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Preparation method of vanillin

A technology of vanillin and elements, applied in the field of preparation of vanillin, to achieve the effects of good stability, accelerated oxygen transfer process, and less side reactions

Pending Publication Date: 2022-04-08
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing copper-based oxidants cannot meet this requirement due to the formation of soluble copper salts under strong alkalinity
In addition, since oxygen will also directly participate in the reaction, a certain amount of by-products will be generated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Catalyst preparation method is as follows:

[0035] Ultrasonicate 10g of graphite oxide in water for 1h, add a certain amount of manganese source, tungsten source and lanthanum source into the water. Among them, the manganese source is manganese acetate, the tungsten source is tungstic acid, and the lanthanum source is lanthanum nitrate hexahydrate. The total mass of manganese source, tungsten source and lanthanum source is 10wt% of graphite oxide mass. Molar ratio of three metal elements: manganese element: tungsten element: lanthanum element = 3:2:6. Ammonia water was added to the above solution to pH = 11, and the resulting precipitate was filtered and washed with ultrapure water until neutral. The washed precipitate was dried at -15°C and 18Pa(a) for 30h. Finally, the sample was calcined in air atmosphere at 250°C for 8h to obtain the catalyst.

[0036] The catalytic oxidation reaction conditions are as follows:

[0037] The sodium salt of 3-methoxy 4-hydroxyma...

Embodiment 2

[0040] Catalyst preparation method is as follows:

[0041] Ultrasonicate 10g of graphite oxide in water for 1h, add a certain amount of manganese source, tungsten source and lanthanum source into the water. Among them, the manganese source is manganese nitrate, the tungsten source is ammonium tungstate, and the lanthanum source is lanthanum chloride. The total mass of manganese source, tungsten source and lanthanum source is 15wt% of graphite oxide mass. The molar ratio of the three metal elements is manganese: tungsten: lanthanum = 5:4:8. Ammonia water was added to the above solution to pH=12, and the resulting precipitate was filtered and washed with ultrapure water until neutral. The washed precipitate was dried at -5°C and 8 Pa(a) for 10 h. Finally, the sample was calcined at 300°C in air atmosphere for 12h to obtain the catalyst.

[0042] The catalytic oxidation reaction conditions are as follows:

[0043] The mass fraction of 3-methoxy 4-hydroxymandelic acid sodium ...

Embodiment 3

[0045] Catalyst preparation method is as follows:

[0046]Ultrasonicate 10g of graphite oxide in water for 2h, add a certain amount of manganese source, tungsten source and lanthanum source into the water. Among them, the manganese source is manganese nitrate, the tungsten source is sodium tungstate dihydrate, and the lanthanum source is lanthanum chloride. The total mass of manganese source, tungsten source and lanthanum source is 18wt% of graphite oxide mass. The molar ratio of the three metal elements is: manganese: tungsten: lanthanum = 6:3:5. Ammonia water was added to the above solution to pH=9, and the resulting precipitate was filtered and washed with ultrapure water until neutral. The washed precipitate was dried at 0° C. and 2 Pa(a) for 30 h. Finally, the sample was calcined at 350°C in air atmosphere for 7h to obtain the catalyst.

[0047] The catalytic oxidation reaction conditions are as follows:

[0048] The mass fraction of 3-methoxy 4-hydroxymandelic acid ...

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Abstract

The invention provides a method for preparing vanillin, which comprises the following steps: carrying out catalytic oxidation reaction on 3-methoxy-4-hydroxymandelic acid sodium salt in an aerobic environment, and then carrying out decarboxylation reaction to obtain vanillin, and the catalyst of the catalytic oxidation reaction is graphite oxide loaded Mn-W-La as a catalyst. According to the method, the catalyst is high in reaction activity and good in stability, long-time operation can be achieved, and the problem that an oxidizing agent needs to be filtered and regenerated in a traditional intermittent process is solved.

Description

technical field [0001] The invention relates to the field of preparation of vanillin, in particular to a preparation method of vanillin. Background technique [0002] Vanillin (English name vanillin), also known as 3-methoxy-4-hydroxybenzaldehyde, is one of the important synthetic fragrances in the world and is widely used in the fields of food, beverage and daily cosmetics. The synthesis of vanillin is chemical synthesis, which can be divided into safrole method, guaiacol-formaldehyde method and guaiacol-glyoxylic acid method. Among them, the safrole method has a long production process, complex process, many by-products, low yield, and limited use; the guaiacol-formaldehyde method also faces the problems of too long process and low yield, and there is no industrial application case . [0003] At present, the mainstream method in the world is the guaiacol-glyoxylic acid method, and vanillin is prepared by condensation, oxidation and decarboxylation of glyoxylic acid and g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/39C07C47/58B01J23/34
CPCY02P20/584
Inventor 范立耸王漭王锐丁大康刘振峰李俊平郑京涛边新建刘释水冯民昌初晓东马德森曹鹤曹文健温道宏杨栋琳
Owner WANHUA CHEM GRP CO LTD
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