A kind of production technology of nanoscale anhydrous ferrous oxalate

A water ferrous oxalate, production process technology, applied in electrochemical generators, structural parts, electrical components, etc., can solve the problems of rising material costs, low lithium iron phosphate capacity, and poor treatment of industrial waste liquids, and achieve high The effect of high specific surface area and high purity

Active Publication Date: 2018-09-28
山东源来环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although there are many methods for preparing lithium iron phosphate, such as high-temperature solid-phase method, hydrothermal method, microwave method, sol-gel method, coprecipitation method, etc., the industrial waste liquid generated by the liquid-phase method is not easy to handle, resulting in material costs. The microwave method cannot achieve large-scale production, so in the preparation method of lithium iron phosphate, the high-temperature solid-phase method is still the mainstream
However, the high-temperature solid-phase method uses raw materials with larger particle size and higher melting point to synthesize lithium iron phosphate with lower actual capacity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Get ready to contain ferrous sulfate 25%, sulfuric acid 20%, the solution 1 of water 55% (above percentage is mass ratio) is placed in metering tank 1; The aqueous solution 2 that is ready to contain oxalic acid 15% is placed in metering tank 2, puts Add 4 tons of solution 1 and 4 tons of solution 2 to the reactor, add 1 kg of anti-flocculating agent A and 2 kg of anti-flocculating agent B at the same time, stir and heat up to 90°C, keep it at 90°C for 3 hours, and cool down to 60°C after the reaction ℃, and pump the mixture to a nano filter press, press filter and wash 5 times, send the filter cake to a vacuum dryer, and dry it at 80 °C at -0.08MPa. The dried nano FeC 2 o 4 2H 2 O is sent to a closed secondary dehydrator filled with xylene through a screw conveyor. At 95-140°C and -0.1MPa, use the azeotropy of xylene and water to remove crystal water during the process of removing xylene. Compared with the conventional thermal decomposition decrystallization water pr...

Embodiment 2

[0031] Prepare solution 1 containing 20% ​​ferrous sulfate, 18% sulfuric acid, and 62% water and place it in metering tank 1; prepare an aqueous solution containing 14% oxalic acid, that is, solution 2, and place it in metering tank 2, and put 4 tons of solution 1 and 4 tons Add solution 2 to the reaction kettle, add 1 kg of anti-flocculation agent A and 4 kg of anti-flocculation agent B at the same time, stir and heat up to 90 ° C, and keep it at 90 ° C for 3 hours, after the reaction is completed, cool down to 60 ° C, and pump the mixture to a nano filter press, press filter and wash 5 times, send the filter cake to a vacuum dryer, and dry it at 80°C at -0.08MPa, and dry the dried nano FeC 2 o 4 2H 2 O is sent to a closed secondary dehydrator filled with xylene through a screw conveyor. At 95-140°C and -0.1MPa, use the azeotropy of xylene and water to remove crystal water during the process of removing xylene. Compared with the conventional thermal decomposition decrystall...

Embodiment 3

[0033]Prepare a solution 1 containing 30% ferrous sulfate, 20% sulfuric acid, and 50% water and place it in metering tank 1; prepare an aqueous solution 2 containing 20% ​​oxalic acid and place it in metering tank 2, and put 4 tons of solution A and 4 tons of solution B Add to the reaction kettle, add 4 kg of anti-flocculation agent A and 1 kg of anti-flocculation agent B at the same time, stir and heat up to 90 ° C, and keep it at 90 ° C for 3 hours, after the reaction is completed, cool down to 60 ° C, and pump the mixture to the nano Filter press, press filter and wash 5 times, send the filter cake to a vacuum dryer, dry at 80°C, -0.08MPa, and dry the dried nano-FeC 2 o 4 2H 2 O is sent to a closed secondary dehydrator filled with xylene through a screw conveyor. At 95-140°C and -0.1MPa, use the azeotropy of xylene and water to remove crystal water during the process of removing xylene. Compared with the conventional thermal decomposition decrystallization water process, ...

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Abstract

The invention discloses a production technique for nanometer anhydrous ferrous oxalate. The production technique comprises two characteristic technological processes: 1) preparing nanometer ferrous oxalate dihydrate by utilizing ferrous sulfate and oxalic acid; and 2) drying the nanometer ferrous oxalate dihydrate and removing crystal water, thereby obtaining the nanometer anhydrous ferrous oxalate. The production technique is energy-saving and environment-friendly; the energy consumption is about 20% lower than that of a common crystal water removing method; the grain size of the obtained nanometer anhydrous ferrous oxalate is 10-100nm; the nanometer anhydrous ferrous oxalate has unique properties of a nanometer material, including high specific surface area, quantum size effect, small size effect, and the like, is high in purity and can be applied to the production of a lithium iron phosphate battery material.

Description

technical field [0001] The invention relates to the technical field of energy storage materials, in particular to a production process of nano-scale anhydrous ferrous oxalate, and the obtained nano-anhydrous ferrous oxalate can be used in the preparation of lithium iron phosphate cathode materials. Background technique [0002] Nanomaterials refer to materials with crystal, amorphous, quasicrystal and interface layer structures with any one-dimensional size less than 100nm. When the particle size is nanoscale, the material itself has surface and interface effects, quantum size effects, small size effects and macroscopic effects. Quantum tunneling effects, these effects make nanomaterials have many strange properties. Since Lijima prepared carbon nanotubes for the first time in 1991, one-dimensional nanomaterials have attracted widespread attention. Since 1991, the United States has listed nanotechnology as "government key technology". Various projects and research institut...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/60H01M10/0525
CPCH01M4/60H01M10/0525Y02E60/10
Inventor 滕鲲凡俊琳王群曹正祥
Owner 山东源来环保科技有限公司
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