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

A layered bimetallic and transition metal technology, applied in the direction of metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problem of low density of catalytic active centers, small specific surface area, Difficult to recycle materials and other issues, to achieve the effect of improving catalytic activity and realizing recycling

Inactive Publication Date: 2012-12-12
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, vigorously stirred, and the pH value was adjusted to 10. The slurry was crystallized at 70 °C for 36 h, and after centrifugation, it was deCO2 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 ...

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PUM

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Abstract

The invention relates to a preparation method of a laminar double metal hydroxide of transition oxometallate and an application thereof. The preparation method comprises the following steps of: dissolving soluble divalent metal salt and trivalent metal salt into water to obtain a solution A; dissolving soluble alkali into the water to obtain a solution B; slowly dripping the solution A and the solution B into a reaction bottle to be mixed and agitated; filtering and drying a mixed solution, and milling to prepare a precursor; dissolving the prepared precursor into the water and agitating at a constant temperature to obtain a solution C; dissolving the transition oxometallate into the water to obtain a solution D; mixing the solution C and the solution D and agitating at the constant temperature; filtering the mixed solution and drying; and milling to obtain a target product LDH-POM (Lactic Dehydrogenase-Polyformaldehyde) to be used as an active catalyst of an organic matter nitrobenzene which is difficult to degrade in oxidized water. The preparation method disclosed by the invention combines structural characteristics and properties of the laminar double metal hydroxide and expresses a good catalytic performance of a metal oxide and oxometallate thereof; and the preparation method takes the laminar double metal hydroxide as a carrier and the transition oxometallate is introduced, so that more catalytic activity centers are provided, the catalytic effect is extremely improved and the laminar double metal hydroxide can be recycled and used.

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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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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