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Method for preparing ethyl alcohol by hydrogenation of acetate

A technology of acetate and methyl acetate, which is applied in the field of hydrogenation of acetate to prepare ethanol, can solve the problems of no catalyst preparation method and reduced hydrogenation activity, and achieve the avoidance of separation and purification, promotion of hydrogenation reaction, and preparation process simple effect

Active Publication Date: 2017-03-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the hydrogenation activity of the Cu-Zn catalyst is significantly reduced in the atmosphere containing CO in the feed gas.
However, the catalysts in the patent are all commercial catalysts, and the preparation method of the catalyst is not given

Method used

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  • Method for preparing ethyl alcohol by hydrogenation of acetate
  • Method for preparing ethyl alcohol by hydrogenation of acetate
  • Method for preparing ethyl alcohol by hydrogenation of acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Dissolve 6.8g of crystalline copper nitrate and 57ml of water in a three-necked flask, stir evenly at room temperature, and then drop in 20% NaOH aqueous solution until pH=12 to form a slurry.

[0039] 4.18g SiO 2 Add the powder to the above slurry, stir evenly, then heat up to 80-90°C, age for 4 hours, filter, and wash. Dry at 120°C for 12h, and bake at 450°C for 3h. Obtain the CuO whose Cu oxide mass accounts for 35wt% of the total mass of the catalyst x / SiO 2 Catalyst, abbreviated as 35Cu / SiO 2 .

Embodiment 2

[0041] 1.37g manganese nitrate aqueous solution (manganese nitrate mass percentage composition 50%) is dissolved in the beaker with 25ml water, adds 4g SiO 2 Stir the powder evenly, and when the solution is volatilized and nearly dry, transfer it to an oven for 12 hours at 120°C to obtain MnO y / SiO 2 sample.

[0042] Dissolve 6.8g of crystalline copper nitrate and 57ml of water in a three-necked flask, stir evenly at room temperature, and then drop in 20% NaOH aqueous solution until pH=12 to form a slurry.

[0043] 4.18 g of MnO prepared above y / SiO 2 Add the powder to the above slurry, stir evenly, then heat up to 80-90°C, age for 4 hours, filter, and wash. Dry at 120°C for 12h, and bake at 450°C for 3h to obtain CuO x -MnO y / SiO 2 catalyst. Wherein the Cu oxide mass accounts for 35wt% of the total mass of the catalyst, and the additive manganese oxide MnO y The mass accounts for 5wt% of the total mass of the catalyst, abbreviated as 35Cu-5Mn / SiO 2 .

Embodiment 3

[0045] 1.05g crystalline zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) dissolve in the beaker with 20ml water, add 4g SiO 2 Stir the powder evenly, and when the solution is volatilized and nearly dry, transfer it to an oven and bake at 120°C for 12 hours to obtain ZnO y / SiO 2 sample.

[0046] Dissolve 6.8g of crystalline copper nitrate and 57ml of water in a three-necked flask, stir evenly at room temperature, and then drop in 20% NaOH aqueous solution until pH=12 to form a slurry.

[0047] 4.3 g ZnO prepared above y / SiO 2 Add the powder to the above slurry, stir evenly, then heat up to 80-90°C, age for 4 hours, filter, and wash. Dry at 120°C for 12h, and bake at 450°C for 3h to obtain CuO x -ZnO y / SiO 2 catalyst. Among them, the mass of Cu oxide accounts for 35wt% of the total mass of the catalyst, and the mass of zinc oxide as an auxiliary agent accounts for 4wt% of the total mass of the catalyst, which is abbreviated as 35Cu-4Zn / SiO 2 .

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Abstract

The invention provides a method for preparing ethyl alcohol from acetate. The method includes the following steps: heating and vaporizing acetate, and under the condition of a catalyst and in a mixed gas atmosphere of CO and H2, introducing or not introducing inert gases to react for preparing the ethyl alcohol; the catalyst is Cu-M / SiO2, wherein Cu is used as an active component and accounts for 10-85 wt% of the total amount of the catalyst based on the calculation of copper oxides; M is used as an adjuvant, accounts for 0.1-20 wt% of the total amount of the catalyst based on the calculation of oxides of M, and refers to one or more of Mn, Zn, Fe, Co and Ni; the mass ratio of SiO2 in the catalyst is 10-89.9 wt%. The catalyst is used for preparing the ethyl alcohol by hydrogenation of acetate in the atmosphere of CO-containing H2 (syngas), CO and H2 in a feed gas have a synergistic effect with the catalyst, the activity of a hydrogenation reaction is improved, and the yield of the reaction product is increased significantly.

Description

technical field [0001] The present invention relates to the technical field of preparing ethanol by hydrogenation of acetate, especially the reaction atmosphere of the reaction includes CO gas, wherein a catalyst used in the reaction is also provided, in which CO can promote the preparation of hydrogenation of acetate Reactivity of ethanol. Background technique [0002] Ethanol is a widely used basic chemical raw material, and can also be used as automobile fuel and additive. Traditional ethanol production is mainly achieved by grain fermentation or ethylene hydration from the petroleum route. [0003] In recent years, ethanol production from syngas via methanol or dimethyl ether has attracted people's attention. Synthesis gas is carbonylated with methanol or dimethyl ether to obtain acetic acid (acetate), which is further hydrogenated to produce ethanol. Moreover, the technology of producing acetic acid by carbonylation of methanol is mature, and ethanol can be obtained ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/08C07C29/149B01J23/72B01J23/889B01J23/80
CPCB01J23/002B01J23/72B01J23/80B01J23/8892B01J2523/00C07C29/149C07C31/08B01J2523/17B01J2523/72B01J2523/41B01J2523/27
Inventor 黄秀敏申文杰马猛薛会福
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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