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Preparation method of laminar double metal hydroxide of transition oxometallate and application

A hydroxide and transition metal technology, applied in the field of layered double metal hydroxide (LDHs) material preparation, can solve the problems of low density of catalytic active centers, small specific surface area, and inability to further improve catalytic performance, and achieve the realization of cycle Utilize and improve the effect of catalytic activity

Inactive Publication Date: 2014-09-17
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the small specific surface area of ​​the material itself, the density of catalytic active centers is small, the catalytic performance cannot be further improved, and the material is difficult to achieve recycling.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Preparation of MgAl-W LDHs

[0025] Mg(NO 3 ) 2 · 6H 2 O(61.44 g, 0.24 mol), Al(NO 3 ) 2 · 9H 2 O (45.00 g, 0.12 mol) was mixed and dissolved in 200 ml to remove CO 2 of deionized water; take another NaNO 3 (68.00 g, 0.80 mol) and NaOH (60.20 g, 1.50 mol) were dissolved in 500 ml deCO 2 of deionized water. in N 2 Under protection, the two solutions were slowly dropped into a 1 L four-necked flask at the same time, stirred vigorously, and the pH value was adjusted to 10, and the slurry was crystallized at 70 °C for 36 h. 2 Wash with deionized water until neutral, dry (40 ℃), and grind to obtain the precursor MA-NO 3 LDHs.

[0026] MgAl-NO 3 (3 g) dissolved in 75 ml deCO 2 of deionized water, placed in a 500 ml four-necked bottle, N 2 Stir at 70 °C for 1 h under protection; take another Na 2 WO 4 2H 2 O (2.5 g) dissolved in 125 ml deCO 2 In deionized water, add the precursor solution; the mixture is in N 2 Stir at 70 °C for 3 h under pro...

Embodiment 2

[0027] Example 2: Preparation of ZnAl-W LDHs

[0028] Zn(NO 3 ) 2 · 6H 2 O(118.8 g, 0.40 mol), Al(NO 3 ) 2 · 9H 2 O (75.00 g, 0.20 mol) was mixed and dissolved in 250 ml for deCO 2 of deionized water; take another NaNO 3 (68.00 g, 0.80 mol) and NaOH (60.20 g, 1.50 mol) were dissolved in 500 ml deCO 2 of deionized water. in N 2 Under protection, the two solutions were slowly dropped into a 1 L four-neck flask at the same time, vigorously stirred, and the pH value was adjusted to 8.5. The slurry was crystallized at 70 °C for 24 h, and after centrifugation, it was deCO2 2Wash with deionized water until neutral, dry (40 ℃), and grind to obtain the precursor ZA-NO 3 LDHs.

[0029] ZnAl-NO 3 (3 g) dissolved in 75 ml deCO 2 of deionized water, placed in a 500 ml four-necked bottle, N 2 Stir at 70 °C for 1 h under protection; take another Na 2 WO 4 2H 2 O (1.65 g) dissolved in 125 ml deCO 2 In deionized water, add the precursor solution; the mixture is in N 2 S...

Embodiment 3

[0030] Example 3: Preparation of MgAl-V LDHs

[0031] Mg(NO 3 ) 2 · 6H 2 O(61.44 g, 0.24 mol), Al(NO 3 ) 2 · 9H 2 O (45.00 g, 0.12 mol) was mixed and dissolved in 200 ml to remove CO 2 of deionized water; take another NaNO 3 (68.00 g, 0.80 mol) and NaOH (60.20 g, 1.50 mol) were dissolved in 500 ml deCO 2 of deionized water. in N 2 Under protection, the two solutions were slowly dropped into a 1 L four-necked flask at the same time, stirred vigorously, and the pH value was adjusted to 10, and the slurry was crystallized at 70 °C for 36 h. 2 Wash with deionized water until neutral, dry (40 ℃), and grind to obtain the precursor MA-NO 3 LDHs.

[0032] MgAl-NO 3 (3 g) dissolved in 75 ml deCO 2 of deionized water, placed in a 500 ml four-necked bottle, N 2 Stir at 55 °C for 1 h under protection; take another Na 2 VO 4 2H 2 O (1.83 g) dissolved in 125 ml deCO 2 In deionized water, add the precursor solution; the mixture is in N 2 Stir at 55 °C for 1 h under pr...

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Abstract

The invention relates to a preparation method and application of a transition metal oxo acid salt intercalated layered double hydroxide. The preparation steps are: dissolving soluble divalent metal salt and trivalent metal salt in water to obtain solution A; dissolving soluble alkali Dissolve in water to obtain alkaline solution B; slowly drop the two solutions of A and B into the reaction flask at the same time, mix and stir, filter the mixed solution, dry, and grind to obtain the precursor; dissolve the prepared precursor In water, stir at constant temperature to obtain solution C; dissolve transition metal oxo acid salt in water to obtain solution D; mix solutions C and D, stir at constant temperature, filter the mixed solution, dry, and grind to obtain the target product LDH-POM, It can be used as an active catalyst for oxidizing refractory organic matter nitrobenzene in water. The present invention combines the structural features and properties of layered double metal hydroxides, and the good catalytic properties exhibited by metal oxides and their oxo acid salts, and uses layered double metal hydroxides as carriers to introduce transition metal oxoacids Salt, thus providing more catalytic active centers, greatly improving the catalytic effect, and can be recycled.

Description

technical field [0001] The invention belongs to the technical field of layered double hydroxide (LDHs) material preparation, and specifically relates to a preparation method of a transition metal oxo-acid intercalated layered double hydroxide and its use as a refractory organic compound in oxidized water treatment Application of nitrobenzene active catalyst. Background technique [0002] Layered double hydroxides (LDHs for short) are an important class of inorganic functional materials, and their general structural formula is , where M 2+ and M 3+ They are divalent and trivalent metal cations respectively, located on the main laminate; A n- is an interlayer anion; X is M 3+ / (M 2+ +M 3+ ) molar ratio; m is the molar mass of interlayer water molecules. The common divalent metal ions that make up LDHs are Mg 2+ , Zn 2+ 、Ni 2+ 、Co 2+ 、Cu 2+ , Mn 2+ etc.; common trivalent metal ions are Al 3+ 、Cr 3+ , Fe 3+ 、Se 3+ , V 3+ Etc., the combination of divalent and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/30B01J23/22B01J23/28B01J37/30C02F1/72C02F101/38
Inventor 隋铭皓陈勇段标标盛力
Owner TONGJI UNIV
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