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Heterogeneous catalytic distillation process for preparing propionate by ester exchange

A heterogeneous catalysis and propionate technology, which is used in the preparation of mutual reaction between ester groups, chemical industry, sustainable manufacturing/processing, etc. , harsh temperature requirements, etc., to achieve the effect of short reaction time, short reaction path and mild reaction conditions

Inactive Publication Date: 2019-05-10
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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  • Heterogeneous catalytic distillation process for preparing propionate by ester exchange
  • Heterogeneous catalytic distillation process for preparing propionate by ester exchange
  • Heterogeneous catalytic distillation process for preparing propionate by 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] Catalyst 7%NiO-13%Co 2 o 3 The amount of / Li-Y is 0.3-5% of the total mass 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] T2 rectification tower: tower diameter 3000mm; tower height 40000mm; the number of trays in the public ...

Embodiment 2

[0053] Under the operating conditions of Example 1, when the total mass flow rate of raw materials is 5000kg / h, changing the molar ratio of raw materials in the T1 rectification tower, the changes in the mass fractions of the components at the top of the tower are shown in Table 2.

[0054] Table 2 The influence of different molar ratios of raw materials on the mass fraction of each component at the top of the T1 distillation column

[0055]

[0056] As can be seen from Table 2, with the increase of the raw material molar ratio, the mass fraction of methyl acetate and methyl propionate at the top of the tower first increases and then decreases, and the mass fraction of propyl acetate increases gradually. When propyl acetate and propionic acid The best raw material ratio is when the molar ratio of methyl ester is 1:3.

Embodiment 3

[0058] 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 1:3, the mass fraction of each component at the top of the tower changes when the reflux ratio of the T1 rectification column is changed. as shown in Table 3.

[0059] Table 3 Effects of different reflux ratios on the mass fraction of each component at the top of the T1 distillation column

[0060]

[0061]

[0062] 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 tends to a steady state, and the content of methyl propionate, propyl propionate and propyl acetate decreases, and the increase of visible reflux ratio contributes to More light methyl acetate at the top of the tower returns to the tower to participate in the reaction again to increase the conversion rate of reactants, but when the reflux ratio is 2:1, the product...

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Abstract

The invention discloses a catalytic rectification process which takes heterogeneous solid base as a catalyst to catalyze methyl propionate and reaction raw material esters such as ethyl formate, propyl formate, butyl formate, ethyl acetate, n-propyl acetate, butyl acetate and the like to synthesize propionate with high added value and high purity in one step. The advantage of the process is that the boiling point of a general product methyl propionate is the lowest, and a reaction system is separated from the top of a reaction rectification tower to push the reaction forward, resulting in a more complete reaction of the reaction raw materials except the methyl propionate. The solid base catalyst is adopted, so that the catalytic efficiency is high, the stability is good, and the liquid phase product and the solid phase catalyst do not need to be separated. In addition, the raw material esters and the product esters generally have no azeotropy and are easy to separate, which is of greatsignificance for large-scale and low-cost production of propionic acid esters with high added value and high purity. The whole reaction process is green, energy-saving, environment-friendly and efficient.

Description

technical field [0001] In the technical field of chemical synthesis of the present invention, specifically, methyl propionate and reaction raw material ester are used as raw materials, and basic materials such as soluble alkali, ionic liquid, and solid alkali are used as catalysts to realize continuous production of high added value and high purity propionic acid Ester process. 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. These 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 temperature performance of lithium-ion batteries has a certain influence. Adding a certain amount of e...

Claims

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Application Information

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IPC IPC(8): C07C67/02C07C69/24
CPCY02P20/10
Inventor 郭建军李新
Owner SHANDONG SHIDA SHENGHUA CHEM GROUP
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