Catalyst for preparing alkene unsaturated aldehyde from alkene unsaturated alcohol and preparation method and application of catalyst

A catalyst and unsaturated technology, applied in chemical instruments and methods, physical/chemical process catalysts, carbon-based compound preparation, etc., can solve problems such as low selectivity, process safety, and poor reactivity, and achieve simple preparation methods and raw materials Cheap and easy to get, active and stable effect

Active Publication Date: 2018-03-20
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Copper catalysts have poor activity and low selectivity to the oxidation of unsaturated alcohols, and cannot meet the requirements of industrialization; although silver catalysts have good activity to the oxidation of unsaturated alcohols and have high yield and selectivity, they cannot be used under high temperature conditions. Under the environment, the silver nan

Method used

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  • Catalyst for preparing alkene unsaturated aldehyde from alkene unsaturated alcohol and preparation method and application of catalyst
  • Catalyst for preparing alkene unsaturated aldehyde from alkene unsaturated alcohol and preparation method and application of catalyst
  • Catalyst for preparing alkene unsaturated aldehyde from alkene unsaturated alcohol and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0047] Example 1:

[0048] Preparation of catalyst A: Add 5.25g of TiO to 43.24g of 25wt% ammonia water under stirring conditions 2 Make it into a suspension, and add 3.99 g of Ir to this suspension 5 (PO 4 ) 6 (OH) 2 , React at 60℃ for 5h, stand at room temperature for 11h, centrifuge the obtained precipitate, lyophilize and roast at 400℃ for 5h as carrier; dissolve 0.17g AgNO3 in 0.2mL water, 0.20g (NH4)2C2O4 was dissolved in 0.32mL of water, and the two solutions were placed in a water bath at 40°C under stirring conditions for reaction. After reacting for 1h, the precipitate was washed. After washing 2-3 times, 0.34 mL of 5mol / L ethylenediamine aqueous solution was added to the precipitate to prepare a silver-amine complex solution, and 3.08 was added to the obtained silver-amine complex solution gCu(NO 3 ) 2 , 0.002gRe(NO 3 ) 3 , 0.38gMo(NO 3 ) 4 Dissolve into a uniform solution, add the prepared carrier to the above solution, stir for about 1 hour, distill off the solvent a...

Example Embodiment

[0051] Example 2:

[0052] Preparation of catalyst B: Except for using 3.06g AgNO 3 , 2.16g Cu(NO 3 ) 2 , 0.01g Re(NO 3 ) 3 , 0.30gMo(NO 3 ) 4 , 3.68g TiO 2 , 4.06g Ir 5 (PO 4 ) 6 (OH) 2 , 3.57g (NH4)2C2O4, 6.12ml of ethylenediamine aqueous solution with a concentration of 5mol / L, 30.26g of ammonia with a concentration of 25wt%, the rest refer to Example 1. In the obtained catalyst B, silver accounted for 18.50wt%, copper accounted for 7wt%, rhenium accounted for 0.05wt%, molybdenum accounted for 0.80wt%, TiO 2 Accounted for 35%, Ir5(PO 4 ) 6 (OH) 2 Accounted for 38.65wt%.

[0053] Catalyst B reaction activity test: Refer to the method of Example 1 for testing, the reaction conversion rate is 72%, and the selectivity of 3-methyl-2-butene-1-al is 97%.

[0054] Catalyst B service life test: According to the method of Example 1, the reaction activity did not decrease within 4000 hours, the conversion rate was maintained at 69-72%, and the selectivity was maintained at 97-98%. After 4200...

Example Embodiment

[0055] Example 3:

[0056] Preparation of catalyst C: except for using 4.13g AgNO 3 , 0.15g Cu(NO 3 ) 2 , 0.09g Re(NO 3 ) 3 , 0.16gMo(NO 3 ) 4 , 4.20g TiO 2 , 3.53g Ir 5 (PO 4 ) 6 (OH) 2 , 4.82g (NH4)2C2O4, 8.27ml of ethylenediamine aqueous solution with a concentration of 5mol / L, 34.59g of ammonia with a concentration of 25wt%, the rest refer to Example 1. In the obtained catalyst C, silver accounted for 25wt%, copper accounted for 0.5wt%, rhenium accounted for 0.43wt%, molybdenum accounted for 0.43wt%, TiO 2 Accounted for 40%, Ir 5 (PO 4 ) 6 (OH) 2 Accounted for 33.65wt%.

[0057] Catalyst C reaction activity test: the test was conducted with reference to the method of Example 1, the reaction conversion rate was 75%, and the selectivity of 3-methyl-2-butene-1-al was 99%.

[0058] Catalyst C service life test: According to the method of Example 1, the reaction activity did not decrease within 4000 hours, the conversion rate was maintained at 73-75%, and the selectivity was maintaine...

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Abstract

The invention discloses a catalyst for preparing alkene unsaturated aldehyde from alkene unsaturated alcohol and a preparation method and application of the catalyst. The catalyst comprises the following components: 1-30wt% of silver, 0.1-10wt% of copper, 0.01-1wt% of rhenium, 0.01-1wt% of molybdenum, 30-50wt% of TiO2 and 20-40wt% of Ir5(PO4)6(OH)2. The catalyst is particularly applicable to preparation of 3-methyl-2-butene-1-aldehyde from 3-methyl-2-butene-1-alcohol through oxidation. The catalyst disclosed by the invention has the characteristics of being high in action activity, good in high temperature resistant sintering property, good in stability, and the like, and is applicable to large-scale industrial production.

Description

technical field [0001] The invention relates to a catalyst for preparing ethylenically unsaturated aldehydes from ethylenically unsaturated alcohols, especially a catalyst for preparing 3-methyl-2-butene-1-aldehyde by oxidation of 3-methyl-2-butene-1 alcohol and its preparation method. Background technique [0002] 3-Methyl-2-butene-1-al, also known as isopentenal, is the raw material for the synthesis of isophytic alcohol; it can also be used as the starting material for the synthesis of citral, and then for the production of vitamin A, vitamin E, β- Carotene; it can also be used to synthesize spices such as damascenone and ironone. [0003] In the patent JPS60246340, it is reported that 3-methyl-2-buten-1-ol is oxidized by oxygen to obtain 3-methyl-2- Butene-1-al, the target product selectivity can reach 96%. This reaction needs to be carried out under relatively high temperature conditions, and the catalyst is easily sintered during the continuous operation of the reac...

Claims

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Application Information

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IPC IPC(8): B01J27/19C07C45/38C07C47/21
CPCB01J27/19C07C45/38C07C47/21
Inventor 张旭张涛吕英东郭劲资程晓波王延斌朱龙龙黎源华卫琦
Owner WANHUA CHEM GRP
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