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Transcritical CO2-catalyzed esterification/condensation-separation coupled reaction method and its equipment

A technology of catalytic condensation and coupling reaction, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of product catalyst pollution, low product conversion rate, poor product quality, etc., to improve reaction The effect of speed and balance conversion rate, improving thermal efficiency and reducing exergy loss

Active Publication Date: 2019-03-08
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the above-mentioned prior art, the catalysts used in the process of preparing esters / carbonylation products are mostly metal catalysts. When using this type of catalyst, if the preparation is food-based esters / carbonylation products, the product is easily catalyzed by the catalyst. Pollution, resulting in poor product quality
At the same time, the traditional method for preparing esters / carbonyl products has a relatively complicated process and low product conversion rate

Method used

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  • Transcritical CO2-catalyzed esterification/condensation-separation coupled reaction method and its equipment
  • Transcritical CO2-catalyzed esterification/condensation-separation coupled reaction method and its equipment
  • Transcritical CO2-catalyzed esterification/condensation-separation coupled reaction method and its equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] as attached Figure 1-4 As shown, the device for catalyzing esterification / condensation-separation coupled method for preparing rosin ester includes: dissolution kettle 1, esterification / condensation reactor 2, expander 3, gas-liquid separator 4, turbine compressor 5, Alcohol separation tower 6, reflux pump 7.

[0045] The discharge port of the dissolving tank 1 is connected with the feed port of the esterification / condensation reactor 2, and the dissolving tank 1 is used for dissolving raw materials required for production. The esterification / condensation reactor 2 is cylindrical. The upper part of the esterification / condensation reactor is provided with a feed port 21, a gas outlet 22, and the bottom is provided with a discharge port 23. The esterification / condensation reactor 2 includes a heating pipe 24 , is a heating coil, which is located inside the esterification / condensation reactor; a gas distributor 25, which includes an air inlet 251 and a plurality of nozzl...

Embodiment 2

[0051] The reaction apparatus used is the same as in Example 1, a transcritical CO 2 Catalyzed esterification / condensation-separation coupling reaction:

[0052] Add ethylene glycol and cyclohexanone into the melting tank 1 in a molar ratio of 1:0.9, then add 50% turpentine with a mass fraction of ethylene glycol and cyclohexanone, heat and melt to form a mixed material, and feed CO 2 Press the material into the esterification / condensation reactor 2, then raise the temperature to 100°C under stirring, and continuously feed CO 2 To esterification / condensation reactor 2 internal pressure is 5.0Mpa, fill with CO 2 The flow rate is 100m 3 / h, then open the esterification / condensation reactor 2 gas outlet valves to make the small molecule by-product steam, CO produced in the esterification / condensation reaction process 2 The mixed gas phase material flows out continuously, and the outflow volume is less than or equal to 22000m 3 / h, pressure ≤ 20.0MPa, enter gas-liquid separato...

Embodiment 3

[0054] The reaction apparatus used is the same as in Example 1, a transcritical CO 2 Catalyzed esterification / condensation-separation coupling reaction:

[0055] Anhydrous methanol and citral are added into the melting tank 1 at a molar ratio of 1:0.85, and then 10% of the mass fraction of anhydrous methanol and citral is added 2 , heating, melting, forming a mixed material, passing CO 2 Press the material into the esterification / condensation reactor 2, then raise the temperature to 80°C under stirring, and continuously feed CO 2 To the pressure in the esterification / condensation reactor 2 is 8.0Mpa, filled with CO 2 The flow rate is 100m 3 / h, then open the esterification / condensation reactor 2 gas outlet valves to make the small molecule by-product steam, CO produced in the esterification / condensation reaction process 2 The mixed gas phase material flows out continuously, and the outflow volume is less than or equal to 22000m 3 / h, pressure ≤ 20.0MPa, enter gas-liquid s...

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Abstract

The invention discloses a transcritical CO2 catalytic esterification / condensation-separation coupling reaction method. The method comprises the following steps: mixing alcohol compounds, acid / aldehyde compounds, and a solvent, dissolving, transferring the solution to a reactor, introducing CO2 into the reactor to carry out reactions; collecting the byproducts in gas phase, converting the gas phase by an expansion machine from a supercritical state into a subcritical state, then introducing the gas phase into a gas-liquid separator, pressurizing the separated CO2 and supplemented CO2 by a turbo-compressor, then introducing the pressurized CO2 into the reactor, carrying out reactions for 0.5 to 10 hours, reducing the pressure in the reactor, and taking out reaction products from the reactor. The equipment used by the provided method comprises an esterification / condensation reactor, which comprises a plurality of heating pipes and a gas distributor. The expansion machine and the turbo-compressor are integrated into one machine, and the turbo-compressor is driven by the recovered expansion work of the reaction system. The provided transcritical CO2 catalytic esterification / condensation-separation coupling reaction method and equipment have the advantages that the technology is convenient, the quality of esters / condensed carbonyl product is high, and the conversion rate is high.

Description

technical field [0001] The invention belongs to the technical field of chemical reaction engineering, in particular to a transcritical CO 2 Catalyzed esterification / condensation-separation coupling reaction method and its equipment. Background technique [0002] Esters / carbonyl products are one of the most important chemical products, especially esters or carbonyl compounds with macromolecular structures. Due to the large steric hindrance of carboxyl groups, the activation energy of esterification / condensation reactions is high, and macromolecular acid alcohols The viscosity of the reaction system is high, which makes the interphase transfer between the reactants difficult. Therefore, it is necessary to use strong acid or acidic metal oxide catalysts and high temperature conditions for the esterification / condensation reaction of alcohols and acids / aldehydes. However, under high temperature conditions, macromolecular acid compounds are prone to decarboxylation side reactions...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07B41/12C07B41/04C07C69/78C07C67/08C07C67/54C07D317/72C07C43/15C07C41/56C07C69/753C07C69/07C07C69/14C07C69/145C07C69/24C07D311/10
CPCY02P20/54
Inventor 陈小鹏梁杰珍王琳琳丁胜芳周丹韦小杰
Owner GUANGXI UNIV
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