Process for preparing ethyl pyruvate from ethyl lactate by gas-phase catalytic oxidizing

A technology of ethyl pyruvate and heterogeneous catalytic oxidation, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of sharp drop in selectivity, unsatisfactory, etc. The effect of easy preparation and simple preparation method

Inactive Publication Date: 2005-06-01
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under certain selectivity, the yield of ethyl pyruvate is all below 65%, which is not ideal
As the reaction temperature increases, the conversion rate increases, but the selectivity drops sharply

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 1.1 Catalyst preparation

[0014] Add 5 g fumed silica gel (Cab-O-Sil) to 10 mL containing 1.57 g AgNO 3 In the aqueous solution, let it stand at room temperature for half an hour, then dry it with infrared lamp under stirring, and then dry it at 120°C for 24 hours. The dried powder was calcined in static air at 350°C for 3 hours, and then reduced with hydrogen at 350°C for 5 hours before use.

[0015] 1.2 Catalytic reaction process

[0016] The reaction was carried out in a fixed-bed straight reaction tube with an inner diameter of 10 mm. The catalyst used was 500 mg of 20 wt% Ag / Cab-O-Sil of 20-40 mesh. Before the reaction, the temperature was raised to 350°C and reduced with hydrogen for 1 hour. When the temperature was lowered to 300°C, it was switched to a mixed gas of air and ethyl lactate. The flow rate of ethyl lactate was 0.6 g / hour, and air:ethyl lactate=15:1. The reaction mixture passed through the catalyst was analyzed online by gas chromatography (the c...

Embodiment 2

[0018] According to the steps and reaction conditions described in Example 1, the Ag / Cab-O-Sil catalyst with a loading capacity of 40 wt% was selected, the reaction conversion rate was 95.0%, and the selectivity was 88.0%.

Embodiment 3

[0020] According to the steps and conditions described in Example 1, the reaction temperature was 260° C., the flow rate of ethyl lactate was 0.4 g / hour, the reaction conversion rate was 81.4%, and the selectivity was 92.7%.

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Abstract

The invention discloses a method for preparing ethyl pyruvate by gas-phase catalytic oxidation of ethyl lactate, which comprises reacting the mixed gas of ethyl lactate steam and air at 250-300 DEG C in the presence of a silver catalyst supported on silica gel to generate ethyl pyruvate. The method catalyst of the invention is easy to prepare, has high activity and selectivity, and the single-pass conversion rate is as high as 80% or more, and the selectivity is as high as 90% or more.

Description

1. Technical field [0001] The invention relates to the catalytic oxidation of ethyl lactate, in particular to the gas-solid heterogeneous catalytic oxidation of ethyl lactate to prepare ethyl pyruvate. 2. Technical Background [0002] Pyruvate is a precursor for the synthesis of L-amino acids [see H.Yamada and H.Kumagai, Pure and Applied Chemistry: IUPAC Bulletin, vol.50, 1989, p.117 and S.Takao et al., J.Ferment.Tech., 62 (1984)329], can also be used as a raw material for the synthesis of cyanoacrylate adhesives. It is also used as a solvent for photoresists in the electronics industry [see Japan Kokai, H4-36752, February6, 1992]. The current production process is the tartaric acid dehydration and decarboxylation method reported in 1881. This method requires an excessive amount of potassium bisulfate as a dehydrating agent, and the yield is about 60%. The price of the main material and the consumption of auxiliary materials are all high, and it can only be intermittent pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/313C07C69/716
Inventor 沈俭一季伟捷韩毓旺陈懿
Owner NANJING UNIV
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