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A method for preparing 4-hydroxyl-6-methyltetrahydro-2-pyrone

A technology of methyltetrahydro and pyrone, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problems of easy degradation of triacetin lactone and other problems , to achieve the effect of low cost, simple and safe operation

Active Publication Date: 2020-01-24
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first step in the conversion of triacetolactone is catalytic hydrogenation. The current problem is that triacetolactone is easily degraded in aqueous solution. The hydrogenation step needs to use n-butanol as a solvent, hydrogen as a hydrogen source, and noble metals as a catalyst.

Method used

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  • A method for preparing 4-hydroxyl-6-methyltetrahydro-2-pyrone
  • A method for preparing 4-hydroxyl-6-methyltetrahydro-2-pyrone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0015] This example provides the preparation of different metal nanoparticles, and the experiment of catalytic hydrogen transfer triacetolactone to prepare 4-hydroxy-6-methyltetrahydro-2-pyrone:

[0016] Preparation of nickel nanoparticles: Dissolve 0.1g of nickel nitrate in 4mL of water, add dropwise to a mixture of 40mL of ethylene glycol and 40mL of water, ultrasonically disperse for 30min, add 16mL of sodium borohydride aqueous solution (0.01g / mL) dropwise to the above The solution was stirred at room temperature for 8h, filtered, and dried in vacuum at 80°C for 24h.

[0017] Preparation of cobalt nanoparticles: Dissolve 0.1g cobalt nitrate in 4mL water, add dropwise to the mixture of 40mL ethylene glycol and 40mL water, ultrasonically disperse for 30min, add 16mL sodium borohydride aqueous solution (0.01g / mL) dropwise to the above The solution was stirred at room temperature for 8h, filtered, and dried in vacuum at 80°C for 24h.

[0018] Preparation of copper nanoparticl...

Embodiment 5-10

[0024] This example provides an experiment for preparing 4-hydroxy-6-methyltetrahydro-2-pyrone by hydrogenation of triacetolactone when different alcohol compounds are used as hydrogen donors:

[0025] Add 0.02g of nickel nanoparticles into the autoclave, then add 0.25g of triacetolactone and 5mL of different alcohol compounds (both as a hydrogen donor and as a reaction solvent), seal it, replace it with nitrogen five times, and then fill it with Inject 0.1MPa of nitrogen gas, react at 50°C for 10 h, and analyze and quantify the composition of the product after the reaction is completed using high-performance liquid chromatography. The specific results are shown in Table 2:

[0026] Table 2. Catalytic results when using different alcohol compounds as hydrogen donors

[0027] Example different alcohols Conversion rate(%) selectivity (%) Yield(%) 5 n-propanol 40 70 24 6 Butanol 50 54 27 7 n-pentanol 48 31 15 8 Cyclohexanol 45 ...

Embodiment 11-13

[0029] This example provides the experiment of preparing 4-hydroxy-6-methyltetrahydro-2-pyrone by hydrogenation of triacetolactone at different reaction temperatures:

[0030] Add 0.02g of nickel nanoparticles into the autoclave, then add 0.25g of triacetolactone and 5mL of different alcohol compounds (both as a hydrogen donor and as a reaction solvent), seal it, replace it with nitrogen five times, and then fill it with Inject 0.1MPa nitrogen, react at different temperatures for 10 h, and use high-performance liquid chromatography to analyze and quantify the composition of the product after the reaction. The specific results are shown in Table 3:

[0031] Table 3. Catalytic results at different temperatures

[0032] Example temperature(℃) Conversion rate(%) selectivity (%) Yield(%) 11 50 100 89 89 12 75 100 90 90 13 100 100 75 75

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Abstract

The invention discloses a method for preparing 4-hydroxy-6-methyltetrahydro-2-pyrone, which includes the following steps: mixing triacetolactone raw materials and alcohol compounds with hydrogen donors and adding them to a closed high-pressure In the reaction kettle, under the conditions of nitrogen pressure of 1-12MPa, reaction temperature of room temperature-150℃, and presence of catalyst, hydrogen transfer reaction was carried out for 0.5-48h to obtain 4-hydroxy-6-methyltetrahydro-2-pyran. Ketone, the catalyst is non-noble metal nanoparticles. The method does not require the use of precious metals, has low cost, is easy to separate and can be reused many times, has a simple reaction system and is easy to be industrialized.

Description

technical field [0001] The present invention specifically relates to a method for preparing 4-hydroxy-6-methyltetrahydropyrone. Background technique [0002] Biomass is the only renewable source of organic carbon and is an ideal candidate to replace petroleum in the production of fuels and chemicals. Therefore, making full use of the organic carbon resources in biomass and developing new routes and methods for converting biomass to fuels and chemicals has become a research hotspot in the field of new energy and new materials. The platform molecules synthesized by microorganisms provide new opportunities for the conversion of carbohydrates into commercial chemicals. These platform molecules derived from microorganisms are the products of a single metabolic pathway of microorganisms and have flexible and controllable functional groups. Chemical catalytic upgrades can convert these platform molecules Transformed into a variety of end products to replace existing petrochemical ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D309/30B01J23/755B01J23/75B01J23/72
CPCC07D309/30B01J23/72B01J23/75B01J23/755B01J35/40Y02P20/584
Inventor 李福伟孙鹏高广夏春谷赵泽伦龙向东吴君
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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