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

A gas-phase catalytic oxidation and ethyl pyruvate technology, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of sharp drop in selectivity and unsatisfactory conditions, and achieve low raw material costs and high production efficiency. The effect of being easy and the preparation method is simple

Inactive Publication Date: 2002-07-24
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 of 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 an 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 for 5 hours at 350°C for 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 20-40 mesh 20wt% Ag / Cab-O-Sil. Before the reaction, be warming up to 350 ℃ and reduce with hydrogen for 1 hour, switch to the mixed gas of air and ethyl lactate when cooling to 300 ℃, ethyl lactate flow rate is 0.6 g / hour, air: ethyl lactate=15: 1. The reaction mixture over the catalyst was analyzed online by gas chromatography (15% PEG6000 / GDX103 column). Steady state was reached after 4 hours...

Embodiment 2

[0018] According to the steps and conditions described in Example 1, the Ag / Cab-O-Sil catalyst with a loading 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

A process for preparing ethyl pyruvate is characterized by that the reaction of the mixture of ethyl lactate vapour and air at 250-300 deg.C in the presence of silica gel carried silver catalyst. Its advantages are high conversion (80%) and selectivity (90%), and high activity and selectivity of catalyst.

Description

1. Technical field [0001] The invention relates to the catalytic oxidation of ethyl lactate, in particular to the 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], it can also be used as a raw material for the synthesis of nitrile acrylate adhesives. It is also used as a solvent for photoresist materials in the electronics industry [see Japan Kokai, H4-36752, Feburary 6, 1992]. The current production technique is the tartaric acid dehydration and decarboxylation method reported in 1881. This method requires excessive potassium hydrogen sulfate as a dehydrating agent, and the yield is about 60%. production. [0003] In the early 1980s, there were patent reports that pyruvic acid was obtained by the oxidat...

Claims

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Application Information

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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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