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Preparation method of ethylene glycol bis(propionitrile) ether

A technology of ethylene glycol bis and ethylene glycol, which is applied in the field of preparation of ethylene glycol bis-ether, can solve the problems of low concentration, influence on molar yield, and difficulty in improving the purity, so as to reduce alkalinity and reduce by-product bis-propylene. Production of nitrile ether and effect of improving molar yield

Active Publication Date: 2016-11-23
ZHANGJIAGANG HICOMER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ethylene glycol bis(propionitrile) ether has strict purity requirements as an additive for lithium-ion battery electrolyte, so high-purity ethylene glycol bis(propionitrile) ether can be better used as an additive for lithium-ion battery electrolyte, but The preparation method of existing ethylene glycol two (propionitrile) ethers is owing to all adopting single alkaline hydroxide as catalyzer, and can carry out normally in order to make reaction, the concentration of single alkaline hydroxide can not be very low, like this Make the alkalinity of solution in the reaction process stronger, thereby the by-product that hydrolysis generates will be more, the by-product in the reactant will greatly influence the molar yield of two (propionitrile) ethers of ethylene glycol, and also Will greatly increase the difficulty of purification of ethylene glycol bis(propionitrile) ether, making it difficult to improve the purity of ethylene glycol bis(propionitrile) ether

Method used

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  • Preparation method of ethylene glycol bis(propionitrile) ether

Examples

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Effect test

Embodiment 1

[0016] In a three-neck flask equipped with mechanical stirring, thermometer, dropping device, and condenser, add 62g (1mol) of ethylene glycol and 159g (3mol) of acrylonitrile for stirring, then slowly raise the temperature, and add the compound base dropwise at a temperature of 30°C Catalyst aqueous solution (mass concentration is 5% triethylbenzyl ammonium hydroxide aqueous solution 186g and mass concentration is 3% sodium hydroxide aqueous solution 62g) 248g, after dropwise addition, at 30 ℃ of temperature insulation 12 hours, then to The reaction solution was neutralized, and then 60.3 g of unreacted acrylonitrile and 413 g of reclaimed water were recovered by distillation in the reactant, and then the reactant was subjected to vacuum distillation under a pressure of -0.01Mpa, and cuts were collected to obtain high-purity acrylonitrile. 159.0 g (purity: 98.52%) of diol bis(propionitrile) ether, the molar yield is 93.14%.

Embodiment 2

[0018] In a three-necked flask equipped with a mechanical stirrer, a thermometer, a dropping device, and a condenser, add 62g (1mol) of ethylene glycol and 106g (2mol) of acrylonitrile for stirring, then slowly raise the temperature, and add the compound base dropwise at a temperature of 50°C Catalyst aqueous solution (mass concentration is 4% triethylbenzyl ammonium hydroxide aqueous solution 248g and mass concentration is 2% sodium hydroxide aqueous solution 74.4g) 322.4g, after dropping, at 50 ℃ temperature insulation 11 hours, Then the reaction solution is neutralized, and then 8.4 g of unreacted acrylonitrile and 524 g of recovered water are recovered by distillation in the reactant, and then the reactant is subjected to vacuum distillation under a pressure of -0.01Mpa, and the fraction is collected to obtain a high-purity 158.5 g of ethylene glycol bis(propionitrile) ether (purity: 98.28%), and the molar yield is 92.61%.

Embodiment 3

[0020] In a three-neck flask equipped with mechanical stirring, thermometer, dropping device, and condenser tube, add 62g (1mol) of ethylene glycol and 265g (5mol) of acrylonitrile for stirring, then slowly raise the temperature, and add the compound base dropwise at a temperature of 70°C Catalyst (mass concentration is 3% triethylbenzyl ammonium hydroxide aqueous solution 217g and mass concentration is 2% sodium hydroxide aqueous solution 80.6g) 297.6g, was incubated at 70 ℃ of temperature for 10 hours after dropping, then Neutralize the reaction solution, then distill and recover 167.8 g of unreacted acrylonitrile and 468 g of recovered water in the reactant, then carry out vacuum distillation on the reactant under the pressure of -0.01Mpa, and collect the fractions to obtain high-purity Ethylene glycol bis(propionitrile) ether 157.1g (purity 98.16%), molar yield 91.67%.

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Abstract

The invention discloses a preparation method of ethylene glycol bis(propionitrile) ether. The preparation method includes: using ethylene glycol and acrylonitrile as reaction raw materials, and allowing the two to have reaction under the reaction temperature of 30-70 DEG C and the catalyzing of a catalyst aqueous solution to generate the ethylene glycol bis(propionitrile) ether, wherein the catalyst aqueous solution is a composite alkali catalyst aqueous solution mixed by a triethyl benzyl ammonium hydroxide aqueous solution and a sodium hydroxide aqueous solution. Due to the fact that the composite alkali catalyst aqueous solution low in alkalinity is used, the alkalinity in the reaction solution is weakened greatly, the generation of the byproduct bis-propionitrile ether can be reduced greatly, the mole yield of the ethylene glycol bis(propionitrile) ether can be increased greatly to reach above 90%, purification can be performed easily to obtain the high-purity ethylene glycol bis(propionitrile) ether, and the purity of the ethylene glycol bis(propionitrile) ether can reach above 95%.

Description

technical field [0001] The invention relates to the field of electrolyte additives for lithium ion batteries, in particular to a preparation method of ethylene glycol bis(propionitrile) ether which can be used as an additive for electrolytes of lithium ion batteries. Background technique [0002] The structural formula of ethylene glycol bis(propionitrile) ether is: Ethylene glycol bis(propionitrile) ether is a new type of additive that can make the electrolyte of lithium-ion batteries more effective. Adding ethylene glycol bis(propionitrile) ether to lithium-ion batteries can inhibit storage or charge and discharge at high temperatures. In addition, it can also improve the cycle life of lithium-ion battery charging and discharging. Ethylene glycol bis(propionitrile) ether has strict purity requirements as an additive for lithium-ion battery electrolyte, so high-purity ethylene glycol bis(propionitrile) ether can be better used as an additive for lithium-ion battery electr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/13
CPCY02P20/582C07C253/30
Inventor 戴江英许国荣许逸达丁敬敏庞宝华刘冬
Owner ZHANGJIAGANG HICOMER CHEM CO LTD
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