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

A technology of angelica lactone and catalyst, which is applied to the catalyst for preparing γ-valerolactone from α-angelica lactone and the field of preparation and application, can solve the problems of long reaction time, complicated process, high process cost and the like, and achieves product yield. The effect of high rate, good safety and simple process

Active Publication Date: 2012-11-14
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 1～3

[0018] Catalyst preparation:

[0019] The nitrate of the active component and manganese nitrate (or barium nitrate, zirconium nitrate) are formulated into a mixed solution according to the composition of the catalyst (see Table 1 for the composition of the catalyst), and are impregnated on the silicon-aluminum composite carrier in equal volume at room temperature. Dry in an oven at ℃ for 24h, and bake at 350℃ for 24h to obtain the agents of Examples 1-3. The reaction conditions and results of hydrogenation of α-angelica lactone to prepare γ-valerolactone are shown in Table 1.

Embodiment 4～9

[0021] Catalyst preparation:

[0022] The chloride salt of the active component and manganese chloride (or barium chloride, zirconium oxychloride) are formulated into a mixed solution according to the catalyst composition (see Table 1 for the composition of the catalyst), and impregnated into the alumina carrier at room temperature above, dried in an oven at 120°C for 2h, and calcined at 600°C for 2h to obtain the agents of Examples 4-9. The reaction conditions and results of hydrogenation of α-angelica lactone to prepare γ-valerolactone are shown in Table 1.

Embodiment 10～12

[0024] Catalyst preparation:

[0025] The chloride salt of the active component and manganese chloride (or barium chloride, zirconium oxychloride) are formulated into a mixed solution according to the composition of the catalyst (see Table 1 for the composition of the catalyst), and impregnated into the silica carrier in equal volume at room temperature Dry in an oven at 100°C for 12 hours, and bake at 400°C for 16 hours to obtain the curing agents of Examples 10-12. The reaction 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 relates to a catalyst for preparing gamma-valerolactone by alpha-angelica lactone, which is characterized by comprising the following components by weight percent calculated by oxide: 0.5-15% of active component, 0.05-20% of catalyst accelerator and the balance of carrier. The invention has the advantages of low cost, simple process, easy operation, high product yield and good 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 Patents(China)
IPC IPC(8): B01J23/656B01J23/58B01J23/46B01J23/44B01J23/42C07D307/33
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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