Catalyst for synthesizing ethyl ethoxyacetate through hydrogenation of diethyl oxalate and preparation method and application of catalyst

A technology of ethyl ethoxyacetate and diethyl oxalate, which is applied to the catalyst for synthesizing ethyl ethoxyacetate by gas-phase hydrogenation of diethyl oxalate and the field of preparation thereof, and can solve the problem of overcapacity, single product, and limited development and industrialization. To achieve the effect of sufficient raw materials, simple preparation method and high selectivity

Active Publication Date: 2016-08-17
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

CN101700496A discloses a kind of Al 2 o 3 Supported Cu-based catalyst, but the main product is glycolate, and the catalyst needs to add precious metal component Ag
Although the copper-based catalysts prepared in this series of studies have high activity and selectivity, the product is single and easily leads to overcapacity of related products, which limits the development of coal and biomass conversion into other fine chemicals and related technologies. promotion of industrialization
More importantly, up to now, there is no literature report on the catalyst for the synthesis of ethyl ethoxy acetate by gas phase hydrogenation of diethyl oxalate.

Method used

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  • Catalyst for synthesizing ethyl ethoxyacetate through hydrogenation of diethyl oxalate and preparation method and application of catalyst

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Experimental program
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Effect test

Embodiment 1

[0020] A method for preparing a catalyst for hydrogenating diethyl oxalate to synthesize ethyl ethoxy acetate, comprising the steps of: (1) uniformly mixing 0.223 g copper acetate and 3.422 g aluminum sulfate; (2) mixing copper ions and aluminum ions The total amount of ions and the molar coordination ratio of oxalic acid are calculated as 1:1.6. Add 4.41 g of oxalic acid to the mixed metal salt in the above step (1) and stir vigorously at room temperature for 6 h; (3) the obtained product in step (2) Move in 50 o C for 8 h, then at 100 o Dry at C for 5 h to obtain the catalyst precursor powder; raise the powder sample prepared in step (3) to 400 °C in air o Calcined at C for 10 h, heating rate 1 o C / min, that is, CuO / Al with a mass content of 5.0 wt% of copper oxide 2 o 3 Diethyl oxalate hydrogenation catalyst.

[0021] The above CuO / Al 2 o 3 1 mL of catalyst was filled in a fixed-bed tubular reactor. The catalyst was heated at a volumetric space velocity of 1800 h -...

Embodiment 2

[0023] A method for preparing a catalyst for hydrogenating diethyl oxalate to synthesize ethyl ethoxy acetate, comprising the following steps: (1) uniformly mixing 0.798 g copper sulfate and 5.009 g aluminum nitrate; (2) mixing copper ions and aluminum ions The total amount of ions and the molar coordination ratio of citric acid were calculated as 1:1.9, and 11.242 g of citric acid was quickly added to the mixed metal salt in the above step (1) and stirred vigorously at room temperature for 3 h; (3) the step (2 ) proceeds into 30 o C for 10 h, then at 80 o C and dried for 8 h to obtain the catalyst precursor powder; (4) heat the powder sample prepared in step (3) to 800 °C in air o Calcined at C for 1 h, heating rate 1 o C / min, that is, CuO / Al with a mass content of 25.0 wt% of copper oxide 2 o 3 Diethyl oxalate hydrogenation catalyst.

[0024] The above CuO / Al 2 o 3 1 mL of catalyst was filled in a fixed-bed tubular reactor. The catalyst was subjected to a volumetric ...

Embodiment 3

[0026]A method for preparing a catalyst for hydrogenating diethyl oxalate to synthesize ethyl ethoxy acetate, comprising the following steps: (1) uniformly mixing 1.876 g copper nitrate and 5.115 g aluminum nitrate; (2) mixing copper ions and aluminum ions The molar coordination ratio of the total amount of ions and tartaric acid is 1:1, and 6.904 g of tartaric acid is quickly added to the mixed metal salt in the above step (1) and vigorously stirred at room temperature for 4 h; (3) the obtained Item moved into 50 o C for 6 h, then at 70 o C for 10 h to obtain catalyst precursor powder; (4) heat the powder sample prepared in step (3) to 700 °C in air o C calcined for 2 h, heating rate 15 o C / min, that is, CuO / Al with a mass content of 40.0 wt% of copper oxide 2 o 3 Diethyl oxalate hydrogenation catalyst.

[0027] The above CuO / Al 2 o 3 1 mL of catalyst was filled in a fixed-bed tubular reactor. The catalyst was subjected to a volumetric space velocity of 3600 h -1 , 0...

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Abstract

A catalyst for synthesizing ethyl ethoxyacetate through hydrogenation of diethyl oxalate is prepared from, by mass, 2.0-65.0wt% of CuO serving as a main active component and 3.5-98.0wt% of Al2O3 serving as a carrier. The catalyst for synthesizing ethyl ethoxyacetate through hydrogenation of diethyl oxalate has the advantages of being high in selectivity, good in stability and suitable for industrial production.

Description

technical field [0001] The invention belongs to a catalyst and its preparation method and application, in particular to a catalyst for synthesizing ethyl ethoxy acetate by gas-phase hydrogenation of diethyl oxalate and its preparation method and application. Background technique [0002] Ethoxyethyl acetate is soluble in water, easily soluble in ethanol and ether, and miscible in most organic solvents such as aromatic hydrocarbons. As a universal solvent, it has a strong dissolving power, especially for polymer polymers. , with the properties of aliphatic ethers and acetates. It is mainly used as a solvent for metal and furniture spraying paint, as a solvent for brushing paint, as a solvent for protective paint, dyes, resins, leather, inks, and in the formulation of hard surface cleaners such as metals and glass. As chemical reagents or organic synthesis intermediates. Therefore, the market demand for ethyl ethoxy acetate is relatively large. [0003] The traditional prep...

Claims

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Application Information

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IPC IPC(8): B01J23/72C07C67/31C07C69/708C07C69/675
CPCB01J23/72B01J37/086C07C67/31C07C69/708C07C69/675
Inventor 陈建刚丁健刘艳廷张娟陈政王补欢陈敏
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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