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Acid-proof catalyst for preparing gamma-valerolactone from levulinic acid, preparation method and application

An acid-resistant catalyst, levulinic acid technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problem of long reaction time, complex process and process cost. Expensive and other problems, to achieve the effect of high product yield, good safety and simple process

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 cyclization. The process is 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. The reaction process is easy to generate peroxide, and there is a risk of explosion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0025] Catalyst preparation:

[0026] The nickel nitrate and the nitrate of the co-catalyst were prepared into a mixed solution with a certain concentration according to the composition of the catalyst (see Table 1 for the composition of the catalyst), impregnated with equal volume on the carrier alumina at room temperature, and dried in an oven at 120°C for 2 hours. After the obtained catalyst was dried, it was subjected to high-temperature treatment at 1500° C. for 3 hours to obtain the catalysts of Examples 1-3.

[0027] Preparation of γ-valerolactone by hydrogenation of levulinic acid:

[0028] Take 10ml of the catalysts of Examples 1-3, evaluate in a fixed bed, and raise the temperature from room temperature to 400°C under hydrogen at a rate of 0.5°C / min. After keeping for 5h, the temperature was lowered to the reaction temperature and the reaction was carried out. The raw material used is levulinic acid, and the reaction temperature, pressure, liquid hourly space veloc...

Embodiment 4～6

[0030] Catalyst preparation:

[0031] Copper nitrate and cocatalyst nitrate were formulated into a mixed solution according to the composition of the catalyst (see Table 1 for the composition of the catalyst), impregnated with equal volumes on the carrier alumina at room temperature, and dried in an oven at 90°C for 24 hours, and the resulting dried catalyst After high-temperature treatment at 700°C for 36 hours, the catalysts of Examples 4-6 were obtained.

[0032] Preparation of γ-valerolactone by hydrogenation of levulinic acid:

[0033] Take 10ml of the catalysts of Examples 4-6, evaluate in a fixed bed, and raise the temperature from room temperature to 300°C under hydrogen at a rate of 0.5°C / min. After keeping for 5h, the temperature was lowered to the reaction temperature and the reaction was carried out. The raw material used is levulinic acid, and the reaction temperature, pressure, space velocity and hydrogen-oil volume ratio are shown in Table 1, and the obtained ...

Embodiment 7～9

[0035] Catalyst preparation:

[0036] Mix nickel nitrate and cocatalyst nitrate according to the composition of the catalyst (see Table 1 for details of the composition of the catalyst), impregnate the same volume on the carrier chromium oxide at room temperature, dry in an oven at 100 ° C for 12 hours, and dry the obtained catalyst After high-temperature treatment at 800°C for 24 hours, the catalysts of Examples 7-9 were obtained.

[0037] Preparation of γ-valerolactone by hydrogenation of levulinic acid:

[0038] Take 10ml of the catalysts of Examples 7-9, evaluate in a fixed bed, and raise it from room temperature to 500°C under hydrogen at a rate of 0.5°C / min. After keeping for 5h, the temperature was lowered to the reaction temperature and the reaction was carried out. The raw material used is levulinic acid, and the reaction temperature, pressure, space velocity and hydrogen-oil volume ratio are shown in Table 1, and the obtained results are shown in Table 1.

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PUM

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Abstract

An acid-proof catalyst for preparing gamma-valerolactone from levulinic acid is characterized by comprising the following components in percentage by mass: based on an oxide, 10 to 70 percent of active component, 0.05 to 20 percent of catalyst accelerator, and the balance of carrier. The acid-proof catalyst has the advantages of low cost, simple process, easy operation, high product yield rate and high safety in a production process.

Description

technical field [0001] The invention belongs to an acid-resistant catalyst for preparing gamma-valerolactone by hydrogenation of levulinic acid, a preparation method and application. Background technique [0002] With the increasing shortage of petrochemical resources and the deterioration of the environment, biomass, as a green renewable resource, has attracted more and more attention at home and abroad. Reaction of biomass or biomass-based platform compounds to generate bio-based chemicals with specific structures is one of the fundamental ways to solve resource and environmental problems, and has broad development prospects. [0003] As an important biomass-based chemical, γ-valerolactone can be used as food flavor, organic synthesis intermediate, polymer polyester monomer, vehicle fuel, adhesive, etc. 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 o...

Claims

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Application Information

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IPC IPC(8): B01J23/889B01J23/78B01J23/755B01J23/86B01J23/72C07D307/33
Inventor 李学宽唐明兴陈铁牛侯相林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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