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Iron oxalate crystal and preparation thereof

A ferrous oxalate and crystal technology, applied in the field of ferrous oxalate crystal and its manufacture, can solve problems such as complex process

Inactive Publication Date: 2009-06-24
海宁市盐官工业投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of production method of ferrous oxalate crystal, this method has overcome the problem of complicated technique of conventional method, and adopt this method to obtain the ferrous monoclinic oxalate crystal with particle size less than 3 μm

Method used

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  • Iron oxalate crystal and preparation thereof
  • Iron oxalate crystal and preparation thereof
  • Iron oxalate crystal and preparation thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Add 4L of deionized water into a constant temperature reactor with a volume of 5L with stirring, heating and heat preservation devices, and then add 556g (2.0mol) of ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) (analytical pure), open the heating device of the constant temperature reactor and make the system temperature rise to 45 ℃, stir simultaneously and make ferrous sulfate heptahydrate dissolve. 284g (2.0mol) ammonium oxalate solid grain {(NH 4 ) 2 C 2 o 4 ·H 2 O} (analytical pure) joins in the ferrous sulfate solution that dissolves completely with the feeding rate greater than 500g / min, simultaneously with the stirring rate mechanical stirring of 500 rev / mins 20 minutes. During this process, the temperature of the system was maintained at 45°C.

[0039] Close the heat preservation device, and let it stand for 30 minutes for aging to precipitate ferrous oxalate crystals.

[0040] The supernatant was separated, and the precipitated ferrous oxalate crystals ...

Embodiment 2

[0045] Add 4L of deionized water to a constant temperature reactor with a volume of 5L with stirring, heating and heat preservation devices, and then add 1335g (4.8mol) of ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) (analytical pure), open the heating device of the constant temperature reactor and make the system temperature rise to 55 ℃, stir simultaneously and make ferrous sulfate heptahydrate dissolve. 681g (4.8mol) of ammonium oxalate solid grain {(NH 4 ) 2 C 2 o 4 ·H 2 O} (analytical pure) joins in the ferrous sulfate solution that dissolves completely with the feed rate greater than 500g / min, simultaneously with the stirring rate mechanical stirring of 800 rev / mins 120 minutes. During this process, the temperature of the system was maintained at 55°C.

[0046] Close the heat preservation device, and let it stand for 30 minutes for aging to precipitate ferrous oxalate crystals.

[0047] The supernatant was separated, and the precipitated ferrous oxalate crystals ...

Embodiment 3

[0052] Add 4L of deionized water to a constant temperature reactor with a volume of 5L with stirring, heating and heat preservation devices, and then add 1890g (6.8mol) of ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) (analytically pure), the heating device of the constant temperature reactor is opened and the system temperature is raised to 75° C., while stirring makes ferrous sulfate heptahydrate dissolve. 965.6g (6.8mol) of ammonium oxalate solid grain {(NH 4 ) 2 C 2 o 4 ·H 2 O} (analytical pure) joins in the ferrous sulfate solution that dissolves completely with the feeding rate greater than 500g / min, simultaneously with the stirring rate mechanical stirring of 1000 rev / mins 150 minutes. During this process, the temperature of the system was maintained at 75°C.

[0053] Close the heat preservation device, and let it stand for 30 minutes for aging to precipitate ferrous oxalate crystals.

[0054] The supernatant was separated, and the precipitated ferrous oxalate cr...

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Abstract

The invention relates to a preparation method of monoclinic ferrous oxalate crystal (FeC2O4.2H2O) with particlesize less than 3mum and the monoclinic ferrous oxalate crystal with particlesize less than 3mum obtained by adopting the method. A solid-liquid two-phase method is adopted and the reaction is controlled by controlling the feeding speed of solid oxalate and the temperature and concentration of bivalence ferrous salt solution, thus achieving the purpose of generating the ferrous oxalate crystals with specific crystal formation and particlesize. The method is characterized in that: the solid oxalate is added into the bivalence ferrous salt water solution with concentration of Fe2+ being 0.5-1.7mol / l at the temperature of 40-80 DEG C at the feeding speed of more than 500g / min for reaction by temperature preservation. The method has simple process and high yield. The ferrous oxalate crystal with particlesize less than 3mum is obtained by the method, and the crystal formation is the monoclinic crystal.

Description

technical field [0001] The invention relates to a ferrous oxalate crystal and a manufacturing method thereof, in particular to a monoclinic ferrous oxalate crystal with a particle size less than 3 μm and a manufacturing method thereof. Background technique [0002] Ferrous oxalate crystals (FeC 2 o 4 2H 2 O) is one of the main materials for making lithium iron phosphate, the positive electrode active material of lithium-ion batteries. [0003] The currently known production method of ferrous oxalate crystals is to mix ferrous iron salt solution with oxalic acid or oxalate solution, and control the growth of ferrous oxalate crystals by strictly controlling process parameters, so as to produce oxalic acid with specific particle size or crystal form The purpose of ferrous crystals. However, these process parameters are protected by manufacturers in the form of commercial secrets, and generally the public cannot know them. In addition, CN 1948259A discloses a production met...

Claims

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Application Information

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IPC IPC(8): C07C55/07C07C51/41C30B29/54
Inventor 白琳曹文玉
Owner 海宁市盐官工业投资有限公司
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