Synthesis method of trimethoxyboroxine

A technology of trimethoxy boron and synthesis method, which is applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., which can solve the problems of unfavorable mass production, green environmental protection concept, and large investment in equipment , long working hours and other issues, to achieve the effect of increasing reversible specific capacity, high purity and low acid value

Active Publication Date: 2018-12-21
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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  • Synthesis method of trimethoxyboroxine
  • Synthesis method of trimethoxyboroxine
  • Synthesis method of trimethoxyboroxine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] At -80°C, add 1 mol of borane methyl sulfide into the Schlenk reaction flask, add 6 mol of THF to it, then mix for 20 seconds under a vacuum of 0.7 Pa, then pass carbon dioxide into it, control the pressure at 100 kPa, first in The temperature was raised to 20°C within 15min, then heated at a heating rate of 3°C / min for 10min, then heated at a heating rate of 3°C / min for 10min, and then heated to 80°C, no borane methyl sulfide was detected, and the reaction ended ( After heating up to 80°C, the timed reaction only takes 30 minutes) to obtain trimethoxyboroxane.

[0017] The obtained trimethoxyboroxane density is 1.1g / cm 3 , boiling point 130°C 760mmHg, purity 99.56%, acid value 34ppm, water content 28ppm, yield 95.3%.

Embodiment 2

[0019] At -70°C, add 1 mol of borane methyl sulfide into the Schlenk reaction flask, add 8 mol of THF to it, then mix for 30 seconds under a vacuum of 0.5 Pa, then pass carbon dioxide into it, control the pressure at 90 kPa, first in Heat up to 30°C within 15min, then heat at a heating rate of 1.5°C / min for 15min, then heat at a heating rate of 2°C / min for 10min, heat up to 72.5°C, detect no borane methyl sulfide, and the reaction ends ( After heating up to 72.5°C, the timed reaction only takes 40 minutes) to obtain trimethoxyboroxane.

[0020] The obtained trimethoxyboroxane density is 1.15g / cm 3 , boiling point 131°C 760mmHg, purity 99.68%, acid value 32ppm, water content 25ppm, yield 95.8%.

Embodiment 3

[0022] At -60°C, add 1 mol of borane methyl sulfide into the Schlenk reaction flask, add 7 mol of THF to it, then mix for 25 seconds under a vacuum of 0.6 Pa, then pass carbon dioxide into it, control the pressure at 95 kPa, first in Heat up to 25°C within 15min, then heat at a heating rate of 2°C / min for 10min, then heat at a heating rate of 2°C / min for 15min, then heat up to 75°C, detect no borane methyl sulfide, and the reaction ends ( After heating up to 75°C, the timed reaction only takes 35 minutes) to obtain trimethoxyboroxane.

[0023] The obtained trimethoxyboroxane density is 1.15g / cm 3 , boiling point 129°C 760mmHg, purity 99.62%, acid value 35ppm, water content 30ppm, yield 96.2%.

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Abstract

The invention provides a synthesis method of trimethoxyboroxine. Borane methyl sulfide serves as a raw material to react with carbon dioxide, trimethoxyboroxine is obtained, borane methyl sulfide is added into a Schlenk reaction bottle at the temperature of -60 - -80 DEG C, THF (tetrahydrofuran) is added into the Schlenk reaction bottle to be mixed for 15-20 seconds under the pressure of 0.5-0.7Pa, carbon dioxide is guided into the reaction bottle, the pressure is controlled to be 90-100kPa, then heating is conducted till the temperature reaches 70-80 DEG C, it is detected that no borane methyl sulfide exists, the reaction is ended, and trimethoxyboroxine is obtained. The preparation method is simple, the preparation technology is clean and environmentally friendly, the preparation processis moderate and stable, the yield of the prepared trimethoxyboroxine is high, the purity is high, the water content is low, and the acid value is low.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte, and relates to a synthesis method of trimethoxyboroxane 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): C07F5/05H01M10/0567H01M10/42
CPCC07F5/05H01M10/0567H01M10/4235Y02E60/10
Inventor 苗强强葛建民闫彩桥王军郝俊张民武利斌侯荣雪
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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