Preparation of nano-palladium catalyst as well as application of nano-palladium catalyst to synthesis of vanillin compounds

A catalyst and nano-palladium technology, applied in the preparation of organic compounds, carbon-based compounds, physical/chemical process catalysts, etc., can solve the problems of long process routes, low reaction efficiency, and many by-products, achieving good selectivity, Environmentally friendly, easy-to-separate effect

Inactive Publication Date: 2015-05-13
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the nitrosation method of guaiacol is mainly used in China to produce vanillin. This method has a long process route, many supporting equipment, serious discharge of three wastes, low reaction efficiency, and many by-products obtained, which brings great

Method used

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  • Preparation of nano-palladium catalyst as well as application of nano-palladium catalyst to synthesis of vanillin compounds
  • Preparation of nano-palladium catalyst as well as application of nano-palladium catalyst to synthesis of vanillin compounds
  • Preparation of nano-palladium catalyst as well as application of nano-palladium catalyst to synthesis of vanillin compounds

Examples

Experimental program
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Effect test

preparation example Construction

[0026] One, the preparation of nano palladium catalyst

[0027] Under an argon atmosphere, add 1 g of nano-sized magnesium oxide support and 0.5 mmol of palladium salt into 50 ml of deionized water to form an impregnating solution, and then fully stir at 5°C for 12 hours to obtain a brown magnesium oxide-supported palladium salt catalyst. Filter and dry in vacuo; then weigh 1g of the above catalyst and add 1.5g of sodium borohydride to 30ml of dry ethanol solution in a hydrogen atmosphere, and stir thoroughly at 5°C for 5h to obtain a black zero-valent palladium catalyst supported on magnesium oxide , the solid was filtered and washed three times with deionized water and acetone, and dried in vacuum to obtain the final catalyst.

[0028] 2. Synthesis of vanillin compounds

[0029] Take the synthesis of vanillin as an example:

Embodiment 1

[0031] Add vanillin (1.54g, 10mmol), nano-palladium catalyst (0.7g, 10%), potassium carbonate (1.66g, 12mmol) and 30ml of toluene into a 50ml three-necked flask, and react at 80°C for 3h under magnetic stirring. After the reaction, cool the reaction solution, filter and recover the catalyst, add an equal volume of deionized water, separate the organic phase, extract the water phase with ethyl acetate three times, each time for 5min, combine the organic phase, spin dry under reduced pressure, and use column chromatography The desired product was isolated 1.4 g in 90% yield.

Embodiment 2

[0033] Add vanillin (1.54g, 10mmol), nano-palladium catalyst (0.4g, 6%), potassium carbonate (1.66g, 12mmol) and 30ml of toluene into a 50ml three-necked flask, and react at 80°C for 3h under magnetic stirring. After the reaction, cool the reaction solution, filter and recover the catalyst, add an equal volume of deionized water, separate the organic phase, extract the water phase with ethyl acetate three times, each time for 5min, combine the organic phase, spin dry under reduced pressure, and use column chromatography The desired product was isolated 1.43g in 93% yield.

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Abstract

The invention discloses preparation of a nano-palladium catalyst as well as an application of the nano-palladium catalyst to synthesis of vanillin compounds and relates to the technical field of organic synthesis. The active ingredient of the nano-palladium catalyst is zero-valence-state single-substance palladium nanoparticles which are obtained by loading high-valence-state palladium salt on a carrier and then reducing the palladium salt to the active ingredient; then vanillyl alcohol compounds are oxidized into the vanillin compounds by the aid of air under actions of the nano-palladium catalyst and an alkali under normal temperature and normal pressure conditions. The prepared nano-palladium catalyst has the characteristics of good selectivity and high yield, is easy to separate after participating in reactions, recyclable and environment-friendly and has a certain industrial application value.

Description

Technical field: [0001] The invention relates to the technical field of organic synthesis, in particular to the preparation of a nano palladium catalyst and its application in the synthesis of vanillin compounds. Background technique: [0002] Vanillin has a charming aroma of vanilla, and its molecular formula is C 8 h 8 o 3 , the system named 3-methoxy-4-hydroxybenzaldehyde. As a spice, vanillin is used in a huge amount, occupying the first place in the spice market in the world today, and it is also one of the most important synthetic spices, known as the "king of spices". [0003] Vanillin has a very wide range of uses: it is used as flavoring material, flavoring and fixative in food markets such as soft drinks, ice cream, cheese, condiments, desserts, dishes, snacks and roasted seeds and nuts; it is used in the fields of wine making and cigarettes Used as a fragrance and fragrance enhancer; used as a fragrance and fragrance agent in common cosmetics and skin care pro...

Claims

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Application Information

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IPC IPC(8): B01J23/44C07C45/38C07C47/575
Inventor 华文亮徐基平王天义汪洋
Owner ANHUI HYEA AROMAS
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