Method for preparing valerolactone

A technology of valerolactone and levulinic acid, applied in chemical instruments and methods, chemical elements of heterogeneous catalysts, organic chemistry, etc., can solve problems such as high reaction conditions such as reaction temperature or reaction pressure, and achieve high yield, reaction mild effects

Inactive Publication Date: 2016-02-24
林康艺
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the prior art, selective hydrogenation from levulinic acid to valerolactone requires higher reaction conditions such as reaction temperature or reaction pressure

Method used

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  • Method for preparing valerolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Preparation of Palladium-loaded Aluminum Nitride:

[0018] Disperse 500mg of aluminum nitride into 10ml of distilled water, add an aqueous solution containing 70mg of potassium chloropalladate, stir at 80°C for 1h, then slowly add sodium borohydride solution (NaBH 4 / Pd molar ratio is 5:1), stirred at room temperature for 4h, filtered, washed with distilled water, and vacuum dried at 80°C to obtain aluminum nitride (5%Pd / ALN) loaded with 5% palladium.

[0019] Catalyzed levulinic acid to prepare valerolactone:

[0020] Accurately weigh 200 mg of levulinic acid and 100 mg of catalyst and add them to the lining of the autoclave, and add 3 ml of water. After sealing the stainless steel autoclave, it was ventilated with hydrogen for 3 times, and then flushed with 1MPa hydrogen at room temperature. Preheat the oil bath to the required temperature, put it into the autoclave, react at 80°C for 4h, stop the reaction, and cool to room temperature.

[0021] After the reaction,...

Embodiment 2~9

[0023] The difference from Example 1 lies in the reaction temperature, hydrogen pressure, loading amount of palladium, mass ratio (A) of palladium-loaded aluminum nitride to levulinic acid, and different palladium. The results are shown in Table 1.

[0024] Table 1

[0025]

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Abstract

The invention discloses a method for preparing valerolactone. The method comprises the following steps: putting acetylpropionic acid and palladium-loaded aluminum nitride into a reaction device; adding distilled water and introducing hydrogen gas to react at 60 DEG C to 100 DEG C for 1 to 6 hours, wherein the loading amount of palladium is 1 percent to 10 percent, the pressure of the hydrogen gas is 0.5MPa to 2MPa, and the mass ratio of the palladium-loaded aluminum nitride to the acetylpropionic acid is (0.2 to 0.8):1. The method has moderate reaction conditions and has a relatively high valerolactone yield.

Description

technical field [0001] The invention relates to a method for preparing valerolactone. Background technique [0002] Hydrogenation reaction is one of the important reactions for converting biomass raw materials to produce fuels and fine chemicals. Levulinic acid from biomass feedstock is an excellent platform compound for the preparation of other important fine chemicals through hydrogenation reactions. Levulinic acid can be selectively hydrogenated to valerolactone, a valuable chemical used as a solvent for resins and as an intermediate for various related compounds. It is also used as a lubricant, plasticizer, gelling agent for non-ionic surfactants, lactone additives for leaded gasoline, and used for dyeing of cellulose esters and synthetic fibers. Valerolactone has a vanillin and coconut fragrance. my country's GB2760-86 stipulates that it is allowed to use edible spices. It is mainly used to prepare peach, coconut, vanilla and other flavors. It is also used as a sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33B01J27/24
CPCC07D307/33B01J27/24B01J2523/31B01J2523/824
Inventor 林康艺
Owner 林康艺
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