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A kind of synthetic method of gamma-valerolactone

A synthetic method, the technology of valerolactone, which is applied in the direction of organic chemistry, can solve the problems of unfriendly chromium to the human body and the environment, and achieve the effects of good reusability, strong operation safety and good economy

Active Publication Date: 2019-10-29
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the composition of the catalyst includes chromium, which is unfriendly to the human body and the environment. Due to environmental protection requirements, it is necessary to consider the comprehensive recovery of chromium and copper in the catalyst

Method used

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  • A kind of synthetic method of gamma-valerolactone
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  • A kind of synthetic method of gamma-valerolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～7

[0029] Add 0.5 g of methyl levulinate and 19.5 g of methanol (2.5 wt %) to a 100 mL autoclave, and then add 0.2 g of CuMgO 2 , CuZnO 2 、CuCaO 2 , CuZrO 3 , CuAlO 2.5 , CuNiO 2.5 、CuBaO 2 (The molar ratio of the two metals is 1:1) As a catalyst, seal the reaction vessel, stir vigorously (500rpm), heat to 220°C and keep it for 4 hours, finish the reaction, cool to room temperature and take a sample, use GC-MS (Shimadzu) Qualitative and quantitative detection were carried out with GC (Agilent), and the detection results are listed in Table 1 as serial numbers 1-7.

Embodiment 8

[0031] Add 1.0 g of methyl levulinate and 19.0 g of isopropanol (5 wt%) to a 100 mL autoclave, and then add 0.2 g of Cu 4 MgO 5 (The molar ratio of copper and magnesium is 4:1) as a catalyst, seal the reaction vessel, stir vigorously (500rpm), heat to 240°C and keep for 2 hours, finish the reaction, cool to room temperature and take a sample, use GC-MS (Shimadzu) and GC (Agilent) for qualitative and quantitative detection (eg figure 1 Shown), the test results are listed in Table 1 with the serial number 8.

Embodiment 9～12

[0033] Add 0.8g methyl levulinate and 19.2g 1-butanol (4wt%) to a 100mL autoclave, then add 0.2g CuMg 2 o 3 , CuZn 2 o 3 , CuCa2 o 3 、Cuba 2 o 3 (the molar ratio of Cu and another active metal is 1:2) as a catalyst, seal the reactor, stir vigorously (500rpm), heat to 260°C and keep for 1 hour, finish the reaction, cool to room temperature and take samples, use GC-MS (Shimadzu) and GC (Agilent) for qualitative and quantitative detection, and the detection results of different catalysts are listed in Table 1 as serial numbers 9-12.

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Abstract

The invention discloses a synthetic method of gamma-valerolactone. The synthetic method of gamma-valerolactone comprises the following steps of: (1) fully mixing methyl levulinate with an alcohol to obtain a mixed raw material liquid, wherein the concentration of the methyl levulinate in the mixed raw material liquid is 2-12wt%; and (2) adding a double metal catalyst into the mixed raw material liquid, heating the mixed raw material liquid in a high pressure reaction kettle to 170-290 DEG C to react for 0.5-9h, and cooling the mixture to room temperature to obtain gamma-valerolactone. By applying a copper-based double metal catalyst, the activity of the catalyst is adjusted by doping a second active metal, so that gamma-valerolactone can be prepared by catalytic in-situ hydrogen production by alcohol and selective catalytic hydrogenation of methyl levulinate.

Description

technical field [0001] The invention belongs to the technical field of organic catalytic synthesis, and in particular relates to a synthesis method of gamma-valerolactone. Background technique [0002] γ-valerolactone is non-toxic and biodegradable, and is considered to be one of the most promising biomass-based platform compounds, which can be used as a renewable carbon source to produce carbon-based chemicals and energy. In recent years, it has received more and more attention from academia and industry. As a raw material, γ-valerolactone can participate in the Ivanov reaction to synthesize drugs, and can synthesize various multi-substituted naphthalenthrenyl compounds through Friedel-Crafts reaction and cyclization, reduction and dehydration reactions of phenyl aromatic compounds, γ-valerolactone It is also possible to synthesize pentenoic acid, butene, valeric acid and 5-nonanone through cyclization and decarboxylation / hydrogenation respectively; in addition, the produc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 唐兴曹雪娟孙勇曾宪海林鹿雷廷宙
Owner XIAMEN UNIV
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