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Bimetallic catalyst for preparing methylbutyrolactone by heterogeneous catalytic hydrogenation and preparation method thereof

A bimetallic catalyst and butyrolactone technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve complex and difficult synthetic routes, simple molecular structures, etc. problem, to achieve the effect of low price, simple process and easy preparation

Active Publication Date: 2018-05-29
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis methods of α-methyl-γ-butyrolactone and β-methyl-γ-butyrolactone still rely on organic chemical synthesis. The molecular structure is simple but the synthesis route is complicated and difficult, which is a difficulty in organic synthesis. At present, these compounds are still mainly derived from fossil fuels. Therefore, with the depletion of fossil resources such as coal and oil and the increasingly serious environmental pollution problems, the development of biomass energy and bio-based chemicals can reduce the dependence on fossil raw materials and realize the utilization of energy resources. Sustainability is very necessary

Method used

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  • Bimetallic catalyst for preparing methylbutyrolactone by heterogeneous catalytic hydrogenation and preparation method thereof
  • Bimetallic catalyst for preparing methylbutyrolactone by heterogeneous catalytic hydrogenation and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1: 5%Pd-10%Cu / TiO 2 Catalyst preparation

[0030] Weigh 0.537g copper chloride dihydrate (CuCl 2 2H 2 O) and 0.175g palladium chloride (the metal content of palladium is 59.5wt%), after adding 6mL ethanol and 0.5mL hydrochloric acid to dissolve, adjust the pH value to 4.12 with dilute ammonia, add 2g carrier TiO after stirring for 10 minutes 2 Stir evenly, then adjust the pH value to 8.56 with ammonia water, after stirring evenly, let it stand at room temperature for 10h, dry it in an oven at 80°C for 5h, and reduce the dried product with hydrogen (reduction condition: 300°C, 5h, hydrogen Flow rate: 50ml / min), the catalyst 5%Pd-10%Cu / TiO that will reduce finally 2 After taking it out, keep it sealed for later use. Examples 2-8 are examples of evaluating the activity of the prepared catalyst, and the evaluation results are shown in Table 1.

Embodiment 2

[0031] Example 2: 5%Pd-10%Cu / TiO 2 Catalytic Hydrogenation of Methanol Solution of Itaconic Acid

[0032]Add 20mL of 1wt% methanol solution of itaconic acid into a 50mL stainless steel autoclave, with respect to itaconic acid, the added molar ratio (active component mol / raw material mol, the active component is the metal component in the catalyst) is 3mol% The ratio of adding 5%Pd-10%Cu / TiO prepared in Example 1 2 catalyst. After replacement with hydrogen for three times, the initial pressure of hydrogen filling was 4MPa, stirring at a speed of 800rmp, and the temperature was programmed to rise to 180°C in 35 minutes. The reactor was connected to a computer to record the temperature and pressure changes during the reaction, and the reaction was carried out for 8 hours. After the reaction, cool to room temperature, take the centrifuged supernatant, pass through a 0.22 μm filter membrane, and analyze and detect by gas chromatography and high performance liquid chromatography. ...

Embodiment 3

[0033] Example 3: 5%Pd-10%Cu / TiO 2 Catalytic Hydrogenation of Ethanol Solution of Itaconic Acid

[0034] According to the method described in embodiment 2, use ethanol instead as reaction solvent, with the 5%Pd-10%Cu / TiO prepared in embodiment 1 2 The hydrogenation of ethanol solution of itaconic acid was catalyzed, and the experimental results are shown in Table 1.

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Abstract

The present invention relates to the field of catalyst synthesis, in particular to a bimetallic catalyst for preparing alpha- and beta-methyl-gamma-butyrolactone, and a preparation method thereof, and a method for preparing the alpha- and beta-methyl-gamma-butyrolactone through heterogeneous catalytic hydrogenation by adopting the catalyst. The noble metal supported catalyst prepared according to the method of the present invention has high activity and selectivity, is easy to prepare and low in price. By adopting the bimetallic catalyst of the present invention, the alpha-methyl-gamma-butyrolactone and beta-methyl-gamma-butyrolactone can be prepared by directly hydrotreating raw materials such as itaconic acid, other additional reaction steps are not needed, reaction conditions are mild, and the method is efficient, simple, easy in operation, economical, pollution-free, simple in process, and is beneficial to large-scale industrial production.

Description

technical field [0001] The invention relates to the field of catalyst synthesis, in particular to a bimetallic catalyst for the preparation of α- and β-methyl-γ-butyrolactone and a preparation method thereof, and the use of the catalyst to prepare α-butyrolactone through heterogeneous catalytic hydrogenation and β-methyl-γ-butyrolactone methods. Background technique [0002] Both α-methyl-γ-butyrolactone and β-methyl-γ-butyrolactone are very important chemical raw materials, widely used in the modification of liquid fuels, the synthesis of new materials, food additives and pharmaceutical research and development, etc. In the field, it is used to synthesize compounds such as pyrrolidone. In the patent CN 101781169A, it is reported that itaconic acid is hydrogenated with a non-noble metal catalyst to form 2-methyl-1,4-butanediol, 2-methylbutyrolactone, 3-methylbutyrolactone and 2-methylbutyrolactone Products such as succinate. [0003] At present, the synthesis methods of α...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C07D307/33
CPCB01J21/063B01J23/44B01J23/72B01J23/8926C07D307/33
Inventor 牟新东王喜成姜义军李慧曹泉
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI