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Production method of ferrous oxalate special for ferrous lithium phosphate

A technology of ferrous oxalate and its production method, which is applied in the field of preparation of known fine chemicals and can solve problems such as single crystal form

Inactive Publication Date: 2009-05-20
HEFEI ASIALON CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The technical problem to be solved is to improve the process to prepare ferrous oxalate with a single crystal form

Method used

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  • Production method of ferrous oxalate special for ferrous lithium phosphate
  • Production method of ferrous oxalate special for ferrous lithium phosphate

Examples

Experimental program
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Embodiment Construction

[0017] 1. Ferrous sulfate pretreatment

[0018] Put ferrous sulfate into a stainless steel water washing kettle, add pure water (distilled water) to stir and wash for 2 to 3 times, filter and separate, add the washed ferrous sulfate into an enamel dissolution kettle, add pure water to stir and dissolve, adjust pH with sulfuric acid To 3, add 2% sucrose at the same time, stir and dissolve, then stand still, clarify, and after filtration and separation, pump the ferrous sulfate clarified solution into the storage tank for subsequent use.

[0019] 2, the synthesis of ferrous monoclinic oxalate

[0020] Add oxalic acid and pure water into a stirring enamel synthesis kettle, stir and dissolve, and control the concentration of oxalic acid to 35-50 wt%. Slowly pass ammonia under stirring, at this time, the temperature in the kettle rises, when the temperature rises to 85-95°C (at this time, the ammonium acid ratio is about 7.5:3.5), stop passing ammonia, and add ferrous sulfate solu...

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Abstract

The present invention relates to a method for preparing ferrous oxalate. Said method uses ferrous sulfate and oxalic acid as raw material, and includes the following steps: pretreatment of ferrous sulfate, said pretreatment includes: water-washing ferrous sulfate and inhibiting hydrolysis of its aqueous solution; mixing the pretreated ferrous sulfate with ammonium oxalate and oxalic acid according to the mole ratio of 3:7-8:2 to obtain their mixed solution; making said mixed solution produce reaction for 10-20 min at 65-95 deg.C, then standing still for 2-4 h, separating, washing and drying so as to obtain the invented product ferrous oxalate.

Description

1. Technical field [0001] The invention relates to a method for preparing known fine chemicals, in particular to a method for producing ferrous oxalate special for lithium iron phosphate. 2. Background technology [0002] Ferrous oxalate, whose chemical name is ferrous oxalate, is currently one of the main raw materials for the preparation of a new lithium battery cathode material—lithium iron phosphate. [0003] The known preparation method of ferrous oxalate is exactly that ferrous sulfate is added in the oxalic acid solution and reacts, and the ferrous oxalate of generation precipitates out, promptly packs factory after separating, washing and drying. The yield of this method is only about 80%, and the product purity is 98-99%. [0004] Ferrous oxalate prepared by known methods cannot meet the requirements of new lithium battery cathode materials, not only the purity is not enough, the particle size is large (35 ~ 45 μm), especially the crystal form is unstable and not s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/07C07C51/41
Inventor 李传友
Owner HEFEI ASIALON CHEM
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