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Catalytic preparation method of veratraldehyde

A technology for the catalytic preparation of veratraldehyde, which is applied in the field of chemistry and chemical engineering, can solve the problems of limited industrial application, scarcity of precious metals and high price, and achieve the effect of high selective repeated use, good performance and high catalyst efficiency

Active Publication Date: 2019-06-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the scarcity and high price of precious metals limit its further industrial application

Method used

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  • Catalytic preparation method of veratraldehyde
  • Catalytic preparation method of veratraldehyde
  • Catalytic preparation method of veratraldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 13

[0023] Typical synthesis method A using catalyst Co / AC in Example 13: Dissolve metal cobalt hydrochloride in 2 g of water, add a certain amount of activated carbon carrier, and stir while adding until the solid just completely absorbs the metal salt solution. Continue to stir for 2 hours, dry it overnight and place it in an oven at 80°C for 12 hours, then heat it at a rate of 10°C / min in an inert atmosphere (nitrogen or argon), and keep it at 700°C for 2 hours to obtain a catalyst . Co catalysts supported by other supports such as silica, titania or alumina were prepared in the same way, labeled as Co / SiO 2 ,Co / TiO 2 ,Co / Al 2 o 3 .

Embodiment 2

[0024] Typical synthesis method B using the catalyst Co-BIm-600 in Example 2: Dissolve metal cobalt acetate in a certain amount of methanol solution, add a certain proportion of benzimidazole ligand, and stir at a certain temperature for 8 h to obtain a polymer. The solvent was removed by centrifugation, dried in an oven and placed in an inert atmosphere N 2 , heated at a heating rate of 10°C / min, kept at 600°C for 2h, and used directly as a catalyst. The rest of the acid-treated catalysts are then soaked in a certain concentration of acetic acid, hydrochloric acid or sulfuric acid to obtain catalysts. The synthesis conditions of the above catalyst are mild, the steps are simple, and the operation is easy.

[0025] The catalysts used in Examples 1-12, 15-16 are synthesized according to the steps of Example 2, and the specific changed substances and addition amounts are shown in Table 1.

[0026] Synthesis of different catalysts in Table 1 Method B

[0027]

[0028]

Embodiment 1

[0030] Co-BIm catalyst, 2mmol veratrol, 0.4mmol K 2 CO 3 and 4 ml of toluene were added to a stainless steel autoclave with a polytetrafluoroethylene liner inside, wherein Co: veratrol = 0.05: 1 (mol: mol). The temperature was raised to a reaction temperature of 100° C. using an automatic temperature controller, and 1.0 MPa of oxygen was introduced to react for 12 hours. During the reaction, the pressure was kept constant. The reaction products were analyzed by GC, and the reaction results are shown in Table 2.

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Abstract

The invention discloses a method for selectively synthesizing veratraldehyde from veratryl alcohol by a catalytic oxidation process. The method uses oxygen or air as an oxidant, and uses a stable andinexpensive metal catalyst to efficiently and highly selectively catalyze the oxidation of veratryl alcohol to synthesize the veratraldehyde. The conversion rate of veratryl alcohol is 99% or above, and the yield of the product veratraldehyde can reach 96%. The method has the advantages of simplicity in operation, mild conditions, and good recyclability of the catalyst.

Description

technical field [0001] The invention relates to the field of chemical engineering, in particular to a method for synthesizing veratraldehyde. Background technique [0002] Designing and developing a green and sustainable catalytic process for the efficient conversion of biomass resources to chemicals has important scientific and applied research value. Starting from renewable lignin, the preparation of aromatic ring compounds with high added value through catalytic conversion process is a hotspot of current research. Using veratrol as raw material to synthesize veratraldehyde by means of catalytic oxidation is a non-petroleum route with important research background and application prospects. Veratrol is a model compound of lignin, which can be obtained from lignin cracking reaction, and the oxidation product veratraldehyde can be widely used in the synthesis of food flavors, antibiotics, veratrazine and methyldopa and other pharmaceutical intermediates. Therefore, the con...

Claims

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Application Information

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IPC IPC(8): C07C45/37C07C47/575B01J23/75
CPCY02P20/584
Inventor 徐杰孙玉霞马红高进罗杨张树静刘鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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