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Preparation method of lithium difluoro(oxalato)borate

A technology of lithium difluorooxalate borate and lithium oxalate, applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve the problem of low purity of LiDFOB, unfavorable industrial production, and loss of reaction raw materials to avoid product loss, cheap materials, and easy access to materials

Active Publication Date: 2019-06-04
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently, the reported lithium difluorooxalate borate (Li[B(C 2 o 4 )F 2 ], LiDFOB) has many preparation methods, but most of them have disadvantages such as immature process, harsh reaction conditions or expensive raw materials, which are not conducive to large-scale industrial production, such as: using LiBF in European patent EP 1195834 4 、CH(CF 3 ) 2 OLi and oxalic acid (H 2 C 2 o 4 ) as a reactant reacts in a polar aprotic solvent to obtain the product LiDFOB. The disadvantage of this preparation method is that the obtained LiDFOB has a low purity and a large amount of LiBF 4 Does not participate in the reaction, causing the loss of reaction raw materials; in Chinese patent CN 104628754, the by-product LiBF 4 and H 2 C 2 o 4 The reaction was carried out while adding AlCl 3 or SiCl 4 as a catalyst, thereby removing LiBF 4 , the disadvantage of this preparation method is that the introduction of impurity ions Cl - ions and produce corrosive HF gas, and under normal temperature or heating conditions, LiBF 4 and H 2 C 2 o 4 The yield of LiDFOB obtained by the reaction is low, and the crude product LiDFOB still needs to undergo multiple recrystallizations to obtain high-purity LiODFB; 2 CO 3 Or LiOH reaction, and then through recrystallization, crystallization and other purification steps to obtain high-purity LiODFB, but the water generated during the reaction will decompose LiODFB, reducing the yield of the reaction

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  • Preparation method of lithium difluoro(oxalato)borate

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Experimental program
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Effect test

Embodiment 1

[0046] Step 1: Under the protection of nitrogen, add 40g of lithium oxalate and 150mL of acetonitrile into a 500mL three-necked flask, and then dropwise add 120g of boron trifluoride in ether solution. Clear reddish-brown solutions of lithium difluorooxalate borate and lithium tetrafluoroborate;

[0047] Step 2: Under the protection of nitrogen, add 66g of potassium oxalate and 300mL of acetonitrile to a 1000mL three-necked flask, then dropwise add 120g of boron trifluoride in ether solution. After the addition, the temperature is raised to 85°C for reaction, and heated to reflux for 10 hours to obtain White suspension of potassium difluorooxalate borate and potassium tetrafluoroborate;

[0048] Step 3: Under the protection of nitrogen, slowly add the transparent reddish-brown solution obtained in step 1 to the white suspension obtained in step 2, and heat to reflux at 80°C for 18 hours;

[0049] Step 4: After the reaction is completed, filter, concentrate the filtrate to 200...

Embodiment 2

[0051] Step 1: Under the protection of nitrogen, add 40g of lithium oxalate and 150mL of dimethyl carbonate to a 500mL three-necked flask, then dropwise add 120g of boron trifluoride in ether solution, after the dropwise addition, raise the temperature to 80°C for reaction, and heat to reflux for 8 hours , to obtain a transparent reddish-brown solution containing lithium difluorooxalate borate and lithium tetrafluoroborate;

[0052] Step 2: Under the protection of nitrogen, add 99g of potassium oxalate and 500mL of dimethyl carbonate to a 1000mL three-necked flask, then dropwise add 180g of boron trifluoride in ether solution, after the dropwise addition, raise the temperature to 80°C for reaction, and heat to reflux for 12 hours , to obtain a white suspension containing potassium difluorooxalate borate and potassium tetrafluoroborate;

[0053] Step 3: Under the protection of nitrogen, slowly drop the transparent red-brown solution obtained in step 1 into the white suspension ...

Embodiment 3

[0056] Step 1: Under the protection of nitrogen, add 40g of lithium oxalate and 150mL of diethyl carbonate to a 500mL three-necked flask, then dropwise add 120g of boron trifluoride in ether solution, after the dropwise addition, raise the temperature to 70°C for reaction, and heat to reflux for 9 hours , to obtain a transparent reddish-brown solution containing lithium difluorooxalate borate and lithium tetrafluoroborate;

[0057] Step 2: Under the protection of nitrogen, add 82.5g of potassium oxalate and 400mL of diethyl carbonate to a 1000mL three-necked flask, then add 150g of boron trifluoride in ether solution dropwise, after the addition, heat up to 80°C for reaction, and heat to reflux for 11 hours, a white suspension containing potassium difluorooxalate borate and potassium tetrafluoroborate was obtained;

[0058] Step 3: Under the protection of nitrogen, slowly add the transparent reddish-brown solution obtained in step 1 to the white suspension obtained in step 2, ...

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Abstract

The invention provides a preparation method of lithium difluoro(oxalato)borate (Li[B(C2O4)F2], LiDFOB). The method effectively recycles the by-product LiBF4, and avoids the waste of lithium atoms while improving the yield. The method utilizes the solubility difference of materials to directly filter out the by-product, and is simple in operation. The crude product is subjected to crystallization directly to obtain high purity LiDFOB, thus avoiding the product loss brought about by repeated recrystallization. The method has the advantages of cheap and easily available materials, simple reactionsteps and mild reaction conditions, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of manufacture of lithium ion battery electrolyte materials, in particular to a lithium difluorooxalate borate (Li[B(C 2 o 4 )F 2 ], LiDFOB) preparation. Background technique [0002] Electrolyte salt is an important part of lithium-ion batteries, and its research and development is very important to the performance and development of lithium-ion secondary batteries. Lithium difluorooxalate borate (Li[B(C 2 o 4 )F 2 ], LiDFOB) can be seen as half of lithium dioxalate borate (LiBOB) and half of lithium tetrafluoroborate (LiBF 4 ), and its performance cleverly combines the advantages of both. Lithium difluorooxalate borate (Li[B(C 2 o 4 )F 2 ], LiDFOB) has excellent high and low temperature performance, its thermal decomposition temperature is as high as 240 ° C, and it has good electrochemical performance at -20 ° C; it has a large solubility in carbonate solvents and a relatively wide electrochemic...

Claims

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Application Information

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IPC IPC(8): C07F5/02
Inventor 刘传松余意
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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