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Method for generating low-carbon ester by condensation of low-carbon aldehyde

A low-carbon ester and aldehyde condensation technology is applied in the field of acetylacetone-based metal salt as a catalyst to catalyze the low-carbon aldehyde condensation to prepare a low-carbon ester. Low cost, lower reaction cost, and less inactivation effect

Inactive Publication Date: 2019-09-27
RUNTAI CHEM TAIXING CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the shortcomings of existing catalysts for the condensation of low-carbon aldehydes to generate low-carbon esters. The present invention provides a new method for the condensation of low-carbon aldehydes to generate low-carbon esters. Activity and other disadvantages, and the amount of catalyst is small, can be reused, the yield is high, basically no waste water is generated in the production, and the green synthesis process can be realized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Mix 10.0g of raw material isobutyraldehyde, 10.0ml of solvent isobutanol and 0.50g of catalyst zirconium acetylacetonate into the autoclave, replace with nitrogen three times and fill with N 2 The reaction was carried out at 0.50 MPa, and the temperature was controlled by a temperature controller at 200°C for 6 hours. After the reaction was stopped, the reaction mixture was lowered to room temperature, and the inert gas in the kettle was slowly discharged, opened, and discharged. The supernatant was taken for gas chromatographic analysis, and the calculated raw material conversion rate was 95.27%, and the yield rate was 90.94%. After the reaction, the catalyst is separated by vacuum distillation, and 10.0 g of isobutyraldehyde and 10.0 ml of solvent isobutanol are added to the recovered catalyst for catalytic recycling. The reaction is carried out according to the above reaction conditions, and the product isobutyric acid is recycled. The yield of isobutyl ester was 87....

Embodiment 2

[0026] Mix 10.0g of raw material isobutyraldehyde, 10.0ml of solvent dodecyl alcohol ester and 0.70g of catalyst magnesium acetylacetonate into the autoclave, replace with nitrogen three times and fill with N 2 The reaction is carried out at 0.25MPa, and the reaction temperature is controlled by a temperature controller at 180°C for 10 hours. After the reaction is stopped, the reaction mixture is lowered to room temperature, and the inert gas in the kettle is slowly discharged, the kettle is opened, and the material is discharged. The supernatant was taken for gas chromatography analysis, and the calculated conversion rate was 86.41%, and the yield was 78.08%. After the reaction, the catalyst was separated by vacuum distillation, and 10.0g of isobutyraldehyde and 10.0ml of solvent dodecyl alcohol ester were added to the recovered catalyst for catalytic recycling, and the reaction was carried out according to the above reaction conditions, and the product isobutyraldehyde was ob...

Embodiment 3

[0028] Mix 10.0g of raw material isobutyraldehyde, 10.0ml of solvent toluene and 0.50g of catalyst aluminum acetylacetonate into the autoclave, replace with nitrogen three times and fill with N 2 The reaction was carried out at 0.5 MPa, and the reaction temperature was controlled by a temperature controller at 160°C for 6 hours. After the reaction was stopped, the reaction mixture was lowered to room temperature, and the inert gas in the kettle was slowly discharged, opened, and discharged. The supernatant was taken for gas chromatography analysis, and the calculated conversion rate was 85.27%, and the yield was 73.04%. After the reaction, the catalyst was separated by vacuum distillation, and 10.0g of isobutyraldehyde and 10.0ml of solvent toluene were added to the recovered catalyst for catalytic recycling, and the reaction was carried out according to the above reaction conditions, and the product isobutyric acid isobutyl was recycled. The yield of ester was 68.22%.

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Abstract

The invention relates to a new method for preparing low-carbon ester by condensation of low-carbon aldehyde through catalysis of acetylacetone metal salts. The method is characterized in that the acetylacetone metal salts are taken as a catalyst, the low-carbon ester is prepared by performing a reaction for 2-4 h under the conditions that the mass ratio of aldehyde to the catalyst is (10:1) to (200:1), the mass ratio of the aldehyde to a solvent is (1:1) to (10:1), the reaction temperature is 80 to 250 DEG C, and the reaction pressure of 0.1 to 1.0 MPa, and the catalyst is recovered and recycled. Compared with the prior art, the defects that a traditional catalyst is not easy to separate, is liable to inactivate, cannot be recycled, and the like are solved; the dosage of the catalyst is less, the yield is high, no waste water is generated basically during production, and a green synthesis process can be realized.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and relates to a method for generating low-carbon esters by condensation of low-carbon aldehydes, in particular to an easy-separated and recyclable acetylacetone metal salt as a catalyst to catalyze the condensation of low-carbon aldehydes to prepare low-carbon A new approach to esters. Background technique [0002] Low-carbon esters, as a small molecular organic compound with a simple structure, were first discovered in the fruits, stems and leaves of plants. With the deepening of research, low-carbon esters are more and more widely used in the fields of industry, medicine, agriculture and coatings. They can be used as solvents and extractants in organic reactions and chemical raw materials, and are also used in the synthesis of insecticides, drugs, It is an important raw material for intermediates such as plasticizers. In addition, most low-molecular-weight esters can even b...

Claims

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Application Information

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IPC IPC(8): C07C67/44C07C69/24
CPCC07C67/44C07C69/24Y02P20/584
Inventor 张润赟吕志果宋文国张世元
Owner RUNTAI CHEM TAIXING CO LTD
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