Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of tetrafluoromalonate phosphate

A technology of lithium tetrafluoromalonate phosphate and sodium malonate, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve serious gas production, corrosion of aluminum foil, electrical conductivity, etc. problems such as low rate of production, to achieve the effects of high production efficiency, mild reaction conditions and low cost

Active Publication Date: 2020-08-04
ZHUHAI SMOOTHWAY ELECTRONICS MATERIALS
View PDF4 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, commercial lithium-ion batteries mainly use LiPF6 as lithium salt, and its biggest disadvantage is: low chemical stability and thermal stability
However, these new lithium salts still have more or less problems when used under some extreme conditions (such as low conductivity, high impedance, corrosion of aluminum foil, serious gas production), and currently only a small amount can be added to the electrolyte as an additive. , therefore, it is of great theoretical and practical significance to design new lithium salts and explore their preparation methods

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of tetrafluoromalonate phosphate
  • A kind of preparation method of tetrafluoromalonate phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 400g of toluene was dropped into a 1000mL two-necked flask, then 41.64g of phosphorus pentachloride and 29.6g of sodium malonate (obtained according to the method of Adv. Submerge the two-necked flask in a 50°C oil bath and turn on the magnetic stirrer to fully stir the reaction. At the same time, nitrogen gas was introduced into it to replace the air in the flask, and the reaction was stopped after 1 hour of reaction.

[0036] The product liquid was filtered under reduced pressure, the white precipitate was removed to obtain a filtrate, and then the filtrate was concentrated and crystallized to obtain 53.12 g of a light yellow to white solid with a yield of 89.2%.

[0037] 53.12g of the above-mentioned obtained solid, 44.94g of the fluorinating reagent NaF and 0.83g of the catalyst NaI were successively dropped into a two-necked flask equipped with 400g of ethylene glycol dimethyl ether, a stirring bar was placed, and the two-necked flask was immersed in a 60°C oil bath...

Embodiment 2

[0041] 400g of toluene was dropped into a 1000mL two-necked flask, then 41.64g of phosphorus pentachloride and 33.2g of sodium 2-fluoromalonate were dropped into it (obtained according to the method of Adv.Energy Mater.2014,4,1301368), Put in a stirrer, immerse the two-neck flask in a 70°C oil bath and turn on the magnetic stirrer to fully stir the reaction. At the same time, pass nitrogen into it to replace the air in the flask, and stop the reaction after 1 hour of reaction.

[0042] The product liquid was filtered under reduced pressure to remove the white precipitate to obtain a filtrate, and then the filtrate was concentrated and crystallized to obtain 57.1 g of a light yellow to white solid with a yield of 90.4%.

[0043] Put 57.1g of the above-mentioned obtained solid, 45.55g of the fluorinating reagent NaF and 0.87g of the catalyst NaI into a two-necked flask containing 400g of tetrahydrofuran in turn, put a stirrer, immerse the two-necked flask in a 70°C oil bath and t...

Embodiment 3

[0047] Drop into 400g toluene in the 1000mL two-necked flask, then drop into 41.64g phosphorus pentachloride and 36.2g 2 fluoro-2-sodium methylmalonate therein (according to non-patent literature: Adv.Energy Mater.2014,4,1301368 method), put a stirrer, immerse the two-necked flask in an oil bath at 50°C and turn on the magnetic stirrer to fully stir the reaction. At the same time, nitrogen gas was introduced into it to replace the air in the flask, and the reaction was stopped after 1 hour of reaction.

[0048] The product liquid was filtered under reduced pressure to remove the white precipitate to obtain a filtrate, and then the filtrate was concentrated and crystallized to obtain 58.42 g of a light yellow to white solid with a yield of 88.3%.

[0049] Put 58.42g of the above-mentioned obtained solid, 44.49g of the fluorinating reagent NaF and 0.88g of the catalyst NaI into a two-necked flask equipped with 400g of acetonitrile in sequence, put a stirring bar, immerse the two-...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of tetrafluoromalonic phosphate. The method comprises the steps as follows: a certain proportion of sodium malonate and phosphorus pentachloride are addedto a non-aqueous solvent A, a reaction is conducted at a certain temperature, solid-liquid separation is performed after complete reaction, a filtrate is obtained, then, concentration crystallizationis performed, and a light yellow to white solid is obtained; the obtained solid and a certain proportion of a fluorinating reagent and a catalyst are added to a non-aqueous solvent B, solid-liquid separation is performed after full reaction at a certain temperature, a filtrate is obtained, a certain amount of MClO4 (M is any one of Li, Na and K) is added to the filtrate for ionic exchange, solid-liquid separation is performed after full exchange, a filtrate is obtained, then, concentration crystallization is performed, and tetrafluoromalonic phosphate is obtained. The method is simple in process, low in cost, mild in reaction condition and high in production efficiency. The product is expected to be used as lithium salt or an additive of a lithium-ion battery electrolyte.

Description

[technical field] [0001] The invention relates to a preparation method of tetrafluoromalonate phosphate used as an additive for non-aqueous electrolyte batteries. [Background technique] [0002] With the improvement of the performance requirements of lithium-ion batteries in the fields of electric vehicles, digital, and energy storage, it is of great significance to develop batteries with high energy density, long life, strong environmental adaptability, and high safety. This puts forward higher requirements on the performance of battery materials and electrolytes. Improving the compatibility of electrolytes and battery materials has always been the direction of research efforts. [0003] The electrolyte lithium salt is an important component of the electrolyte, and its composition and properties play a decisive role in the overall performance of the lithium-ion battery. The electrolyte lithium salt is not only the provider of lithium ions in the electrolyte, but also its a...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574
CPCC07F9/65742
Inventor 毛冲刘李阳戴晓兵
Owner ZHUHAI SMOOTHWAY ELECTRONICS MATERIALS