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4-dimethylaminopyridine supported catalyst used for preparation of menthol ester lactate

A technology of dimethylaminopyridine and supported catalysts, applied in the direction of physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, carboxylate preparation, etc., can solve the problem of not giving yield, not giving Synthetic reaction details, etc.

Inactive Publication Date: 2011-06-01
ZHEJIANG SHUREN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent does not give details of the synthetic reaction nor the yield of ML obtained

Method used

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  • 4-dimethylaminopyridine supported catalyst used for preparation of menthol ester lactate
  • 4-dimethylaminopyridine supported catalyst used for preparation of menthol ester lactate
  • 4-dimethylaminopyridine supported catalyst used for preparation of menthol ester lactate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of 5% 4-dimethylaminopyridine / attapulgite catalyst

[0024] Weigh 4-dimethylaminopyridine (C 7 h 10 N 2 ) 1g, be dissolved in 95% ethanol, take by weighing attapulgite 19g roasted at 150 ℃ for 4 hours and mix with 4-dimethylaminopyridine solution, the impregnation medium is 95% ethanol, solid-to-liquid ratio (impregnation medium volume and carrier Mass ratio) 1mL / g. Stir at room temperature for 20 minutes, let stand for 1 hour, and then stir for 10 minutes; after the catalyst filter cake is air-dried, keep it in an oven at 80°C for 1 hour, and then activate it at 160°C for 2 hours to obtain 5% 4-dimethylaminopyridine / Attapulgite catalyst.

Embodiment 2

[0026] Preparation of 10% 4-dimethylaminopyridine / attapulgite catalyst

[0027] Weigh 4-dimethylaminopyridine (C 7 h 10 N 2 ) 2g, be dissolved in 95% ethanol, take by weighing attapulgite 28g roasted at 200 ℃ for 3 hours and mix with 4-dimethylaminopyridine solution, the impregnation medium is deionized water, solid-to-liquid ratio (impregnation medium volume and carrier Mass ratio) 3mL / g. Stir at room temperature for 20 minutes, let stand for 1 hour, and then stir for 10 minutes; after the catalyst filter cake is air-dried, keep it in an oven at 85°C for 2 hours, and then activate it at 150°C for 1.5 hours to obtain 10% 4-dimethylaminopyridine / Attapulgite catalyst.

Embodiment 3

[0029] Preparation of 15% 4-dimethylaminopyridine / attapulgite catalyst

[0030] Weigh 4-dimethylaminopyridine (C 7 h 10 N 2 ) 4g, be dissolved in 95% ethanol, take by weighing attapulgite 16g roasted 2 hours at 220 ℃ and mix with 4-dimethylaminopyridine solution, impregnation medium is 95% ethanol, solid-to-liquid ratio (impregnation medium volume and carrier Mass ratio) 5mL / g. Stir at room temperature for 20 minutes, let stand for 1 hour, and then stir for 10 minutes; after the catalyst filter cake is air-dried, keep it in an oven at 90°C for 2.5 hours, and then activate it at 140°C for 2 hours to obtain 20% 4-dimethylaminopyridine / Attapulgite catalyst.

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PUM

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Abstract

The invention relates to a 4-dimethylaminopyridine supported catalyst used for esterification reaction of lactic acid and menthol. A catalyst carrier is attapulgite; a 4-dimethylaminopyridine catalyst supported on the attapulgite is prepared by an impregnation method first, and the 4-dimethylaminopyridine catalyst can be used for catalyzing and synthesizing the menthol ester lactate; and the yield of the menthol ester lactate can reach over 90 percent under the optimizing condition. The 4-dimethylaminopyridine supported catalyst has the advantages of high activity, capability of being used repeatedly and the like and is easy to separate. The menthol ester lactate is fresheners widely used in spices, oral cavity care and cosmetics.

Description

technical field [0001] The invention relates to an esterification catalyst, a preparation method and an application of menthol and lactic acid. The esterification product, menthyl lactate, is a cooling agent widely used in spices, oral care and cosmetics. Background technique [0002] Menthyl lactate is an ester of menthol and lactic acid, a cooling agent widely used in flavors, oral care, and cosmetics. [0003] Replacing traditional catalysts in esterification reaction with solid catalysts has become an important field of catalytic research. Heterogeneous catalysts are easy to separate from the reaction products and can also be the basis for fixed-bed catalysis. Attapulgite is a kind of hydrous magnesium-rich phosphate clay mineral with chain layer structure. With high compressive strength and large specific surface area, it is mainly used for molecular sieves in the chemical industry. [0004] In the 1960s, when Litvinenko and others used 4-dimethylaminopyridine instea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C69/68C07C67/08
Inventor 金建忠哈成勇
Owner ZHEJIANG SHUREN UNIV
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