Homogeneous-phase catalytic rectification process for preparing propionic ester through ester-ester exchange

A homogeneous catalysis and propionate technology, which is applied in the preparation of carboxylate, the preparation of mutual reaction between ester groups, and the chemical industry, etc. Strict requirements and other problems, to achieve the effect of stable catalyst performance without deactivation, low cost and easy separation

Inactive Publication Date: 2019-05-21
SHANDONG SHIDA SHENGHUA CHEM GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The optimal reaction temperature of this method is 32-36°C, and the temperature requirements are relatively strict, so it is not ideal to use alkaline lipase to catalyze the synthesis of ethyl propionate
Propionate is prepared by esterification and carbonylation, there will be by-products, and there are alcohols in the product. Lithium-grade propionate requires high purity and no other trace impurities. Therefore, through esterification and carbonylation It is not ideal to obtain ethyl propionate to improve the low-temperature performance of lithium-ion battery electrolyte. It is of great significance to open up a new reaction route and process for large-scale preparation of high-purity propionate
[0006] There are a large number of reports on transesterification reactions in China, such as the transesterification of propylene carbonate and methanol to prepare dimethyl carbonate, the transesterification of dimethyl carbonate and ethanol to prepare ethyl methyl carbonate, etc., but the report on the synthesis of propionate by transesterification hardly

Method used

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  • Homogeneous-phase catalytic rectification process for preparing propionic ester through ester-ester exchange
  • Homogeneous-phase catalytic rectification process for preparing propionic ester through ester-ester exchange
  • Homogeneous-phase catalytic rectification process for preparing propionic ester through ester-ester exchange

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Using methyl propionate and propyl acetate as raw materials, the ratio of propyl propionate to methyl acetate is 1:1, and the excess methyl propionate is recycled.

[0042] The dosage of the catalyst KOH is 0.3-5wt% of the total mass sum of the raw materials, and the ratio of the cross-sectional area of ​​the initial distillation section to the side line section is 1:1.

[0043] The operating conditions are as follows:

[0044] Distillation tower T1: tower diameter 1000mm; tower height 19000mm; the number of plates in the public rectification section, initial distillation section, side line section, and public stripping section are 10, 20, 30, and 15 respectively; the pressure inside the tower is 1 MPa; The temperature is 60°C; the bottom temperature of the common stripping section is 71°C; the bottom temperature of the side line section is 74°C.

[0045] Distillation tower T2: tower diameter 3000mm; tower height 40000mm; the number of trays in the public rectification...

Embodiment 2

[0052] Under the operating conditions of Example 1, when the total mass flow rate of raw materials is 5000kg / h, changing the molar ratio of the raw materials in the first reactive distillation column of T1, the changes in the mass fractions of the components at the top of the tower are shown in Table 2.

[0053] Table 2 Effect of different molar ratios of raw materials on the mass fraction of each component at the top of the first reactive distillation column of T1

[0054]

[0055] It can be seen from Table 2 that with the increase of the molar ratio of raw materials, the mass fraction of methyl acetate at the top of the tower gradually decreases, and the mass fraction of ethyl propyl ester gradually increases. When the molar ratio of propyl acetate and methyl propionate is 1:2 is the best raw material ratio.

Embodiment 3

[0057] Under the operating conditions of Example 2, the total raw material mass flow rate is 5000kg / h, and when the molar ratio of propyl acetate and methyl propionate is 1:2, the reflux ratio of the first reactive distillation column of T1 is changed, and the components at the top of the column The quality fraction changes are shown in Table 3.

[0058] Table 3 Effects of different reflux ratios on the mass fraction of each component at the top of the first reactive distillation column of T1

[0059]

[0060]

[0061] As can be seen from Table 3, along with the increase of reflux ratio, the mass fraction of methyl acetate at the top of the tower increases gradually, and the content of methyl propionate, propyl propionate and propyl acetate decreases, and the increase of visible reflux ratio contributes to more The methyl acetate, the light component at the top of the tower, returns to the tower to participate in the reaction again to increase the conversion rate of the ...

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Abstract

The invention provides a catalytic rectification process which takes homogeneous-phase soluble alkali or ionic liquid as a catalyst to catalyze methyl propionate and various esters such as ethyl formate, propyl formate, butyl formate, ethyl acetate, propyl acetate and butyl acetate to synthesize propionic ester with high added value and high purity in one step. The process has the advantages of simple reaction system and short reaction path; a product is high in selectivity and purity and generates no by-products absolutely. The reaction time is short, the activity of the catalyst is high, andthe catalyst can be repeatedly used. Azeotropy between raw material esters and a product ester does no happens generally, separation is easy, and the process has great significance in large-scale andlow-cost production of the propionic ester with high added value and high purity. The whole reaction process is environmentally friendly, capable of saving energy and efficient.

Description

technical field [0001] The technical field of chemical synthesis of the present invention is specifically based on methyl propionate and reaction raw material ester (including but not limited to ethyl formate, propyl formate, butyl formate, ethyl acetate, propyl acetate, butyl acetate, etc.) As the raw material, the ionic liquid of homogeneous soluble alkali is used as the catalyst to realize the process of continuous production of high value-added and high-purity propionate. Background technique [0002] Propionate can be applied to cellulose esters and ethers, solvents for various natural or synthetic resins; as a spice, it can be used to blend apple, banana, plum, pineapple, and as butter, western wine and other foods essence. It can also be used as a fragrance for advanced daily cosmetics. Such products are also used as intermediates in organic synthesis. Studies have shown that ethyl propionate and propyl propionate have a significant effect on LiFePO 4 The low temp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/02C07C67/54C07C69/24C07C69/14
CPCY02P20/10
Inventor 郭建军李新
Owner SHANDONG SHIDA SHENGHUA CHEM GROUP
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