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A kind of synthetic method of battery grade ferromanganese oxalate

A synthesis method, ferromanganese oxalate technology, applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., can solve the problems of difficult waste water treatment, impurity removal and purification, and environmental protection pressure, so as to reduce production Difficulty in quantity and handling, low production cost, and advanced discharge performance

Active Publication Date: 2020-05-19
赤峰开瑞科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] With the continuous expansion of market demand, there are many synthesis methods of ferromanganese oxalate, the positive electrode material of new energy vehicle lithium battery in the prior art, but there are still many methods for synthesizing ferromanganese oxalate in domestic chemical companies in the same industry. Such defects as: long process route, difficult impurity removal and refining, low product quality, large environmental pollution, high environmental protection pressure and other defects, and some synthesis methods have difficulties in separation, difficult treatment of waste water, and relatively complicated processes. Raw material quality and ratio control are demanding, relatively high investment and other defects

Method used

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  • A kind of synthetic method of battery grade ferromanganese oxalate
  • A kind of synthetic method of battery grade ferromanganese oxalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 80ml of concentrated sulfuric acid with a mass fraction of 98%, add a certain amount of water, and dilute it into dilute sulfuric acid with a mass fraction of 20% for later use; take 85ml of oxalic acid with a mass fraction of 45%, add a certain amount of mother liquor, and dilute it into a mass fraction of 25% dilute oxalic acid, for subsequent use;

[0022] Add 14.74 g (0.263 mol) of iron to the prepared dilute sulfuric acid solution, the reaction temperature is 40°C, and react for 1 to 2 hours to ensure complete reaction; at the same time, add the prepared dilute sulfuric acid solution to another reaction kettle 21.85g (0.397mol) of manganese metal was added to the mixture, the reaction temperature was 35°C, and the reaction was carried out for 1-2 hours;

[0023] The complete liquid of above-mentioned reaction carries out thorough mixing;

[0024] Start the mixer, to Add 62.41g (0.693mol) of prepared oxalic acid solution to the uniformly mixed liquid...

Embodiment 2

[0032] Take 100ml of concentrated sulfuric acid with a mass fraction of 98%, add a certain amount of water, dilute it into dilute sulfuric acid with a mass fraction of 20%, and set aside. Take 100ml of oxalic acid with a mass fraction of 40%, add a certain amount of mother liquor, dilute it into dilute oxalic acid with a mass fraction of 20%, and set aside.

[0033] Add 12.894g (0.23mol) of iron to the prepared dilute sulfuric acid solution, the reaction temperature is 36°C, and react for 1-2 hours to ensure complete reaction; Add 23.675g (0.43mol) of manganese metal to the mixture, the reaction temperature is 38°C, and the reaction is 1-2h;

[0034] The complete liquid of above-mentioned reaction carries out thorough mixing;

[0035] Start the mixer, to Add 62.41 g (0.693 mol) of the prepared oxalic acid solution to the uniformly mixed liquid, in which the excess of oxalic acid is 5%, control the pH value in the mixing tank between 5.5-6.5, the reaction temperature...

Embodiment 3

[0039] Take 90ml of concentrated sulfuric acid with a mass fraction of 98%, add a certain amount of water, and dilute it into dilute sulfuric acid with a mass fraction of 20%, and set aside; take 90ml of oxalic acid with a mass fraction of 50%, add a certain amount of mother liquor, and dilute into a mass fraction of 20% dilute oxalic acid, for subsequent use;

[0040] Add 16.579g (0.3158mol) of iron into the prepared dilute sulfuric acid solution, the reaction temperature is 35°C, and react for 1-2 hours to ensure complete reaction; at the same time, add the prepared dilute sulfuric acid solution to another reaction kettle Add 20.033g (0.364mol) of manganese metal to the mixture, the reaction temperature is 37°C, and the reaction is 1-2h;

[0041] The complete liquid of above-mentioned reaction carries out thorough mixing;

[0042] Start the mixer, to Add 62.41g (0.693mol) of prepared oxalic acid solution to the uniformly mixed liquid, in which the excess of oxalic...

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Abstract

The invention discloses a method for synthesizing battery-grade ferromanganese oxalate. Raw materials used in the method comprise iron, manganese, sulfuric acid and oxalic acid. The method comprises: reacting iron and dilute sulfuric acid to form a ferrous sulfate solution, adding manganese sulfate monohydrate to the ferrous sulfate solution, and stirring until completely dissolving; adding a certain amount of oxalic acid and ammonium oxalate to reaction mother liquor, stirring until completely dissolving, adding a standby mixed solution of manganese sulfate and ferrous sulfate, reacting for 1 to 2 hours, separating and filtering, washing, and performing vacuum drying to obtain a ferromanganese oxalate finished product finally. In the invention, low-cost raw materials are converted into ferromanganese oxalate, the technology is advanced and reasonable, the production cost is low and the economic benefit is good, so that the ferromanganese iron is a reasonable choice for auxiliary raw materials of positive electrode materials of novel energy vehicle lithium batteries in the future. After the reaction, the mother liquor is returned to the acid-forming process of concentrated sulfuric acid and oxalic acid, respectively. As the mother liquor after the reaction contains sulfuric acid solution, the mother liquor is recycled, the consumption of the raw materials is reduced, and the difficulty of wastewater treatment in the subsequent process is reduced.

Description

technical field [0001] The invention belongs to the technical field of new chemical materials, and in particular relates to a method for synthesizing ferromanganese oxalate, a raw material for a new energy lithium battery cathode material. Background technique [0002] With the continuous expansion of market demand, there are many synthesis methods of ferromanganese oxalate, the positive electrode material of new energy vehicle lithium battery in the prior art, but there are still many methods for synthesizing ferromanganese oxalate in domestic chemical companies in the same industry. Such defects as: long process route, difficult impurity removal and refining, low product quality, large environmental pollution, high environmental protection pressure and other defects, and some synthesis methods have difficulties in separation, difficult treatment of waste water, and relatively complicated processes. Raw material quality and ratio control are demanding, relatively high inves...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07C55/07
CPCC07C51/412C07C55/07
Inventor 刘武申正军肖琳李鸿雁
Owner 赤峰开瑞科技有限公司