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Method for preparing cell grade ferrous oxalate with steel acid pickling waste liquor

A technology of iron and steel pickling waste liquid and ferrous oxalate, which is applied in the direction of carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problem of poor crystal phase structure and crystallinity, which affects the quality of ferrous oxalate products , The process is not well controlled, etc., to achieve the effect of uniform particles, more profits, and better crystal quality

Active Publication Date: 2016-07-06
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. Because the pickling waste liquid in steelworks is generally mixed with electroplating additives, mainly composed of C, H, O and other elements, the ferrous oxalate prepared by the above method can reach a purity of 99.5 even though the particle size is fine and uniform. %, but because the impurities of electroplating additives cannot be removed, the crystal phase structure and crystallinity are not good, and the crystal quality is not high, which directly affects the quality of lithium batteries prepared in the later stage
[0006] 2. The temperature of the whole preparation process is too high, close to the boiling point of water, so it can only be used for relatively stable pickling solutions such as sulfuric acid pickling solution and nitric acid picking solution. It will continue to volatilize at a high temperature, resulting in poor control of the process and affecting the quality of ferrous oxalate products
[0007] 3. Excessively high preparation temperature has relatively high requirements on the entire set of production equipment, and the energy consumption is too high, sometimes the output is not enough to offset the cost

Method used

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  • Method for preparing cell grade ferrous oxalate with steel acid pickling waste liquor
  • Method for preparing cell grade ferrous oxalate with steel acid pickling waste liquor
  • Method for preparing cell grade ferrous oxalate with steel acid pickling waste liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Pretreatment of waste iron and steel pickling: raise the temperature of waste iron and steel pickling to 85°C, add iron filings to adjust the concentration of ferrous ions to 180g / L, and use sulfuric acid and deionized water to adjust the pH value of the solution to 2 , At this time, a black oily substance will appear on the surface of the solution. Use a straw to remove the black oily substance produced on the surface of the solution, keep it warm at 85°C for 6 hours, and filter to remove impurities after standing still;

[0028] (2) Adding a dispersant: adding a mass-to-weight ratio of 20% dispersant polyvinylpyrrolidone to the solution pretreated in step (1), and mixing evenly;

[0029] (3) Generate ferrous hydroxide suspension: add ammoniacal liquor to adjust the pH value of the solution to 6 in the solution treated in step (2), and control the reaction temperature to be 25° C. to generate ferrous hydroxide suspension;

[0030] (4) generate ferrous oxalate preci...

Embodiment 2

[0033] All the preparation processes are the same as in Example 1, except that in step (1), an appropriate amount of iron filings is added and the acidity is adjusted by sulfuric acid and deionized water to adjust the ferrous ions to 200g / L.

Embodiment 3

[0035] All the preparation processes are the same as in Example 1, except that in step (1), an appropriate amount of iron filings is added and acidity is adjusted by sulfuric acid and deionized water to adjust the ferrous ions to 150g / L.

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Abstract

The invention relates to a method for preparing cell grade ferrous oxalate with steel acid pickling waste liquor.Through removing electroplating additive and adjusting the content of ferrous ions in the acid pickling waste liquor and the usage amount of dispersing agent, ferrous oxalate which is high in purity and crystallinity and even in appearance and has nanoscale can be prepared under a room temperature condition.Resource utilization optimization is adopted for the acid pickling waste liquor, in this way, economic burdens of steelworks caused by sewage treatment can be relieved, a cheap iron source is sought for preparation of cell grade lithium iron phosphate, the new method can be provided for effectively regulating the purity and particle size of cell grade ferrous oxalate, and more profits are created for the steelworks.

Description

technical field [0001] The invention relates to the technical field of material synthesis, in particular to a method for preparing battery-grade ferrous oxalate by using iron and steel pickling waste liquid. Background technique [0002] The pickling waste liquid produced by hot rolling of steel generally contains 0.05-5g / L H + and 60-250g / L Fe 2+ . Due to its severe corrosiveness, it has been included in the "National List of Hazardous Wastes". The direct discharge of this kind of waste liquid not only seriously pollutes the environment, but also causes great waste. At present, the treatment and application of iron and steel pickling waste liquid are mostly for the recovery of iron, or the recovery of iron oxides as fuel, or the use of pickling waste liquid to prepare sewage treatment agents. [0003] Lithium iron phosphate electrode material has abundant resources, low price, no pollution to the environment, and good thermal stability. It is considered to be one of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C55/07
CPCC07C51/412C07C55/07
Inventor 张英杰李雪朱子翼邱振平董鹏
Owner KUNMING UNIV OF SCI & TECH
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