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Preparation method of La2CuO4 with three-dimensional macroporous structure and La1.6Sr0.4CuO4

A la1.6sr0.4cuo4, three-dimensional macroporous technology, applied in chemical instruments and methods, copper compounds, inorganic chemistry, etc., can solve the problems that the colloidal crystal template method is difficult to obtain, the template agent is easy to collapse, etc., and the particle size of the product can be reached And the effect of controllable pore size and cheap raw materials

Active Publication Date: 2016-01-27
SHANGHAI NAT ENG RES CENT FORNANOTECH
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Problems solved by technology

The colloidal crystal template method is the main method for preparing three-dimensional macroporous structure (like) perovskite oxides, such as Dai et al. 2 CuO 4 formalecombustion.CatalysisToday, 2011,175(1):209~215.] La 2 CuO 4 Perovskite, but its pore size is small, only 53-64nm
At the same time, the literature only reported the hole-like La 2 CuO 4 The synthesis of the three-dimensional macroporous La 1.6 Sr 0.4 CuO 4 Perovskite-like
Due to the high temperature for forming perovskite-like under normal conditions, it generally needs to be at 800 o Above C, for La with perfect crystal phase structure 1.6 Sr 0.4 CuO 4 More so, at high temperature, templates are often prone to collapse, making it difficult to obtain perovskite-like La with uniform pore structure by colloidal crystal template method. 2 CuO 4 and La 1.6 Sr 0.4 CuO 4
If a three-dimensional macroporous perovskite-like La 2 CuO 4 and La 1.6 Sr 0.4 CuO 4 , it is necessary to choose a suitable precursor preparation method and select a specific roasting method, and the simultaneous satisfaction of the two conditions is a great technical challenge for the current research.

Method used

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  • Preparation method of La2CuO4 with three-dimensional macroporous structure and La1.6Sr0.4CuO4
  • Preparation method of La2CuO4 with three-dimensional macroporous structure and La1.6Sr0.4CuO4
  • Preparation method of La2CuO4 with three-dimensional macroporous structure and La1.6Sr0.4CuO4

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Experimental program
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Effect test

Embodiment 1

[0028] 3.15g lanthanum nitrate (La(NO 3 ) 3 ×6H 2 O), 0.9g copper nitrate (Cu(NO 3 ) 2 ×3H 2 O) and 2.0 g of citric acid were added to a beaker containing 25 mL of methanol, stirred for 1 h, the mixture was transferred to a beaker containing 2.0 g of PMMA and soaked for 5 h, vacuum filtered, dried at room temperature for 15 h, and placed in a tube furnace medium roasting. The roasting process is divided into two steps: (1) at N 2 In air flow (20mL / min), rise from room temperature to 700°C at a rate of 1°C / min and keep at this temperature for 4 hours, then cool to 50°C in the same atmosphere; (2) switch to air flow (20mL / min), raised from 50°C to 300°C at the same rate and kept at this temperature for 3h, continued to raise the temperature to 800°C and kept at this temperature for 5h. The three-dimensional ordered macropore La 2 CuO 4 Catalyst, the pore size is 130~150nm.

Embodiment 2

[0030] 2.52gLa(NO 3 ) 3 ×6H 2 O, 0.31gSr(NO 3 ) 2 , 0.9gCu(NO 3 ) 2 ×3H 2 O and 2.0 g of citric acid were added to a beaker containing 38 mL of methanol, and after stirring for 2 hours, the mixture was transferred to a beaker containing 2.0 g of PMMA and soaked for 12 hours, vacuum filtered, dried at room temperature for 12 hours, and then placed in a tube furnace Roasting. The roasting process is divided into two steps: (1) at N 2 In air flow (20mL / min), rise from room temperature to 700°C at a rate of 1°C / min and keep at this temperature for 4 hours, then cool to 50°C in the same atmosphere; (2) switch to air flow (20mL / min), raised from 50°C to 300°C at the same rate and kept at this temperature for 3h, continued to raise the temperature to 800°C and kept at this temperature for 5h. Three-dimensional worm-like macropore La 1.6 Sr 0.4 CuO 4 catalyst.

Embodiment 3

[0032] 3.15gLa(NO 3 ) 3 ×6H 2 O, 0.9gCu(NO 3 ) 2 ×3H 2 O and 2.0g citric acid were added to a beaker containing a mixture of 8mL methanol and 17mL ethylene glycol, and after stirring for 2h, solution A was obtained; 0.75gL-lysine was dissolved in 7.5mL deionized water to obtain L- Aqueous solution of lysine B. Mix solution A and solution B to form a precursor solution. The former body solution was transferred to a beaker containing 2.0g PMMA and soaked for 12 hours, vacuum filtered, dried at room temperature for 12 hours, and then placed in a tube furnace for roasting. The roasting process is divided into two steps: (1) at N 2 In air flow (20mL / min), rise from room temperature to 900°C at a rate of 1°C / min and keep at this temperature for 2 hours, then cool to 50°C in the same atmosphere; (2) switch to air flow (20mL / min), raised from 50°C to 700°C at the same rate and kept at this temperature for 4h. Three-dimensional worm-like macropore La 2 CuO 4 .

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Abstract

The invention discloses a preparation method of La2CuO4 with a three-dimensional macroporous structure and La1.6Sr0.4CuO4 and belongs to the field of material preparation. The preparation method is characterized in that PMMA (polymethyl methacrylate) is taken as a template, citric acid is taken as a complexing agent, methanol or a mixed solution of methanol and glycol is taken as a solvent, La2CuO4 with a three-dimensionally ordered macroporous structure or the three-dimensional macroporous structure and La1.6Sr0.4CuO4 oxides are prepared by changing a calcination condition under the condition that lysine is introduced or not introduced. The mole ratio of metal salt to citric acid is (1:1)-(1:2), and the mass ratio of total metal salt to PMMA is (1.5-2.5):1. The preparation method has the advantages that raw materials are low in price, the size and the pore diameter of product particles are controllable and the like.

Description

technical field [0001] The invention relates to a three-dimensional macroporous structure La 2 CuO 4 and La 1.6 Sr 0.4 CuO 4 The preparation method of , specifically relates to a three-dimensional ordered structure La 2 CuO 4 and La 1.6 Sr 0.4 CuO 4 and three-dimensional worm-like macropore La 2 CuO 4 and La 1.6 Sr 0.4 CuO 4 method of preparation. Background technique [0002] Perovskite-like composite oxides (A 2 BO 4 ) is a layered perovskite composed of perovskite structural units (ABO 3 ) with other types of structural primitives (such as AO, B 2 o 3 ) is a kind of superstructure composite oxide formed by combination. Due to the alternate combination of two different structures, in addition to some important properties similar to perovskite, it also has unique characteristics, such as high catalytic performance and superconductivity. In the studied system, La is more studied at the A site, and affected by the formation conditions and structural stabil...

Claims

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Application Information

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IPC IPC(8): C01G3/00
Inventor 何丹农袁静金彩虹
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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