Method for synthesizing propionate through ester-ester exchange path

A technology of propionate and transesterification, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. Harsh and other problems, to achieve the effect of multiple times of repeated use, short reaction time, and short reaction path

Inactive Publication Date: 2019-03-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 method 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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  • Method for synthesizing propionate through ester-ester exchange path
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  • Method for synthesizing propionate through ester-ester exchange path

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preparation example Construction

[0028] The preparation methods of several typical catalysts are as follows:

[0029] The imidazole ionic liquid is 1-methyl-3-methylimidazolium bromide, and its preparation method is as follows: use N-methylimidazole and methyl bromide as raw materials to prepare the ionic liquid, and first pour the measured N-methylimidazole into In a 250 mL three-necked flask, heat it in a water bath at 30 °C, then add a metered amount of methyl bromide dropwise to the above solution under stirring, and fill it with N 2 protection, and continued to stir for 12 h to obtain white crystals, which were washed 3 times with 100 mL of ethyl acetate to remove unreacted raw materials. components, and finally vacuum-dried at 70 °C for 24 h to obtain 1-methyl-3-methylimidazolium bromide ionic liquid.

[0030]N-ethylpyridine tetrafluoroborate is selected as the pyridine ionic liquid, and its preparation method is as follows: Measure a certain amount of pyridine 79.1g and bromoethane 174.4g, respectivel...

Embodiment 1

[0043] In a three-necked flask, the influence of different catalysts on the conversion of raw materials was explored. Methyl propionate and methyl acetate were added into a 250 mL three-neck flask, and catalysts such as ionic liquid, soluble strong base, organic base, and solid base were added respectively. The catalyst addition is 3% of the total mass of raw materials. The three-necked flask is connected with a spherical condenser and a thermometer. The reaction temperature is 84°C, the molar ratio of methyl propionate to ethyl acetate is 1:1, and the reaction time is 4 hours. Start stirring, heat the solution to a certain temperature for reaction, take a sample for analysis after 5 minutes of stabilization, inject gas chromatography, the chromatographic analysis conditions are: the temperature of the vaporization chamber is 230 °C, the FID detector is used, the detector temperature is 250 °C, and the chromatographic column is HP-FFAP , the stationary phase is modified poly...

Embodiment 2

[0048] In a three-necked flask, the influence of different reaction raw materials on the conversion rate of raw materials was explored. The catalyst is 7%NiO-13%Co2O3 / Li-Y as an example, and different esters of raw materials are added to a 250 mL three-necked flask, and the amount of 7%NiO-13%Co2O3 / Li-Y is 3% of the total mass of raw materials . The three-necked flask is connected with a spherical condenser and a thermometer. The reaction temperature is 84°C, the molar ratio of raw materials is 1:1, and the reaction time is 4 hours. Stirring was started, the solution was heated to react, and after being stable for 5 minutes, samples of different reaction raw materials were respectively taken for chromatographic analysis and calculation. The raw material conversion rate is shown in Table 2.

[0049] Table 2 Effect of different reaction raw materials on the conversion rate of raw materials

[0050]

[0051] As can be seen from Table 2, when the reaction raw material is a ...

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Abstract

The invention provides a method for synthesizing propionate through an ester-ester exchange path and relates to a method for synthesizing the propionate. According to the method, reaction raw materials include, but are not limited to ethyl formate, propyl formate, butyl formate, ethyl acetate, propyl acetate, butyl acetate and the like; the method for synthesizing the propionate through an ester exchange one-step method is adopted. A catalyst comprises alkaline materials including ionic liquid, soluble strong base, solid base and the like respectively; the catalyst has the advantages of high catalysis efficiency and no pollution. By taking methyl propionate and ethyl acetate reaction as an example, KOH is used as the catalyst, the mol ratio of the raw materials is 1 to 1, the reaction temperature is 60 DEG C and the reaction time is 5 min; the conversion ratios of the methyl propionate and the ethyl acetate can reach 70 percent or more; products comprise ethyl propionate and the methylacetate. The whole reaction path has the characteristics of short synthetic route, simple technological flow and high yield and the catalyst is stable, does not become inactive and can be repeatedlyutilized.

Description

technical field [0001] The invention relates to a method for synthesizing propionate, in particular to a method for synthesizing propionate through an ester exchange route. 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 propionate on LiFePO 4 The low temperature performance of lithium-ion batteries has a certain influence. Adding a certain amount of propionate can increase the ionic conductivity of the carbonate electrolyte and improve the relationship between the electrolyte and the positive electrode LiFePO. 4 The compatibility of the material and the negative electrode graphite material reduces the visco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/24C07C67/02C07C67/54
CPCC07C67/02C07C67/54C07C69/24
Inventor 石磊刘铭钰叶青张冬喜
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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