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Method for synthesizing 2-ethyl-2-hexenal

A technology of hexenal and ethyl hexanol, which is applied in the field of synthesizing 2-ethyl-2-hexenal, can solve the problems of increasing energy consumption and material consumption, reducing the concentration of butyraldehyde in the liquid phase, disadvantages, etc.

Active Publication Date: 2014-06-18
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The liquid phase condensation reaction is carried out under normal pressure, and a large amount of butyraldehyde is gasified, which reduces the concentration of butyraldehyde in the liquid phase, which is not conducive to the reaction; the gasification, condensation process and solvent recovery of butyraldehyde increase energy consumption and material consumption; Using a tank reactor, the reacted catalyst needs to be filtered and separated, which is not conducive to large-scale industrial continuous production

Method used

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  • Method for synthesizing 2-ethyl-2-hexenal
  • Method for synthesizing 2-ethyl-2-hexenal

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Experimental program
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Effect test

Embodiment 1

[0020] 10g of MgO / Al with a Mg / Al ratio of 1.25 was loaded into the fixed bed reactor 2 o 3 The solid base catalyst is replaced by nitrogen gas, the reaction temperature is set at 80°C, and the solvent 2-ethylhexanol is added to completely wet the catalyst. Under the conditions of butyraldehyde feed rate of 10 g / h, mass ratio of 2-ethylhexanol to butyraldehyde of 0.1, and reaction pressure of 0.1 MPa, butyraldehyde was condensed and dehydrated to generate 2-ethyl-2-hexenal. The reaction product was distilled at 0.1MPa and 100°C. The butyraldehyde extracted from the top of the tower is returned to the raw material inlet, and after the extraction from the tower kettle is chromatographically separated to separate the water phase, the organic phase is analyzed by gas chromatography. The reaction was carried out for 48 hours, the single-pass conversion rate of butyraldehyde was 63.51%, and the overall yield of 2-ethyl-2-hexenal was 95.71%. After the reaction, the catalyst Mg / Al ...

Embodiment 2

[0022] 10g of MgO / Al with a Mg / Al ratio of 1.25 was loaded into the fixed bed reactor 2 o 3 The solid base catalyst is replaced by nitrogen gas, the reaction temperature is set at 120° C., and the solvent 2-ethylhexanol is added to completely wet the catalyst. Under the conditions of butyraldehyde feed rate of 10 g / h, mass ratio of 2-ethylhexanol to butyraldehyde of 1, and reaction pressure of 0.2 MPa, butyraldehyde was condensed and dehydrated to generate 2-ethyl-2-hexenal. The reaction product was distilled at 0.15MPa and 110°C. The butyraldehyde extracted from the top of the tower is returned to the raw material inlet, and after the extraction from the tower kettle is chromatographically separated to separate the water phase, the organic phase is analyzed by gas chromatography. The reaction was carried out for 48 hours, the single-pass conversion rate of butyraldehyde was 80.03%, and the overall yield of 2-ethyl-2-hexenal was 96.26%. After the reaction, the catalyst Mg / A...

Embodiment 3

[0024] 10g of MgO / Al with a Mg / Al ratio of 1.25 was loaded into the fixed bed reactor 2 o 3 The solid base catalyst is replaced by nitrogen gas, the reaction temperature is set at 120° C., and the solvent 2-ethylhexanol is added to completely wet the catalyst. Under the conditions of butyraldehyde feed rate of 10g / h, mass ratio of 2-ethylhexanol to butyraldehyde of 3, and reaction pressure of 0.2MPa, butyraldehyde was condensed and dehydrated to generate 2-ethyl-2-hexenal. The reaction product was distilled at 0.12MPa and 110°C. The butyraldehyde extracted from the top of the tower is returned to the raw material inlet, and after the extraction from the tower kettle is chromatographically separated to separate the water phase, the organic phase is analyzed by gas chromatography. The reaction was carried out for 48 hours, the single-pass conversion rate of butyraldehyde was 75.74%, and the overall yield of 2-ethyl-2-hexenal was 96.45%. After the reaction, the catalyst Mg / Al ...

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Abstract

The present invention relates to a method for synthesizing 2-ethyl-2-hexenal. The method comprises that: 2-ethyl hexanol and butyraldehyde are mixed according to a mass ratio of 0.1-10; a condensation dehydration reaction is performed at a temperature of 80-220 DEG C under pressure of 0.1-1.0 MPa under an effect of a solid base to obtain a single-phase mixture of 2-ethyl-2-hexenal, 2-ethyl hexanol and water; the reactant is distilled at a temperature of 100-110 DEG C under pressure of 0.1-0.15 MPa, the unreacted butyraldehyde circularly returns to the condensation reactor, and an organic phase and aqueous phase two-phase mixture of 2-ethyl-2-hexenal and 2-ethyl hexanol is extracted; and the organic phase and aqueous phase two-phase mixture is subjected to condensation and chromatography separation to obtain a 2-ethyl-2-hexenal and 2-ethyl hexanol mixture. With the method, the 2-ethyl-2-hexenal yield achieves 96%, the loss of the catalyst active ingredient is less, no basic organic wastewater is generated, and the solvent is not required to be separated and recovered.

Description

technical field [0001] The invention relates to a method for synthesizing 2-ethyl-2-hexenal, in particular to a method using a fixed-bed reactor, using solid alkali as a catalyst, and 2-ethylhexanol as a solvent to condense butyraldehyde A method for synthesizing 2-ethyl-2-hexenal by dehydration reaction. Background technique [0002] 2-Ethyl-2-hexenal is an intermediate in the synthesis of 2-ethylhexanol, which is mainly used in the manufacture of dioctyl phthalate and dioctyl terephthalate, and is also used in diesel additives, Synthetic lubricants, antioxidants, solvents, and defoamers are important basic organic chemical raw materials and chemical auxiliary raw materials. 2-Ethyl-2-hexenal is prepared by condensation and dehydration of butyraldehyde. [0003] US 5,055,620 describes an aldol condensation reaction process. MgO-Al 2 o 3 As a catalyst, butyraldehyde is condensed in gas phase to generate 2-ethyl-2-hexenal. ZL 99813760.X and ZL 01809710.3 disclose proces...

Claims

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Application Information

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IPC IPC(8): C07C45/74C07C47/21
CPCC07C45/74C07C47/21
Inventor 崔龙李正赵胤穆庆峰姚剑山陶文晶田艳明周玮邓广金宋长华
Owner PETROCHINA CO LTD
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