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Catalyst system for preparing L-menthol and preparation method and application thereof

A technology of catalyst and menthol, which is applied in the catalyst system for preparing L-menthol and its preparation field, to achieve the effects of easy recovery, high catalytic activity, and reduced introduction of impurities

Active Publication Date: 2019-10-22
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a catalyst and method for preparing L-menthol, thereby solving many problems existing in the prior preparation of L-menthol technology

Method used

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  • Catalyst system for preparing L-menthol and preparation method and application thereof
  • Catalyst system for preparing L-menthol and preparation method and application thereof
  • Catalyst system for preparing L-menthol and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Place a 250mL reaction flask in an ice water bath, add 23mL98wt% concentrated sulfuric acid, add a solid mixture of 1g graphite powder and 0.5g sodium nitrate under stirring, and then add 3g potassium permanganate in 6 times, control the reaction temperature not to exceed 20℃ , Stir the reaction for 2 hours, then heat to 35℃, continue to stir for 30 minutes, then slowly add 46mL of deionized water, increase the temperature to 98℃, continue heating for 20 minutes, the solution is brown, add 5g hydrogen peroxide, continue stirring After 15 minutes, the reaction flask was removed and filtered while it was hot, and washed with 5 wt% HCl aqueous solution and deionized water until no sulfate radicals were detected in the filtrate. Finally, the filter cake was placed in a vacuum drying cabinet at 60° C. to fully dry the GO, which was dispersed in a deionized aqueous solution with a concentration of 5 mg / mL.

Embodiment 2

[0077] Add 0.05g of phosphomolybdic acid (additional amount is 5wt% of the mass of graphene oxide) to 200mL GO solution prepared in Example 1 for mixing and adsorption, ultrasonic dispersion for 30min, leave it for 24 hours to dry naturally, and then at 65℃ Vacuum drying until there is no free water, and then drying at 120°C for 5 hours to obtain phosphomolybdic acid-graphene oxide (HMoP-GO);

[0078] Take 1g of HMoP-GO and 10g of epigallocatechin gallate (EGCG) dissolved in 100g of water (HMoP-GO:EGCG: water mass ratio = 1:10:100), transfer to the reactor, and fill with nitrogen to 6MPaG, heating up to 90℃, stirring rate of 150rpm, stirring for 4 hours, then 0.22g nickel chloride (nickel addition amount is 10wt% of HMoP-GO) was added to the reactor, in nitrogen at 90℃, 150rpm at 6MPaG After stirring for 4 hours, the pressure was released and the temperature was lowered. The mixed solution was washed with deionized water three times and dried in vacuum at 70°C until there was no ...

Embodiment 3

[0081] Take 0.06g of phosphomolybdic acid (additional amount is 6wt% of the mass of graphene oxide) and add it to the 200mL GO solution prepared in Example 1 for mixing and adsorption, ultrasonic dispersion for 35min, leave it for 24 hours to dry naturally, and then at 70℃ Vacuum drying until there is no free water, and drying at 120°C for 5 hours to obtain phosphomolybdic acid-graphene oxide (HMoP-GO);

[0082] Take 1g of HMoP-GO and 7g of epigallocatechin gallate (EGCG) dissolved in 100g of water (HMoP-GO:EGCG: water mass ratio = 1:7:100), transfer them into the reactor, and fill with nitrogen to 5MPaG, heat up to 110℃, stir at 200rpm, stir for 3 hours, then add 0.264g nickel chloride (nickel addition amount is 12wt% of HMoP-GO) into the reaction kettle, 110℃, 200rpm under 5MPaG in nitrogen After stirring for 3 hours, the pressure was released and the temperature was reduced. The mixed solution was washed 3 times with deionized water, and dried in vacuum at 70°C until there was...

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Abstract

The invention discloses a catalyst system for preparing L-menthol and a preparation method and application thereof. The catalyst system structure for preparing L-menthol is nickel-phosphomolybdic acid-oxidized epigallocatechin gallate-graphene (Ni-HMOP-O EGCG-GN). Under the action of the catalyst, L-menthol is converted from L-menthone, and through the synergistic effect of various components of the heterogeneous catalyst, the reaction can be efficiently and rapidly carried out under mild conditions, the highest reaction conversion rate and chemical selectivity can reach more than 99.5%, the catalyst has long service life, the activity is basically stable after being applied for 20 times, and the highest application can reach 50 times.

Description

Technical field [0001] The invention belongs to the field of menthol preparation, and relates to a method for preparing and synthesizing chiral L-menthol from L-menthone, in particular to a catalyst system for preparing L-menthol and a preparation method and application thereof. Background technique [0002] Menthol, also known as menthol, is a type of natural cyclic terpene alcohol that exists in nature. The menthol molecule has 3 chiral centers, so there are 8 stereoisomers and 4 racemic compounds as shown below. D,L-menthol has a cooling effect, other isomers have no cooling effect, and the smell of L-menthol and D-menthol is obviously different. L-menthol is a brisk sweet pungent smell with a unique mint fragrance , D-menthol is a pungent pungent smell with a slight camphor smell. L-menthol has a cooling effect but D-menthol does not. Therefore, L-menthol has higher industrial value and can be used in daily and edible flavors, medicines, tobacco and oral products. [0003] ...

Claims

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Application Information

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IPC IPC(8): B01J31/34C07C29/145C07C35/12
CPCB01J31/34C07C29/145C07C2601/14C07C35/12Y02P20/584
Inventor 方文娟董菁王亚新于磊王联防于斌成张永振黎源
Owner WANHUA CHEM GRP CO LTD
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