[0001] The invention belongs to the technical field of functionalized polyacids, in particular to a polyacid complex, a nanocomposite material containing it (that is, a polyacid complex of a POMs compound with good adsorption function, and a magnetic Fe complex) 3 o 4 Nanoparticles combine to form magnetic nanocomposite materials), synthetic methods, and applications in the selective adsorption of cationic dyes. The nanocomposite material combines polyacid complexes POMs with Fe 3 o 4 The combination of nanoparticles not only improves the adsorption efficiency, but also can achieve good recycling under the action of an external magnetic field. Background technique

[0002] With the continuous development of human society, the discharge of numerous industrial dye wastewaters poses a serious threat to the water environment and human health. At present, there are mainly two strategies for dye treatment, one is photocatalytic degradation, which is mainly unde...

Examples

Embodiment 1

[0031] A preparation method of a nanocomposite material containing polyacid complexes, specifically comprising the steps of:

[0032] 1) Preparation of Fe 3 o 4 Nanoparticles can be synthesized with reference to literature methods (Liu HongLing., Wu JunHua., MinJi Hyun, Zhang XiaoYan, Kim Young Keun. Tunable synthesis and multifunctionalities of Fe 3 o 4 -ZnO hybrid core-shell nanocrystals. Mater. Res. Bull. 2013, 48 , 551–558).

[0033] 2) Preparation of polyacid complexes:

[0034] 2-Acetylpyrazine thiosemicarbazone (0.097 g, 0.5 mmol), Ni(ClO 4 ) 2 ·6H 2 O (0.091 g, 0.25 mmol) was added to a small beaker containing a mixed solution of 15 mL distilled water and 10 mL methanol, stirred at 60°C for 30 min to fully dissolve it, then the solution was cooled to room temperature, and molybdic acid was added Sodium solution (0.24 g, by 1 mmolNa 2 MoO 24 4H 2 O dissolved in 10 mL of water), followed by concentrated H 3 PO 4 Adjust the pH value of the solution so tha...

Embodiment 2

[0041] 2 mg, 4 mg, 6 mg, 8 mg, 10 mg, 12 mg and 14 mg of magnetic adsorbent Fe 3 o 4 The @multi-acid complex was added to 10 mL and 15 mg / L methylene blue solutions respectively, and reacted at room temperature for 3 h. The result is as image 3 As shown in a, when 12 mg of magnetic adsorbent is used, the adsorption efficiency of methylene blue is the highest, which can reach 97.84%. Therefore, for this adsorption process, 12 mg / 10 mL was considered to be the optimal dosage / volume ratio, and this ratio was also used as the implementation of the next investigation.

Embodiment 3

[0043] 12 mg of magnetic adsorbent Fe 3 o 4 Add the polyacid complex to 10 mL methylene blue solution containing 5 mg / L, 10 mg / L, 15 mg / L, 20 mg / L, 25 mg / L and 30 mg / L, and react at room temperature for 3 h . The result is as image 3 As shown in b, as the concentration of methylene blue increases, the adsorption rates of the magnetic adsorbent to methylene blue are 95.02%, 97.53%, 97.84%, 97.76%, 95.81% and 94.70% ( image 3 b). Therefore, 15 mg / L is the optimum adsorption concentration for this process.

Images