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Ruthenium-iron bimetallic catalyst and preparation method and application thereof

A bimetallic catalyst and reaction technology, used in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve problems such as high operating conditions, quality impact, equipment corrosion, etc. , to achieve the effect of improving conversion rate and selectivity, optimizing selective adsorption, and solving corrosion problems

Active Publication Date: 2021-10-26
SUZHOU SINOCOMPOUND TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] (1) The catalyst needs to be reduced by hydrogen, which requires a high temperature and high pressure environment, and the operation risk is high, and the active metals are prone to agglomeration at high temperature; (2) The catalyst needs to be aged in oxygen after hydrogen reduction, and the metal will inevitably become dull. The corresponding oxides are generated by hydrogenation, which affects the activity and selectivity of the catalyst, and due to the high risk of negative hydrogen ruthenium carbon, oxygen aging operation is inevitable; (3) considerable amount of trimethylamine, etc. are required in the hydrogenation process Organic amines, whose special odor will affect the quality of nerol and geraniol products, and due to their strong volatility and flammability, require high operating conditions
In addition, most of the above methods use ruthenium chloride, ferric chloride, ferrous chloride, etc. as precursors, and chlorides are easy to cause corrosion of equipment.

Method used

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  • Ruthenium-iron bimetallic catalyst and preparation method and application thereof
  • Ruthenium-iron bimetallic catalyst and preparation method and application thereof
  • Ruthenium-iron bimetallic catalyst and preparation method and application thereof

Examples

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preparation example Construction

[0044] The invention provides a kind of preparation method of ruthenium-iron bimetallic catalyst, comprises the steps:

[0045] Mixing ruthenium carbonyl, activated carbon and the first solvent, performing the first thermal decomposition reaction to prepare ruthenium carbonyl carbon;

[0046] Mixing the carbonyl ruthenium carbon, carbonyl iron and a second solvent, and performing a second thermal decomposition reaction to prepare the ruthenium-iron bimetallic catalyst.

[0047] In some examples, the ruthenium carbonyl is selected from at least one of ruthenium pentacarbonyl and triruthenium dodecacarbonyl. Further, ruthenium carbonyl is triruthenium dodecacarbonyl.

[0048] In some examples, the iron carbonyl is selected from at least one of iron pentacarbonyl and triiron dodecacarbonyl. Further, the iron carbonyl is triiron dodecacarbonyl.

[0049] In some examples, in the ruthenium-iron bimetallic catalyst, the mass percentage of ruthenium is 4%-6%, and the mass percentag...

Embodiment 1

[0064] Add 15mL of acetone and 0.1g of ruthenium dodecacarbonyltriruthenium (0.33mmol) into a 50mL three-necked flask, dissolve and add 1.8g of dry activated carbon, stir at 40°C under argon for 1h, then remove under reduced pressure and collect the acetone , to obtain black powder carbonyl ruthenium carbon.

[0065] In another 50mL three-necked flask, add 15g octadecylamine (0.056mol), triiron dodecacarbonyl (0.60mmol) methanol solution containing 0.1g iron (mass concentration 95%) and the aforementioned ruthenium carbonyl carbon, under argon Stir at 60°C for 1 hour to remove methanol, then raise the temperature to 130°C and keep it for 1 hour, and finally raise the temperature to 220°C and keep it for 0.5 hours. C Catalyst 1. Its XPS spectrum is as figure 1 shown.

Embodiment 2

[0067] Add 15 mL of acetone and 0.1 g of ruthenium dodecacarbonyl triruthenium (0.33 mmol) into a 50 mL three-neck flask, dissolve and add 1.88 g of dry activated carbon, stir at 40°C under argon for 1 h, then remove under reduced pressure and collect the acetone , to obtain black powder carbonyl ruthenium carbon.

[0068] In another 50mL three-necked flask, add 15g of octadecylamine (0.056mol), 0.02g of iron-containing triiron dodecacarbonyl (0.12mmol) methanol solution (mass concentration 95%) and the aforementioned ruthenium carbonyl carbon, under argon Stir at 60°C for 1 hour to remove methanol, then raise the temperature to 130°C and keep it for 1 hour, and finally raise the temperature to 220°C and keep it for 0.5 hours. C Catalyst 2.

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Abstract

The invention relates to a ruthenium-iron bimetallic catalyst and a preparation method and application thereof. The preparation method of the ruthenium-iron bimetallic catalyst comprises the following steps: mixing ruthenium carbonyl, activated carbon and a first solvent, and carrying out a first thermal decomposition reaction to prepare ruthenium carbonyl carbon; and mixing the carbonyl ruthenium carbon, carbonyl iron and a second solvent, and carrying out a second thermal decomposition reaction to prepare the ruthenium-iron bimetallic catalyst. According to the preparation method, the problems of hydrogen reduction risk in traditional production, agglomeration of active metal at high temperature, passivation of the catalyst by subsequent aging operation and the like are effectively avoided, raw materials with special smell do not need to be adopted, and meanwhile, the catalytic performance of the prepared catalyst is ensured.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a ruthenium-iron bimetallic catalyst and its preparation method and application. Background technique [0002] Nerol (cis-3,7-dimethyl-2,6-octadienol) and geraniol (trans-3,7-dimethyl-2,6-octadienol) are interchangeable The cis-trans isomer is a typical chain monoterpene compound with a pleasant rose aroma. It is widely used in various food flavors and daily chemical flavor formulations, and is also a key intermediate for the synthesis of other important fragrances. At present, nerol and geraniol are mainly obtained from natural plant extraction and industrial synthesis. The raw materials extracted from natural plants are planting products, which are easily affected by factors such as weather, pests, and planting areas. The purchase price and quantity of raw materials fluctuate greatly, and large-scale production is limited and cyclical. Therefore, industrial synthesis is the ...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J37/08C07C29/141C07C33/02
CPCB01J23/8906B01J37/086C07C29/141C07C33/02
Inventor 钱棋春张佳琪马家豪
Owner SUZHOU SINOCOMPOUND TECH
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