Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Microwave process of synthesizing lithium dioxalate borate

A technology of bis-oxalate lithium borate and microwave method, applied in the field of lithium borate, can solve the problems such as LiBOB that have not been seen, and achieve the effects of short synthesis time, less impurities and high yield

Inactive Publication Date: 2007-08-22
SHANDONG HIRONG POWER SUPPLY MATERIAL
View PDF1 Cites 22 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In published articles and patents, there is no report on synthesizing LiBOB using the same method as the present invention

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
  • Microwave process of synthesizing lithium dioxalate borate
  • Microwave process of synthesizing lithium dioxalate borate
  • Microwave process of synthesizing lithium dioxalate borate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Press H 2 C 2 o 4 2H 2 O: LiOH·H 2 O:H 3 BO 3 =2.1:1:1 ratio, weigh H 2 C 2 o 4 2H 2 O 13.23 g, LiOH·H 2 O 2.1 g, mechanically mixed for 2 min before adding H 3 BO 3 3.09 g, continue mixing for 3 minutes. Put the mixed material into a beaker, then put the beaker in a microwave oven, adopt 160W, the first section is 5 minutes, heat preservation is 10 minutes, and the second section is 9 minutes to synthesize LiB(C 2 o 4 ) 2 , as can be seen from the XRD pattern, the synthesized product is basically LiB(C 2 o 4 ) 2 , but contains a small amount of impurities. There is no impurity peak in the XRD figure of the product after one purification. The results are shown in Figure 2.

Embodiment 2

[0023] Press H 2 C 2 o 4 2H 2 O: LiOH·H 2 O:H 3 BO 3 =2.2:1:1 ratio, weigh H 2 C 2 o 4 2H 2 O 27.87 g, LiOH·H 2 O 4.2 g, mechanically mixed for 3 min before adding H 3BO 3 6.214 grams, continue mixing for 4 minutes. Put the mixture into the beaker, then put the beaker into the microwave oven, the first section of 160W, 5 minutes, keep warm for 10 minutes. The second stage 160W 25 minutes, keep warm for 10 minutes. The XRD pattern of the synthesized product is shown in Figure 3. Comparing Figure 1 and Figure 3, it can be seen that increasing the proportion of oxalic acid and increasing the intermediate stirring link are conducive to reducing the content of impurities.

Embodiment 3

[0025] Press H 2 C 2 o 4 2H 2 O: LiOH·H 2 O:H 3 BO 3 =2.1:1:1 ratio, weigh H 2 C 2 o 4 2H 2 O 27.87 g, LiOH·H 2 O 4.2 g, mechanically mixed for 3 min before adding H 3 BO 3 6.214 grams, continue mixing for 4 minutes. Put the mixture into a beaker, then put the beaker into the microwave oven, the first stage is 210W, 5 minutes, keep warm for 10 minutes, stir once between the two stages. The second stage is 330W for 30 minutes, and keep warm for 10 minutes. The XRD pattern of the synthesized product is shown in Figure 4. Comparing Figure 3 and Figure 4, it can be seen that increasing the microwave power is beneficial to reduce the content of impurities.

[0026] Fig. 5 is the NMR boron spectrum before and after the purification of the product of Example 3, as can be seen, the product before purification does not have any impurity peaks except a B main peak of LiBOB, indicating that the product does not contain boron impurities at this time, and it shows as Less ...

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 present invention is microwave process of synthesizing LiB(C2O4)2 material, and belongs to the field of lithium borate material technology. The process includes mixing oxalic acid and LiOH.H2O in ratio of (2.5-1.8) to 1 or oxalic acid and Li2CO3 in ratio of (4.1-3.8) to 1 mechanically in a stirrer of 12000 rpm; adding H3BO3 in the ratio to LiOH.H2O of (0.8-1) to 1 and the ratio to Li2CO3 of (1.9-2) to 1 before further stirring for 1-10 min; and setting mixture into beaker and setting the beaker in a microwave oven of 2.45 GHz frequency and 700 W maximum power for two stage synthesis of power of 100-400 W and 200-600 W separately. Compared with common solid phase synthesis process, the present invention has the advantages of fast heating, short synthesis process, low power consumption, and high product yield and purity.

Description

technical field [0001] The invention belongs to the technical field of lithium borate, and in particular provides a method for synthesizing bisoxalatolithium borate LiB(C 2 o 4 ) 2 method, applied to lithium-ion battery electrolyte salts. Background technique [0002] As a new type of power supply, lithium-ion batteries have been widely valued since they were proposed and commercialized in the 1990s. They have high specific energy, no memory effect, no pollution, small self-discharge, high working voltage, and long cycle life. Long and other advantages. As an important part of lithium-ion batteries, the electrolyte solution has a crucial influence on the performance of lithium-ion batteries. LiPF is currently the most commercially used 6 . Although containing LiPF 6 Salt electrolytes have high electrical conductivity and electrochemical stability window, but poor thermal stability. In organic solvents, LiPF 6 The following balance exists: [0003] LiPF 6 (sol.) = ...

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 Applications(China)
IPC IPC(8): C07F5/02
Inventor 仇卫华王赛刘伟黄佳原
Owner SHANDONG HIRONG POWER SUPPLY MATERIAL
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products