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Loaded composite metal catalyst used for unsaturated alcohol oxidation and preparation method thereof

A composite metal and catalyst technology, applied in the direction of metal/metal oxide/metal hydroxide catalyst, carbon-based compound preparation, organic compound preparation, etc., can solve the problems that the catalyst is difficult to repeat, the reactor operation is expensive, and the cost of the catalyst is high. , achieving good stability, improving reaction performance and structural stability, and simple preparation method

Active Publication Date: 2014-05-07
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] DE-B 2715209 and EP-B 55354 describe the process of oxidative dehydrogenation of 3-methyl-3-butenol in the presence of oxygen using silver or copper crystals as a catalyst. The disadvantage of this process is that the cost of the catalyst is very high, It can only be obtained if the silver catalyst particle size distribution is relatively uniform or has a certain partic

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Weigh 1.45 g AgNO 3 Dissolved in 5 ml of water, 0.76g (NH 4 ) 2 C 2 o 4 Dissolved in 8 ml of water, the two solutions were placed in a water bath at 40 °C under stirring conditions to react. Wash the precipitate after reacting for 1 hour, add 2 ml of ethylenediamine solution with a molar concentration of 10 mol / L to the silver oxalate precipitate produced after washing for 2-3 times to obtain a silver-amine complex solution, add the resulting silver-amine Add 0.015 g Cs to the complex solution 2 CO 3 , 0.60g Cu(NO 3 ) 2 ·3H 2 O, 0.35 mg Sc (NO 3 ) 3 ·3H 2 O, 0.020 g Sr(CH3COO) 2 , 0.010 g ZrO 2 Sol, 0.020 g CeO 2 The sol dissolves into a homogeneous solution. 5 g of α-Al 2 o 3 The carrier was added to the above solution, stirred for about 1 hour, dried at 100°C to remove the solvent, and calcined at 260°C for half an hour to obtain 6.1 g of Catalyst A. Among them, silver accounts for 15 wt%, copper accounts for 2.6 wt%, scandium accounts for 0.009 wt%,...

Embodiment 2

[0071] Weigh 3.47 g AgNO 3 Dissolved in 5 ml of water, 2.17 g (NH 4 ) 2 C 2 o 4 Dissolve in 10 ml of water, and place the two solutions in a 40°C water bath with stirring to react. Wash the precipitate after reacting for 1 hour, and add 2 ml of ethylenediamine with a concentration of 15 mol / L to the silver oxalate precipitate after washing for 2-3 times to obtain a silver-amine complex solution. Add 0.015 g Cs to 2 CO 3 , 0.14 g Cu(NO 3 ) 2 ·3H 2 O, 0.43 g Sc 2 (SO 4 ) 3· ·8H 2 O, 0.020 g Sr(CH 3 COO) 2 , 1.8 mg ZrO 2 Sol, 1.8 mg CeO 2 The sol dissolves into a homogeneous solution. 5 g of α-Al 2 o 3 The carrier was added to the above solution, stirred for about 1 hour, dried and evaporated at 100°C to remove the solvent, and calcined at 300°C for half an hour to obtain 7.4g of catalyst B, in which silver accounted for 30wt%, copper accounted for 0.5wt%, scandium accounted for 1wt%, oxidized Ceria zirconia sol accounted for 0.05wt%.

[0072] Reaction perfor...

Embodiment 3

[0075] Weigh 0.16 g AgNO 3 Dissolved in 5 ml of water, 0.08 g (NH 4 ) 2 C 2 o 4 Dissolve in 5 ml of water, and place the two solutions in a water bath at 40°C with stirring. Wash the precipitate after reacting for 1 hour, and add 2 ml of glycerine triamine with a concentration of 0.5 mol / L to the silver oxalate precipitate after washing for 2-3 times to obtain a silver-amine complex solution. Add 0.03 g Cs to the mixture 2 CO 3 , 1.65 g CuSO 4 ·5H 2 O, 0.24 g Sc(NO 3 ) 3 ·3H 2 O, 0.040 g Sr(CH3COO) 2 , 0.5 g ZrO 2 Sol, 0.5 g CeO 2 The sol dissolves into a homogeneous solution. 10 g of α-Al 2 o 3 The carrier was added to the above solution, stirred for about 1 hour, dried at 100°C to remove the solvent, and calcined at 400°C for half an hour to obtain catalyst C. Finally, 10.5 g of catalyst C was obtained, in which silver accounted for 1 wt%, copper accounted for 4 wt%, scandium accounted for 0.4 wt%, and cerium oxide zirconia sol accounted for 1 wt%.

[0076]...

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Abstract

The invention discloses a load composite metal catalyst used for unsaturated alcohol oxidation and a preparation method thereof. The catalyst comprises: 0.001-0.3wt% of an alkali metal, 0.001-1wt% of an alkaline earth metal, 0.001-1wt% of scandium, 0.05-1wt% of cerium oxide and zirconia sol, 0.3-10wt% of copper, 1-30wt% of silver, and 60-95wt% of a carrier. The preparation method includes: using a precipitant to precipitate a silver salt solution, making the obtained silver precipitate into a silver-amine solution by an amine compound, employing an amine complexing solution of a soluble copper salt, a scandium salt, an alkali metal salt, an alkaline earth metal salt and additives to spray or dip the catalyst carrier, and then carrying out drying and roasting to obtain the loaded silver-copper composite catalyst. The catalyst provided by the invention has the characteristics of high reactivity, good stability and fewer three wastes, etc., thus being suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a supported composite metal catalyst for oxidation of unsaturated alcohols and a preparation method thereof. Background technique [0002] Oxidation reactions are an important process in organic synthesis and play an important role in the functionalization of reaction intermediates for pharmaceutical, fine chemical and agricultural chemical products. Whether it is laboratory preparation or industrial production, the oxidation process of alcohols into carbonyl compounds plays an important role in various types of oxidation transformations. In terms of chemical properties and various uses, carbonyl compounds occupy a special important position, and they are often the starting materials for synthesis. This is why aldehydes and ketones have become important raw materials and intermediates in chemical processes, especially fine chemical processes. Therefore, the oxidation of alcohols to corresponding carbonyl compounds is one of th...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J27/224C07C45/38C07C47/21
Inventor 郑素娟刘英俊崔乐超石玉赵文娟李乐乐黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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