Method for preparing trisacetylacetonate iridium through solid phase synthesis

Abstract

The invention discloses a method for preparing trisacetylacetonate iridium through solid phase synthesis. The method comprises: grinding acetylacetone and sodium carbonate according to a certain ratio, adding a certain amount of iridium trichloride hydrate and a reducing agent for grinding to obtain solid powder, and performing heating, secondary grinding, cooling, washing and drying. The yield can reach 55-60%. The method is mild in condition, friendly to the environment, easy to operate, and high in yield. The adverse effect of a solvent on a functional complex in a reaction operation process is prevented, and the method is suitable for massive production of trisacetylacetonate iridium.

Description

technical field

[0001] The invention relates to a method for preparing iridium triacetylacetonate by a solid-phase synthesis method, which belongs to the field of catalysis. Background technique

[0002] Iridium belongs to the platinum group metal elements, and its resources are very scarce and expensive. The noble metal iridium film has excellent oxidation resistance, high electrical conductivity, excellent catalytic activity, and good stability. These properties make the noble metal iridium film widely used in many fields such as electrode materials, microelectronics, solid-state fuel cells and gas sensors, and is known as the "vitamin" of modern industry. Noble metal iridium films are generally prepared by metal-organic chemical vapor deposition. In the whole preparation process, the selection of a suitable metal-organic source is a key factor affecting the preparation. In the past, metal halides were often used for deposition, but the gasification and decomposition temp...

Examples

Embodiment 1

[0016] Take 8.2mL of acetylacetone and 3.2g of sodium carbonate and grind them in a mortar, then add 3.5g of iridium trichloride hydrate and 2mmol of ascorbic acid and grind to form a paste until it is ground into a solid powder, heat it in a microwave at 800W for 10min, take out Then continue grinding, after cooling to room temperature, wash with distilled water, filter with suction, wash with methanol, and vacuum dry to obtain 2.72 g of iridium triacetylacetonate.

[0017] Productive rate=actual yield of iridium triacetylacetonate / theoretical yield of iridium triacetylacetonate=2.72g / 4.86g=55.9%.

[0018] Carry out result analysis to it, characteristic structure parameter: 1, 1 H-NMR (500MHz, DMSO): δ (ppm) = 5.43 (s, 2H, CH), 1.97 (s, 12H, CH 3 ); 2. MS: measured value m / z=490.87, theoretical value m / z=490.54; 3. Elemental analysis: measured value C 36.47%, H 4.27%, theoretical value C 36.76%, H 4.29%.

Embodiment 2

[0020] Take 12.4mL of acetylacetone and 6.8g of sodium bicarbonate and grind them in a mortar, then add 3.5g of iridium trichloride hydrate and 2mmol of ascorbic acid and grind to form a paste until it is ground into a solid powder, and heat it in a microwave oven at 950W for 9min. After taking it out, continue to grind, cool to room temperature, wash with distilled water, filter with suction, wash with methanol, and vacuum dry to obtain 2.89 g of iridium triacetylacetonate.

[0021] Productive rate=actual yield of iridium triacetylacetonate / theoretical yield of iridium triacetylacetonate=2.89g / 4.86g=59.5%.

[0022] Analyze the results, characteristic structure parameters: 1s, 1 H-NMR (500MHz, DMSO): δ (ppm) = 5.46 (s, 2H, CH), 1.95 (s, 12H, CH 3 ); 2. MS: measured value m / z=490.90, theoretical value m / z=490.54; 3. Elemental analysis: measured value C 36.68%, H 4.30%, theoretical value C 36.76%, H 4.29%.

Embodiment 3

[0024] Take 9.0mL of acetylacetone and 2.6g of sodium carbonate and grind them in a mortar, then add 3.5g of iridium trichloride hydrate and 1mmol of hydrazine hydrate and grind to form a paste until it is ground into a solid powder, and heat it in a microwave oven at 1100W for 9min. After taking it out, continue to grind, cool to room temperature, wash with distilled water, filter with suction, wash with methanol, and vacuum dry to obtain 2.86 g of iridium triacetylacetonate.

[0025] Productive rate=actual yield of iridium triacetylacetonate / theoretical yield of iridium triacetylacetonate=2.86g / 4.86g=58.8%.

[0026] Carry out result analysis to it, characteristic structure parameter: 1, 1 H-NMR (500MHz, DMSO): δ (ppm) = 5.45 (s, 2H, CH), 1.95 (s, 6H, CH 3 ); 2. MS: measured value m / z=490.75, theoretical value m / z=490.54; 3. Elemental analysis: measured value C 36.66%, H 4.30%, theoretical value C 36.76%, H 4.29%.

technical field

[0001] The invention relates to a method for preparing iridium triacetylacetonate by a solid-phase synthesis method, which belongs to the field of catalysis. Background technique

[0002] Iridium belongs to the platinum group metal elements, and its resources are very scarce and expensive. The noble metal iridium film has excellent oxidation resistance, high electrical conductivity, excellent catalytic activity, and good stability. These properties make the noble metal iridium film widely used in many fields such as electrode materials, microelectronics, solid-state fuel cells and gas sensors, and is known as the "vitamin" of modern industry. Noble metal iridium films are generally prepared by metal-organic chemical vapor deposition. In the whole preparation process, the selection of a suitable metal-organic source is a key factor affecting the preparation. In the past, metal halides were often used for deposition, but the gasification and decomposition temp...

Examples

Embodiment 1

[0016] Take 8.2mL of acetylacetone and 3.2g of sodium carbonate and grind them in a mortar, then add 3.5g of iridium trichloride hydrate and 2mmol of ascorbic acid and grind to form a paste until it is ground into a solid powder, heat it in a microwave at 800W for 10min, take out Then continue grinding, after cooling to room temperature, wash with distilled water, filter with suction, wash with methanol, and vacuum dry to obtain 2.72 g of iridium triacetylacetonate.

[0017] Productive rate=actual yield of iridium triacetylacetonate / theoretical yield of iridium triacetylacetonate=2.72g / 4.86g=55.9%.

[0018] Carry out result analysis to it, characteristic structure parameter: 1, 1 H-NMR (500MHz, DMSO): δ (ppm) = 5.43 (s, 2H, CH), 1.97 (s, 12H, CH 3 ); 2. MS: measured value m / z=490.87, theoretical value m / z=490.54; 3. Elemental analysis: measured value C 36.47%, H 4.27%, theoretical value C 36.76%, H 4.29%.

Embodiment 2

[0020] Take 12.4mL of acetylacetone and 6.8g of sodium bicarbonate and grind them in a mortar, then add 3.5g of iridium trichloride hydrate and 2mmol of ascorbic acid and grind to form a paste until it is ground into a solid powder, and heat it in a microwave oven at 950W for 9min. After taking it out, continue to grind, cool to room temperature, wash with distilled water, filter with suction, wash with methanol, and vacuum dry to obtain 2.89 g of iridium triacetylacetonate.

[0021] Productive rate=actual yield of iridium triacetylacetonate / theoretical yield of iridium triacetylacetonate=2.89g / 4.86g=59.5%.

[0022] Analyze the results, characteristic structure parameters: 1s, 1 H-NMR (500MHz, DMSO): δ (ppm) = 5.46 (s, 2H, CH), 1.95 (s, 12H, CH 3 ); 2. MS: measured value m / z=490.90, theoretical value m / z=490.54; 3. Elemental analysis: measured value C 36.68%, H 4.30%, theoretical value C 36.76%, H 4.29%.

Embodiment 3

[0024] Take 9.0mL of acetylacetone and 2.6g of sodium carbonate and grind them in a mortar, then add 3.5g of iridium trichloride hydrate and 1mmol of hydrazine hydrate and grind to form a paste until it is ground into a solid powder, and heat it in a microwave oven at 1100W for 9min. After taking it out, continue to grind, cool to room temperature, wash with distilled water, filter with suction, wash with methanol, and vacuum dry to obtain 2.86 g of iridium triacetylacetonate.

[0025] Productive rate=actual yield of iridium triacetylacetonate / theoretical yield of iridium triacetylacetonate=2.86g / 4.86g=58.8%.

[0026] Carry out result analysis to it, characteristic structure parameter: 1, 1 H-NMR (500MHz, DMSO): δ (ppm) = 5.45 (s, 2H, CH), 1.95 (s, 6H, CH 3 ); 2. MS: measured value m / z=490.75, theoretical value m / z=490.54; 3. Elemental analysis: measured value C 36.66%, H 4.30%, theoretical value C 36.76%, H 4.29%.

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