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Preparation method of vanillin-1,2-propylene glycol acetal

A technology of ethyl vanillin and propylene glycol acetal, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problems of unsuitable for industrial production, high catalyst preparation cost, Unfriendly to the environment and other issues, to achieve the effects of easy control, high product yield, and simple preparation process

Active Publication Date: 2015-02-25
SHENZHEN BOTON FLAVORS & FRAGRANCES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, domestic Chen Jiexiao, Luo Jinyue and others use SO 4 2- / ZrO 2 Type solid superacid catalyzes and synthesizes the product, but the catalyst used in this method is expensive to prepare, and the strong acidity corrodes the equipment heavily, is not friendly to the environment, and is not suitable for industrial production

Method used

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  • Preparation method of vanillin-1,2-propylene glycol acetal
  • Preparation method of vanillin-1,2-propylene glycol acetal
  • Preparation method of vanillin-1,2-propylene glycol acetal

Examples

Experimental program
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Effect test

Embodiment 1

[0034] a. Add 5.0 g of phosphoric acid and 45.0 g of acetic anhydride into a three-necked flask equipped with a thermometer, a stirrer, and a reflux condenser, heat to and keep at 35° C. and stir for 24 hours to obtain 50.0 g of composite catalyst.

[0035] b. Add 1.0kg (6.0mol) ethyl vanillin, 0.92kg (12.0mol) 1,2-propylene glycol, and 50.0g composite catalyst in a three-necked flask equipped with a thermometer, agitator, oil-water separator and reflux condenser And 2.0kg toluene, stir and be heated to reflux dehydration, dehydration time 20 hours. After the reaction was completed, the system was lowered to room temperature. The reaction solution was washed with saturated brine, and then a small amount of Na with a mass concentration of 20% was added to the system. 2 CO 3 solution, and adjust the system to pH=8-9. Then distill off toluene and unreacted 1,2-propanediol under normal pressure, then distill under reduced pressure, collect the 150~152℃ / 0.2kPa fraction, which is...

Embodiment 2

[0043] a. Add 3.0 g of phosphoric acid and 27.0 g of acetic anhydride into a three-neck flask equipped with a thermometer, a stirrer, and a reflux condenser, heat to and keep at 35° C. and stir for 24 hours to obtain 30.0 g of composite catalyst.

[0044] b. Add 1.0kg (6.0mol) ethyl vanillin, 0.92kg (12.0mol) 1,2-propylene glycol, and 30.0g composite catalyst in a three-necked flask equipped with a thermometer, agitator, oil-water separator and reflux condenser And 2.0kg toluene, stir and be heated to reflux dehydration, dehydration time 20 hours. After the reaction was completed, the system was lowered to room temperature. The reaction solution was washed with saturated brine, and then a small amount of Na with a mass concentration of 20% was added to the reaction solution. 2 CO 3 solution, and adjust the system to pH=8-9. Then, toluene and unreacted 1,2-propanediol were distilled off under normal pressure, and then distilled under reduced pressure to obtain 0.84 kg of pro...

Embodiment 3

[0046] a. Add 25.0 g of phosphoric acid and 25.0 g of acetic anhydride into a three-neck flask equipped with a thermometer, a stirrer, and a reflux condenser, heat to and keep at 35° C. and stir for 24 hours to obtain 50.0 g of composite catalyst.

[0047] b. Add 1.0kg (6.0mol) ethyl vanillin, 0.92kg (12.0mol) 1,2-propylene glycol, and 50.0g composite catalyst in a three-necked flask equipped with a thermometer, agitator, oil-water separator and reflux condenser And 2.0kg toluene, stir and be heated to reflux dehydration, dehydration time 20 hours. After the reaction was completed, the system was lowered to room temperature. The reaction solution was washed with saturated brine, and then a small amount of Na with a mass concentration of 20% was added to the reaction solution. 2 CO 3 solution, and adjust the system to pH=8-9. Then, the toluene and unreacted 1,2-propanediol were distilled off under normal pressure, and then distilled under reduced pressure to obtain 0.68 kg o...

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Abstract

The invention relates to the technical field of perfumes, and discloses a preparation method of vanillin-1,2-propylene glycol acetal. The preparation method comprises the following steps: dissolving ethyl vanillin and 1, 2-propylene glycol in an organic solvent, and carrying out a condensation reaction under the action of a composite catalyst to prepare vanillin-1,2-propylene glycol acetal; and the composite catalyst is an acetic anhydride and phosphoric acid mixture. The method is an improved traditional synthesis method, and uses cheap phosphoric acid and acetic anhydride to prepare the composite catalyst, so the preparation method disclosed in the invention has the advantages of simple reaction method, easy control of the reaction process, high reaction yield reaching 98%, and suitableness for industrialized production.

Description

technical field [0001] The invention relates to the technical field of perfumes, in particular to a preparation method of ethyl vanillin 1,2-propanediol acetal. Background technique [0002] The development of the flavor and fragrance industry depends on the continuous discovery of new high-quality fragrance raw materials. Ethyl vanillin 1,2-propanediol acetal has sweet and rich vanillin fragrance, long-lasting fragrance, and can be used as a fixative. In 1998, the American Flavor and Extract Manufacturers Association (FEMA) announced the FEMA number of ethyl vanillin propylene glycol acetal as 3838, and suggested that the dosage in food should be 0.08-429mk / kg. The research on ethyl vanillin 1,2-propanediol acetal has been reported abroad, for example: Beresnevich’s research used benzene as a solvent and sulfonated cation as a catalyst to synthesize the target product, with a yield of 50% to 98%. . However, domestic Chen Jiexiao, Luo Jinyue and others use SO 4 2- / ZrO ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/22B01J31/02
CPCC07D317/22B01J27/16B01J31/0201B01J35/19
Inventor 马洪亮姜兴涛李锐李剑政吴奇林李庆廷
Owner SHENZHEN BOTON FLAVORS & FRAGRANCES
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