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Preparation of iron oxalate hydrous salt crystal

A technology of ferrous oxalate and hydrated salt, applied in the preparation of carboxylate, organic chemistry and other directions, can solve the problems of large crystal size of ferrous oxalate hydrate and easy generation of impurities in ferrous oxalate hydrate crystals, and achieve high purity. Effect

Active Publication Date: 2011-05-25
海门市创豪工业设计有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to overcome the ferrous oxalate hydrate crystal particle size that existing method prepares is larger, and in the process of preparing ferrous oxalate hydrate crystal, easily produces the defect of impurity phase, provides a kind of can obtain particle size smaller and Preparation method of ferrous oxalate hydrate salt crystal with higher purity

Method used

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  • Preparation of iron oxalate hydrous salt crystal
  • Preparation of iron oxalate hydrous salt crystal
  • Preparation of iron oxalate hydrous salt crystal

Examples

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Effect test

Embodiment 1

[0033] Under stirring, 20 liters of 2.0 mol / liter ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) solution, in 1 minute, add to the dihydrate oxalic acid (H 2 C 2 o 4 ·H 2 (0) In the reaction vessel of the solution, after the addition is completed, the temperature of the reaction mixture is 50° C., and ferrous oxalate hydrate crystals are precipitated thereupon, and aged for 30 minutes.

[0034] Next, the ferrous oxalate was recovered by filtration, and the recovered ferrous oxalate was washed three times with 60 liters of deionized water. Next, the washed ferrous oxalate was dried at 80° C. for 12 hours to obtain 5.85 kg of dried product (90.3% yield).

[0035] The SEM image of this ferrous oxalate hydrate crystal measured by the JSM-5610-LV scanning electron microscope of Japan JEOL company is as follows figure 1 shown.

[0036]The XRD diffraction pattern of this lithium ferrous phosphate dry product measured by the D / MAX2200PC type X-ray powder diffractometer of Rigaku...

Embodiment 2

[0038] Prepare FeC according to the method identical with embodiment 1 2 o 4 2H 2 O, the difference is that 20 liters of 1.3 mol / liter oxalic acid dihydrate (H 2 C 2 o 4 ·H 2 O) solution was added to 20 liters of 1.5 mol / liter ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) solution, the addition time is 10 seconds, and the temperature of the reaction mixture is 30°C. After filtering, washing and drying, 4.19 kg of dry product was obtained (yield 89.6%).

[0039] The SEM image of this ferrous oxalate hydrate crystal measured by the JSM-5610-LV scanning electron microscope of Japan JEOL company is as follows figure 2 shown.

[0040] The XRD diffraction pattern of this lithium ferrous phosphate dry product measured by the D / MAX2200PC type X-ray powder diffractometer of Rigaku Corporation Japan is as follows Figure 7 shown.

Embodiment 3

[0042] Prepare FeC according to the method identical with embodiment 1 2 o 4 2H 2 O, the difference is that 20 liters of 5 mol / liter ferrous sulfate heptahydrate (FeSO 4 ·7H 2 (0) Solution is pumped in the reactor at a constant speed of 20 liters / minute, and simultaneously by a metering pump, 20 liters of 5 mol / liter of dihydrate oxalic acid (H 2 C 2 o 4 ·H 2 O) The solution was uniformly pumped into the reactor at a rate of 20 liters / minute, and the temperature of the reaction mixture was 70° C. After filtering, washing and drying, 15.62 kg of dry product was obtained (yield 86.8%).

[0043] The SEM image of this ferrous oxalate hydrate crystal measured by the JSM-5610-LV scanning electron microscope of Japan JEOL company is as follows image 3 shown.

[0044] The XRD diffraction pattern of this lithium ferrous phosphate dry product measured by the D / MAX2200PC type X-ray powder diffractometer of Rigaku Corporation Japan is as follows Figure 8 shown.

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Abstract

The invention provides a method for preparing ferrous oxalate hydrated salt crystals. The method comprises the following steps: carrying out the contact reaction between a solution A and a solution B. The contact manner and condition of the solution A and the solution B are provided to allow the produced ferrous oxalate hydrated salt to be supersaturated in the reaction mixed solution of the solution A and the solution B. By adopting the method, the prepared ferrous oxalate hydrated salt crystals have smaller average particle size and higher purity.

Description

technical field [0001] The invention relates to a preparation method of ferrous oxalate hydrate crystal. Background technique [0002] At present, lithium cobalt oxide (LiCoO 2 ), lithium nickel cobalt oxide (LiNi x co 1-x o 2 ), lithium nickel cobalt manganese oxide (LiNi x co y mn 1-x-y o 2 ) and lithium manganate (LiMn 2 o 4 ). LiCoO 2 、LiNi x co 1-x o 2 and LiNi x co y mn 1-x-y o 2 It has high conductivity and reversibility of lithium ion deintercalation, but has poor safety performance and high cost. Lithium manganate (LiMn 2 o 4 ) is relatively cheap and safe, but it not only has a small discharge capacity, but also has poor cycle life under high temperature conditions, and its cycle life cannot meet the needs of actual use. [0003] In order to solve the problems existing in the above-mentioned lithium battery materials, Professor J.B.Goodenough of the University of Texas in the United States et al. In an academic article published in the America...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/07C07C51/41
Inventor 白琳
Owner 海门市创豪工业设计有限公司
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