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The synthetic method of lithium battery additive 3-cyanopropyl dimethyl fluorosilane

A technology of cyanopropyldimethylfluorosilane and dimethyldichlorosilane, which is applied in the field of organosilicon compound synthesis, can solve the problems of increased product cost, slow initiation speed, and slow initiation process, so as to facilitate production and reduce volatilization , easy to react effect

Active Publication Date: 2021-05-18
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, dimethylchlorosilane requires a special process to prepare, is difficult to obtain, has low purity, is expensive, and greatly increases the product cost.
Simultaneously, using dimethyl chlorosilane and allyl nitrile as raw materials, the initiation process is slow, requiring a large amount of noble metal catalysts, which also causes the problems of slow initiation speed and high cost.

Method used

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  • The synthetic method of lithium battery additive 3-cyanopropyl dimethyl fluorosilane
  • The synthetic method of lithium battery additive 3-cyanopropyl dimethyl fluorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Adopt route one to prepare 3-cyanopropyl dimethyl fluorosilane:

[0032] (1) Heat 41.4g (1.8mol) of sodium metal and 420g of anhydrous toluene to 108°C under stirring, then add 103.5g (1mol) of 4-chloro-n-butyronitrile dropwise, dropwise for 2 hours, and continue at 110°C React for 1h to get N≡CCH 2 CH 2 CH 2 Na suspension;

[0033] (2) Warm up 116.1g (0.9mol) dimethyldichlorosilane to 40°C, add N≡CCH dropwise 2 CH 2 CH 2 Add the Na suspension solution dropwise for 3 hours, continue to react at 45°C for 1 hour, and filter to obtain the crude product of 3-cyanopropyldimethylchlorosilane; carry out vacuum distillation on the crude product, and collect 97°C / -0.1MPa The distillate obtains 3-cyanopropyl dimethyl chlorosilane;

[0034] (3) Ammonium bifluoride was added to the reactor, and 3-cyanopropyldimethylsilyl chloride was added dropwise, and the addition was completed after 0.5h, and the reaction was continued for 2h. After adding n-hexane and stirring for 15 mi...

Embodiment 2

[0037] Adopt route one to prepare 3-cyanopropyl dimethyl fluorosilane:

[0038] (1) Heat 46g (2mol) of sodium metal and 350g of anhydrous toluene to 105°C under stirring, then add 103.5g (1mol) of 4-chloro-n-butyronitrile dropwise for 1 hour, and continue the reaction at 108°C for 1.5 h, to get N≡CCH 2 CH 2 CH 2 Na suspension;

[0039] (2) Warm up 129g (1mol) dimethyldichlorosilane to 35°C, add N≡CCH dropwise 2 CH 2 CH 2Na suspension, after 2 hours of dropwise addition, continue to react at 40°C for 1.5h, filter to obtain the crude product of 3-cyanopropyldimethylsilyl chloride; carry out vacuum distillation on the crude product, collect 97°C / -0.1 The cut of MPa obtains 3-cyanopropyl dimethyl chlorosilane;

[0040] (3) Ammonium bifluoride was added to the reactor, and 3-cyanopropyldimethylsilyl chloride was added dropwise, and the addition was completed after 0.5h, and the reaction was continued for 2h. After adding n-hexane and stirring for 15 minutes, the liquid prod...

Embodiment 3

[0043] Adopt route two to prepare 3-cyanopropyl dimethyl fluorosilane:

[0044] (1) Heat 41.4g (1.8mol) of sodium metal and 500g of anhydrous toluene to 108°C under stirring, then add 103.5g (1mol) of 4-chloro-n-butyronitrile dropwise, dropwise for 2 hours, and continue at 110°C React for 1h to get N≡CCH 2 CH 2 CH 2 Na suspension;

[0045] (2) Add 116.1g (0.9mol) of dimethyldichlorosilane to 136.8g (2.4mol) of ammonium bifluoride and stir for 1 hour to obtain dimethyldifluorosilane;

[0046] (3) Dimethyldifluorosilane is heated to 35°C in a pressure vessel (pressure 0.6MPa), and N≡CCH 2 CH 2 CH 2 The Na suspension was slowly added dropwise to the container, and the dropwise addition was completed after 3 hours, and the reaction was continued at 40°C for 2 hours to obtain the crude product of 3-cyanopropyldimethylsilyl chloride;

[0047] (4) The crude product was rectified under reduced pressure, and the fraction at 81°C / -0.1MPa was collected to obtain 3-cyanopropyldimet...

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Abstract

The invention relates to the technical field of organosilicon compound synthesis, in particular to a method for synthesizing lithium battery auxiliary agent 3-cyanopropyldimethylfluorosilane. The synthesis method is as follows: 4-chloro-n-butyronitrile is added dropwise in an anhydrous solvent of sodium to react to obtain N≡CCH 2 CH 2 CH 2 The suspension of Na, then through any one of the following two routes, to obtain 3-cyanopropyl dimethyl fluorosilane; route one is N≡CCH 2 CH 2 CH 2 Na first reacts with dimethyl dichlorosilane to obtain 3-cyanopropyl dimethyl chlorosilane, and then obtains 3-cyanopropyl dimethyl fluorosilane through fluorination; to obtain dimethyldifluorosilane, and then with N≡CCH 2 CH 2 CH 2 Na reaction gives 3‑cyanopropyldimethylfluorosilane. The raw materials used in the invention are easy to obtain, low in cost and higher in purity, the method used is easy to react, and is economically feasible.

Description

technical field [0001] The invention relates to the technical field of organosilicon compound synthesis, in particular to a synthesis method of 3-cyanopropyldimethylfluorosilane, a lithium battery auxiliary agent. Background technique [0002] Lithium-ion batteries have the advantages of high open circuit voltage, long cycle life, high energy density, no memory effect, and environmental friendliness, making them the first choice for large and medium-sized energy storage devices such as various portable electronic products and electric vehicles. Advances in material technology are the basis for the development of lithium-ion batteries. Electrode and electrolyte materials are one of the core components of lithium-ion batteries, which play a decisive role in battery performance and are currently the main constraints on the further development of lithium-ion batteries. Finding new electrode and electrolyte materials and improving traditional materials have become the current Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
Inventor 伊港王春晓刘海龙胡庆超耿宁张玉娇肖月玲
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL