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Preparation method of 1,2,3-tris(2-cyanoethoxy)propane

A cyano group and propane technology, applied in the field of preparation of 1,2,3-tripropane, can solve the problems of unfavorable mass production and green environmental protection concept, large equipment investment, high energy consumption, and achieve high atomic utilization rate, The effect of small equipment investment and high yield

Pending Publication Date: 2021-06-04
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

1,2,3-tris(2-cyanooxy)propane is used as an additive in the battery electrolyte, which can reduce the battery expansion after being placed at high temperature and improve the performance of the battery, but the existing 1,2,3-tris(2 The preparation method of -cyanooxy) propane has many wastes, high energy consumption, long working hours and large equipment investment, which is not conducive to industrialized mass production and green environmental protection concept

Method used

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  • Preparation method of 1,2,3-tris(2-cyanoethoxy)propane
  • Preparation method of 1,2,3-tris(2-cyanoethoxy)propane

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Experimental program
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Effect test

Embodiment 1

[0027] Take 9.209g of glycerol, raise the temperature to 80°C, add 0.189g of sodium methoxide, cool down to 60°C, add 13.59g of acrylonitrile dropwise, control the temperature during the dropping process to 55°C, add the time for 4 hours, and continue to cool down to 30°C , add 3.1g of acrylonitrile dropwise, control the temperature during the dropping process to 30°C, add dropwise for 0.5h, stir at 20°C for 2h, after the reaction is complete, add the system to twice the amount of water, and stir for about 20 minutes. The system was separated into layers, the aqueous phase was extracted with dichloromethane, and the organic phases were combined. Dry, filter through silica gel activated carbon, and spin dry at 40°C under -0.1 atmospheric pressure to obtain 22.63g of 1,2,3-tris(2-cyanooxy)propane (yellow liquid), with a yield of 90.04%. Determined by gas chromatography, the purity of the resulting product is 99.06%, as Figure 1-3 , using mass spectrometry, H spectrum and C spe...

Embodiment 2

[0030] Take 9.209g of glycerol, raise the temperature to 70°C, add 0.216g of sodium methoxide, cool down to 65°C, add 13.876g of acrylonitrile dropwise, control the temperature during the dropping process to 50°C, drop the time for 5h, and continue to cool down to 35°C , add 3.084g of acrylonitrile dropwise, control the temperature during the dropping process to 15°C, add dropwise for 1h, stir at 15°C for 3h, after the reaction is complete, add the system to twice the amount of water, and stir for about 20 minutes. The system was separated into layers, the aqueous phase was extracted with dichloromethane, and the organic phases were combined. Dry, filter through silica gel activated carbon, and spin dry at 60°C under -0.1 atmospheric pressure to obtain 22.64g of 1,2,3-tris(2-cyanooxy)propane (yellow liquid), with a yield of 90.10%. As determined by gas chromatography, the purity of the obtained product is 99.03%, and the obtained product is identified as 1,2,3-tris(2-cyanooxy)...

Embodiment 3

[0032] Take 9.209g of glycerol, raise the temperature to 90°C, add 0.21g of sodium methoxide, cool down to 55°C, add 13.33g of acrylonitrile dropwise, control the temperature during the dropping process to 60°C, drop the time for 3 hours, and continue to cool down to 25°C , add 3.1g of acrylonitrile dropwise, control the temperature during the dropping process to 20°C, add dropwise for 40min, stir at 30°C for 2.5h, after the reaction is complete, add the system to twice the amount of water, and stir for about 20 minutes. The system was separated into layers, the aqueous phase was extracted with dichloromethane, and the organic phases were combined. Dry, filter through silica gel activated carbon, and spin dry at 50°C under -0.1 atmospheric pressure to obtain 22.75g of 1,2,3-tris(2-cyanooxy)propane (yellow liquid), with a yield of 90.54%. As determined by gas chromatography, the purity of the obtained product is 99.28%, and the obtained product is identified as 1,2,3-tris(2-cya...

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Abstract

The invention provides a preparation method of 1,2,3-tris(2-cyanoethoxy)propane, and belongs to the technical field of battery electrolytic solution additives. The method comprises the following steps: taking glycerol as a raw material, heating to 70-90 DEG C, adding sodium methoxide, cooling to 55-65 DEG C, dropwise adding a first batch of acrylonitrile, controlling the temperature in the dropwise adding process to 50-60 DEG C and the dropwise adding time to 3-5 hours, continuously cooling to 25-35 DEG C, dropwise adding a second batch of acrylonitrile, controlling the temperature in the dropwise adding process to be 15-30 DEG C and the dropwise adding time to be 0.5-1 h, stirring for 2-3 h at a temperature of 15-30 DEG C, extracting, drying, carrying out activated carbon suction filtration, and carrying out spin drying to obtain the 1,2,3-tris(2-cyanoethoxy)propane. According to the invention, the preparation method is simple, and the prepared 1,2,3-tris(2-cyanoethoxy)propane is high in yield and purity and has a good effect when being applied to a battery electrolyte.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte additives, and relates to 1,2,3-tris(2-cyanooxy)propane used in battery electrolytes, in particular to 1,2,3-tris(2-cyanooxy) Method for the preparation of propane. Background technique [0002] In recent years, there has been an increasing demand for small, lightweight secondary batteries capable of obtaining high energy density as power sources. Among them, lithium-ion batteries have the highest specific energy and can realize thinning of rechargeable batteries. Because lithium-ion batteries have high volume specific energy and mass specific energy, are rechargeable and non-polluting, they have considerable development prospects. [0003] With the continuous expansion of the use of lithium-ion batteries, the safety performance of lithium-ion batteries has become a bottleneck restricting the development, battery additives functional additives have become a new technology development...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/13
CPCC07C253/30C07C255/13
Inventor 张民葛建民闫彩桥王军郝俊武利斌侯荣雪田丽霞张茜
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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