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Synthetic method of triphenoxyboroxine

A technology of triphenoxy boron and synthesis method, which is applied in the direction of chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, electrochemical generators, etc., which can solve unfavorable mass production and green environmental protection concepts, Problems such as large equipment investment and high energy consumption can achieve the effect of increasing reversible specific capacity, high purity and high yield

Inactive Publication Date: 2018-09-28
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the existing battery electrolyte additives are prepared, there are many wastes, high energy consumption, long working hours, and large investment in equipment, which is not conducive to industrialized mass production and the concept of green environmental protection.

Method used

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  • Synthetic method of triphenoxyboroxine
  • Synthetic method of triphenoxyboroxine
  • Synthetic method of triphenoxyboroxine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 1.02 mol of borane methyl sulfide into the Schlenk reaction flask, add 6 mol of THF to mix, then add 1 mol of phenol and 1 mol of water to it, heat and react at 70°C and 5 atm for 1 hour, then react at 80°C and pressure 120Pa for 30 minutes , and then reacted at 5 Pa and 100°C for 20 min, concentrated to dryness, and cooled to room temperature to obtain triphenoxyboroxane.

[0017] The density of the detected triphenoxyboroxane is 1.24g / cm 3 , boiling point 418°C 760mmHg, purity 99.58%, water content 38ppm, acid value 47ppm, yield 96.3%.

Embodiment 2

[0019] Add 1.03mol of borane methyl sulfide into the Schlenk reaction flask, add 8mol of THF to mix, then add 1mol of phenol and 1mol of water to it, heat the reaction at 80°C and 1 atm for 1.5h, and then react at 70°C and pressure of 80Pa 40min, and then reacted at 3Pa, 80°C for 30min, concentrated to dryness, and cooled to room temperature to obtain triphenoxyboroxane.

[0020] The density of the detected triphenoxyboroxane is 1.23g / cm 3 , boiling point 407°C 760mmHg, purity 99.56%, water content 40ppm, acid value 52ppm, yield 95.7%.

Embodiment 3

[0022] Add 1.02 mol of borane methyl sulfide into the Schlenk reaction flask, add 7 mol of THF to mix, then add 1 mol of phenol and 1 mol of water to it, heat and react at 75°C and 3 atm for 1.2h, then react at 75°C and pressure 100Pa 30min, then reacted at 4Pa, 90°C for 25min, concentrated and dried, and cooled to room temperature to obtain triphenoxyboroxane.

[0023] The density of the detected triphenoxyboroxane is 1.22g / cm 3 , boiling point 412°C 760mmHg, purity 99.78%, water content 30ppm, acid value 35ppm, yield 96.8%.

[0024] 2. Application test

[0025] Assembled batteries were tested for cycle performance. Lithium cobalt oxide was used as the positive electrode material, mesophase carbon microspheres were used as the negative electrode, aluminum foil and copper foil were used as current collectors for the positive and negative electrodes, and ceramic separators were used as the diaphragm to form a soft pack battery. After injecting the electrolyte, the The pouch b...

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Abstract

A synthetic method of triphenoxyboroxine belongs to the technical field of battery electrolyte and includes: subjecting borane-dimethylsulfide complex as a raw material to reaction with phenol to obtain triphenoxyboroxine, adding borane-dimethylsulfide complex into a Schlenk reaction flask, adding THF (tetrahydrofuran), mixing, adding phenol and water into the mixture, heating to allow reacting under 70-80 DEG C and 1-5 atm for 1-1.5 h, allowing reacting under 70-80 DEG C and 8-120 Pa for 30-40 min, allowing reacting under 3-5 Pa and 80-100 DEG C for 20-30 min, concentrating and drying, and cooling to room temperature to obtain triphenoxyboroxine. The synthetic method has the advantages that preparation is simple, a preparation technique is good in cleanliness and environmental friendliness, the preparation process is mild and stable, and prepared triphenoxyboroxine has high yield, high purity, low water content and low acid value.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte, and relates to a synthesis method of triphenoxyboroxane used in battery electrolyte. Background technique [0002] In recent years, portable electronic devices such as video cameras, digital cameras, cellular phones, and notebook computers have been widely used, and reducing their size and weight and achieving their long lifespan have become urgent demands. Accompanying this demand, batteries, particularly secondary batteries that are small and lightweight and capable of obtaining high energy density have been developed as power sources. [0003] Among them, lithium ion secondary batteries in which lithium ions are inserted and extracted for charge and discharge reactions, lithium metal secondary batteries in which lithium metal is deposited and dissolved, and the like are very promising. This is because such secondary batteries can provide higher energy density compared to lead batt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/05H01M10/0567
CPCC07F5/05H01M10/0567Y02E60/10
Inventor 郝俊王军闫彩桥葛建民苗强强张民武利斌侯荣雪
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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