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Gradient catalysis technology for synthesizing cooling agent mono-L-menthyl glutarate

A technology of glutaric acid mono-catalysis technology, which is applied in the field of synthesizing cooling agent glutaric acid mono-L-menthyl by gradient catalytic technology, which can solve the problem of unstable content ratio of dimenthyl glutaric acid mixture and inability of menthol Reaction, the use of a large amount of solvent and other problems, to achieve the effect of reducing risk, increasing the ratio, and using less solvent

Active Publication Date: 2020-07-03
ANHUI CHINAHERB FLAVORS & FRAGRANCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Therefore, the prior art adopts strong acid catalysis for the synthetic menthyl glutarate to quickly form dimenthyl glutarate, the product yield is low, and the amount of solvent used is large, menthol c

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0026] Example 1

[0027] Weigh 200 mesh 10g silica gel, then add 25g of 20wt% sodium carbonate aqueous solution, stir for 1 hour, then let stand for 5 hours, filter out the white particles through a 500 mesh filter, put it in a 150 ℃ oven, bake for 3 hours to dry , the dried particles were added to 100 g of 10wt% sodium hydrogen sulfate ethanol solution, stirred for 4.5 hours, the particles gradually grew up, then filtered out the particles, put into an oven, and dried at 60 ° C for 1 hour to obtain 17 g of catalyst. First weigh 124.8g of menthol in the reactor, then add 100.3g of glutaric anhydride, add 17g of catalyst, then add 60g of tetrahydrofuran; start stirring, the stirring speed is controlled at 100r / min, turn on heating, and the heating temperature is 82 ℃, catalyzed by sodium bisulfate for 3 hours, then heated to 90 ℃, catalyzed by sodium carbonate for 4 hours, and the stirring rate was controlled at 200 r / min; sampling, the menthol was completely converted, the he...

Example Embodiment

[0028] Example 2

[0029] Weigh 200 mesh 10g silica gel, then add 25g of 20wt% sodium carbonate aqueous solution, stir for 1 hour, then stand for settling for 5 hours, filter out the white particles through a 500 mesh filter, put it in a 150 ℃ oven, bake for 3 hours to dry , the dried particles were added to 100 g of a 15wt% sodium hydrogen sulfate ethanol solution, stirred for 4.5 hours, the particles gradually grew, and then filtered out of the particles, placed in an oven, and dried at 60°C for 1 hour to obtain 17 g of catalyst. First weigh 124.8g of menthol in the reaction kettle, then add 118.8g of glutaric anhydride, add 17g of catalyst, then add 60g of tetrahydrofuran; start stirring, the stirring speed is controlled at 100r / min, turn on heating, and the heating temperature is 85°C, catalyzed by sodium bisulfate for 3 hours, then heated to 90°C, catalyzed by sodium carbonate for 4.5 hours, and the stirring rate was controlled at 200 r / min; sampling, the menthol was comp...

Example Embodiment

[0030] Example 3

[0031]Weigh 200 mesh 15g silica gel, then add 25g of 20wt% sodium carbonate aqueous solution, stir for 1 hour, then let stand for 5 hours, filter out the white particles through a 500 mesh filter, put it into a 150 ℃ oven, bake for 3 hours to dry , the dried particles were added to 100 g of 15wt% sodium bisulfate ethanol solution, stirred for 4.5 hours, the particles gradually grew up, then filtered out the particles, put into an oven, and dried at 60 ° C for 1 hour to obtain 21.7 g of catalyst. First weigh 124.8g of menthol in the reactor, then add 118.8g of glutaric anhydride, add 17g of catalyst, then add 60g of tetrahydrofuran; start stirring, the stirring speed is controlled at 100r / min, turn on heating, and the heating temperature is 83 ° C, catalyzed by sodium hydrogen sulfate for 3 hours, then heated to 94 ° C, catalyzed by sodium carbonate for 5 hours, and the stirring rate was controlled at 200 r / min; sampling, the menthol was completely converted,...

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Abstract

The invention discloses a gradient catalysis technology for synthesizing a cooling agent mono-L-menthyl glutarate. The method comprises the following steps: adding menthol, glutaric anhydride, a catalyst and an organic solvent into a reaction kettle, uniformly stirring and mixing, heating to carry out catalytic reactions, filtering after reactions to obtain a mixed solution; adding water into themixed solution, fully stirring, standing, and separating a lower water layer from an upper oil layer; adding the oil layer into a distillation kettle, and carrying out fractional distillation to obtain the product. The defects in the prior art are overcome, the gradient temperature is adopted, the maximal catalytic efficiency of the catalyst can be achieved, synthesis of double menthyl glutarate is hindered, the yield of mono-L-menthyl glutarate is increased, in the synthesis process, the use amount of a solvent is small, the danger of industrial production is reduced, and the method has economic and environmental protection values.

Description

technical field [0001] The invention relates to the technical field of synthesizing the cooling agent glutaric acid mono-L-menthyl, and specifically belongs to the synthesis of the cooling agent glutaric acid mono-L-menthyl by gradient catalysis technology. Background technique [0002] As a cooling agent, natural menthol has very important uses in daily chemicals, food, medicine and cigarette products. However, due to the high volatility and irritation of menthol, its cooling effect is short and strong, and it is even harmful to human skin and skin. Eyes are harmful, and its special mint smell limits its wide application in daily chemical products. L-menthyl glutarate is a new type of cooling agent. The national standard requires the content of monomenthyl glutarate to be greater than or equal to 72%, and the content of dimenthyl glutarate to be less than 28%. There is no requirement for menthol. However, the national standard requires that L-menthyl glutarate can be added...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/42C07C67/48
CPCC07C67/08C07C67/48C07C69/42
Inventor 李莉党亚李淑清范金材赵娅罗放赵宝葛树辉
Owner ANHUI CHINAHERB FLAVORS & FRAGRANCES
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