Catalyst for preparing gamma-valerolactone from alpha-angelica lactone, and preparation method and application thereof

A technology of angelica lactone and catalyst, which is applied in the catalyst, preparation method and application field of preparing gamma-valerolactone from alpha-angelica lactone, can solve the problems of long reaction time, complex process, many by-products, etc., and achieve The effect of high product yield, good safety and easy operation

Active Publication Date: 2010-06-16
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Liu Daojun et al. (Perfume, Fragrance and Cosmetics, 1999, 4, 1-4) used levulinic acid as a raw material to prepare γ-valerolactone through three processes of lye neutralization, catalytic hydrogenation and acid lactonization, and the process was complicated. , many side reactions, low yield
Tang Tianshu (Spice, Fragrance and Cosmetics, 1996, 4, 5-7) reported a method for synthesizing γ-valerolactone using levulinic acid as raw material through esterification, microbial carbonyl reduction and lactonization. Breeding is difficult, the reaction time is long, the by-products are many, and the yield is only 61.1%.
Patent WO 02074760 shows that levulinic acid can react with 700-800psi hydrogen under the action of a noble metal catalyst to generate γ-valerolactone, and the yield can reach 96%, but the process cost is expensive due to the use of noble metals, and it is difficult to produce on a large scale
The patent US0254384 pointed out that in supercritical carbon dioxide medium, the highest yield of this reaction can reach 99%, but the process needs to consume a lot of carbon dioxide, and will produce a small amount of 2-methyltetrahydrofuran (peroxides are easily generated under the reaction process, and there is a risk of explosion)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Adopt the precipitation method to prepare the catalyst with zinc oxide as the carrier, according to the catalyst composition, the nitrate and zinc nitrate of the active component, the cocatalyst are made into a mixed solution (the composition of the catalyst is shown in Table 1), and the mixture is mixed with sodium carbonate lye. Precipitation, the reaction temperature is 50°C, and the pH is controlled at around 9.0. After the feeding is completed, it is aged at the reaction temperature for 1 hour, filtered and washed 5 times. The obtained filter cake was dried in an oven at 90° C. for 24 hours, and then calcined at 350° C. for 24 hours to obtain the catalyst of Example 1. The process conditions and results of hydrogenation of α-angelica lactone to prepare γ-valerolactone are shown in Table 1.

Embodiment 2

[0027] Adopt the precipitation method to prepare the catalyst with zinc oxide as the carrier, according to the catalyst composition, the nitrate and zinc nitrate of the active component, the promoter are made into a mixed solution (the composition of the catalyst is shown in Table 1), and the ammonium carbonate lye is added dropwise to In the prepared nitrate mixed solution, the reaction temperature is 90°C, and the pH is controlled at about 6.0. After the feeding is completed, it is aged at the reaction temperature for 1 hour, filtered and washed 3 times. The obtained filter cake was dried in an oven at 120° C. for 2 hours, and then calcined at 600° C. for 2 hours to obtain the catalyst of Example 2. The process conditions and results of hydrogenation of α-angelica lactone to prepare γ-valerolactone are shown in Table 1.

Embodiment 3

[0029] Adopt the precipitation method to prepare the catalyst with zinc oxide as the carrier, add the mixed solution of the active component, the nitrate of the cocatalyst and the zinc nitrate (the composition of the catalyst is shown in Table 1) dropwise in the sodium carbonate lye, react The temperature is 80°C, and the pH is controlled at about 7.0. After the feeding is completed, it is aged at the reaction temperature for 1 hour, filtered and washed 5 times. The obtained filter cake was dried in an oven at 100° C. for 12 hours, and then calcined at 500° C. for 5 hours to obtain the catalyst of Example 3. The process conditions and results of hydrogenation of α-angelica lactone to prepare γ-valerolactone are shown in Table 1.

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PUM

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Abstract

The invention provides a catalyst for preparing gamma-valerolactone from alpha-angelica lactone, which is characterized by comprising the following components in percentage by mass of oxide: 10-90% of an active component, 0.05-20% of a cocatalyst and a carrier. The method has the advantages of low cost, simple technique, easy operation, high product yield and high safety in the production process.

Description

technical field [0001] The invention belongs to a catalyst for preparing gamma-valerolactone by hydrogenation of alpha-angelica lactone, a preparation method and application. Background technique [0002] γ-valerolactone (C 5 h 8 o 2 , Mw=100.10), the chemical name is 4-hydroxy-3-pentenolide or 5-methyl-2(3H)-furanone, which can be used as food flavor, organic synthesis intermediate, polymer polyester unit Body, vehicle fuel, adhesives, etc. are used in many industries. In my country, this product is only produced in small batches, and the price is very expensive, which seriously affects the promotion and utilization of this product. [0003] At present, the preparation method of gamma-valerolactone mainly uses levulinic acid as a raw material, and it is obtained by first hydrogenating with a heterogeneous catalyst and then lactonizing. Liu Daojun et al. (Perfume, Fragrance and Cosmetics, 1999, 4, 1-4) used levulinic acid as a raw material to prepare γ-valerolactone thr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/889B01J23/80B01J23/78B01J23/755C07D307/33
Inventor 侯相林唐明兴陈铁牛李学宽齐永琴杜明仙吕占军周立公
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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