Preparation method for electronic-grade n-propyl propionate

An electronic-grade n-propyl propionate technology, which is applied in the field of preparation of electronic-grade n-propyl propionate, can solve the problems of slow progress in n-propyl propionate research, unrecorded metal ion content, and expensive catalysts, etc., reaching Reduce re-investment costs, facilitate rectification and purification, and facilitate product separation

Inactive Publication Date: 2019-07-05
SHENZHEN ESUN IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The catalyst is also a hydrogen-type styrene-stilbene copolymer with sulfonate groups. The resin pore size is <8nm, which can effectively absorb impurities during the reaction process to improve product purity. High-purity n-propyl propionate obtained through rectification The purity content of the finished product is 99.7%, and the content of metal ions is not recorded, and this type of ion exchange resin catalyst is expensive, and the reaction temperature is too high to easily lose activity, and the resulting finished product is not suitable for lithium battery electrolyte solvents
[0006] There are few domestic reports on research on electronic grade propyl propionate, and the general purity is around 99%. Research on n-propyl propionate, a lithium battery electrolyte solvent that strictly controls the content of metal ions, is progressing slowly

Method used

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  • Preparation method for electronic-grade n-propyl propionate
  • Preparation method for electronic-grade n-propyl propionate
  • Preparation method for electronic-grade n-propyl propionate

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0028] The synthesis of embodiment 1 n-propyl propionate crude product

[0029] 1.1 Catalyst synthesis

[0030] Feed according to the molar ratio of N-methyl-2-pyrrolidone and p-toluenesulfonic acid 1:1~1.5:1, stir and react at 60°C~120°C for 4h, then filter the reaction solution, add ethyl acetate to wash the solid, and The obtained white solid was dried to obtain the ionic liquid [HNMP]PTSA (N-methyl-2-pyrrolidone p-toluenesulfonate). The improved ionic liquid [HNMP] PTSA catalyst is insoluble in propionic acid and propanol at the beginning of the esterification reaction, and starts to dissolve in the reaction liquid after the heating reaction and undergoes a homogeneous reaction. After the reaction is completed, it is cooled to room temperature, and the catalyst Precipitated in solid form. Different from the p-toluenesulfonic acid catalytic esterification process, it is always dissolved in the reaction solution and cannot be recycled, which affects the subsequent sepa...

Embodiment 2

[0041] The preparation of embodiment 2 purity greater than or equal to 99.99 n-propyl propionate

[0042] 2.1 Synthesis of Propyl Propionate Crude Product

[0043] Weigh 740.8g of propionic acid and 901.5g of propanol in a 3L reaction flask, then add 111.12g of ionic liquid [HNMP]PTSA catalyst and 200mL of water-carrying agent cyclohexane, heat and reflux to separate water, take samples for analysis, and test the conversion After the yield reached more than 99%, the reaction was stopped, and after the esterification liquid was cooled to room temperature, the solid (catalyst) was filtered off to obtain the crude product of n-propyl propionate.

[0044] 2.2 Vacuum distillation

[0045]The n-propyl propionate crude product is added in the rectification tower to carry out rectification under vacuum. The height of the rectification tower is 1.3m, and the inner diameter of the tower is 32mm. The number of plates was 42.

[0046] In this example, the temperature at the botto...

Embodiment 3

[0058] The preparation of embodiment 3 electronic grade n-propyl propionate

[0059] 3.1 Synthesis of Propyl Propionate

[0060] Weigh 740.8g of propionic acid and 901.5g of propanol into a 3L reaction flask, then add 111.12g of ionic liquid [HNMP]PTSA catalyst and 200mL of water-carrying agent cyclohexane, heat and reflux at 100°C for 8 hours to separate water, and take samples for analysis. It is tested that the conversion rate reaches more than 99%, and the reaction is stopped. After the esterification liquid is cooled to room temperature, the solid (catalyst) is filtered off to obtain the crude product of n-propyl propionate.

[0061] 3.2 Vacuum distillation

[0062] The n-propyl propionate crude product is added in the rectification tower to carry out rectification under vacuum. The height of the rectification tower is 1.3m, and the inner diameter of the tower is 32mm. The number of plates was 42. The bottom temperature of the rectification tower is 50°C, the tem...

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Abstract

The invention relates to a preparation method for electronic-grade n-propyl propionate. The method comprises the following steps: performing a reaction on propionic acid and n-propanol to form crude n-propyl propionate under the catalysis of [HNMP]PTSA, performing reduced-pressure rectification, performing ion exchange resin adsorption impurity removal, and performing sub-boiling distillation to obtain the electronic-grade n-propyl propionate with a content of >= 99.99% and a metal ion content of less than 1 ppb, wherein the electronic-grade n-propyl propionate can be used as an electrolyte solvent in the lithium battery industry. According to the method provided by the invention, the catalyst used in the method has a high catalytic esterification rate, and the method adopts conventional purification equipment, has high product purity, is convenient to operate, and can realize industrialized production.

Description

technical field [0001] The invention belongs to the field of lithium battery electrolyte solvents, in particular to a preparation method of electronic grade n-propyl propionate. Background technique [0002] N-propyl propionate is an organic solvent widely used in chemical industry, paint, cosmetics, electronics and other fields. It has a low melting point (-76°C), low viscosity (0.68mPa. ~124°C), high dielectric constant (4.7, 20°C) and other properties, making it especially suitable as a lithium battery electrolyte solvent. Generally, n-propyl propionate as an electrolyte solvent requires a purity of 99.5 or higher, and higher requirements require a purity of 99.9 or higher. The higher the purity, the higher the oxidation resistance voltage of the prepared lithium battery, which can effectively prevent the battery from being overcharged. , to improve its security. In addition to the purity requirements, it is also necessary to strictly control the metal ion content of n-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/48C07C69/24
CPCC07C67/08C07C67/48C07C69/24
Inventor 陈锐周行贵袁浩杨义浒
Owner SHENZHEN ESUN IND
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