CN106356532B - A kind of production technology of nanoscale anhydrous oxalic acid ferrous iron - Google Patents
A kind of production technology of nanoscale anhydrous oxalic acid ferrous iron Download PDFInfo
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- CN106356532B CN106356532B CN201610911870.3A CN201610911870A CN106356532B CN 106356532 B CN106356532 B CN 106356532B CN 201610911870 A CN201610911870 A CN 201610911870A CN 106356532 B CN106356532 B CN 106356532B
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- oxalic acid
- deflocculant
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- ferrous
- anhydrous oxalic
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of production technologies of nanoscale anhydrous oxalic acid ferrous iron, including two feature process flows：First, producing nanoscale ferrous oxalate dihydrate by ferrous sulfate and oxalic acid；Crystallization water production nanometer anhydrous oxalic acid ferrous iron is taken off second is that being dried by nanometer ferrous oxalate dihydrate.Energy conservation and environmental protection, energy consumption save 20% or so than commonly de- crystallization water method.The granule size of obtained nanometer anhydrous oxalic acid ferrous iron is 10~100nm, has high-specific surface area, quantum size effect, and the special performance of the nano materials such as small-size effect, purity is high, can be applied to production lithium iron phosphate cell material.
Description
Technical field
The present invention relates to energy storage material technical fields, more particularly to a kind of production work of nanoscale anhydrous oxalic acid ferrous iron
Skill, the nanometer anhydrous oxalic acid ferrous iron of gained can be used for the preparation of lithium iron phosphate positive material.
Background technology
Nano material refers to the material of arbitrary crystal of the one-dimensional size less than 100nm, noncrystal, quasicrystal and interface structure
Material, when particle size is nanoscale, material itself have surface and interfacial effect, quantum size effect, small-size effect and
Macro quanta tunnel effect, these effects make nano material have many peculiar performances.Lijima is prepared for for the first time since 1991
Since carbon nanotube, monodimension nanometer material causes the extensive concern of people.From 1991, nanotechnology is classified as " political affairs by the U.S.
Mansion key technology ".Nano material and nanotechnology are classified as weight by the various projects such as the Natural Science Fund In The Light of China and research institution
Point research project.The preparation method of nano material usually has two kinds of Physical and chemical method.But it up to the present, developed
Nanometer product and nanotechnology industrialization relatively difficult to achieve, commercial scale.
Lithium ion battery is rechargeable battery with fastest developing speed in recent years, compared with other accumulators (such as with Ni-MH battery,
Nickel-cadmium cell, lead-acid battery etc.), due to lithium ion battery specific capacity height, good cycle, that pollution-free, self-discharge rate is low etc. is excellent
Point has captured the market share in battery of mobile phone, cells in notebook computer field with overwhelming dominance at present.To lithium ion battery
Speech, main composition material includes electrolyte, isolation film, positive and negative pole material etc..In general, in lithium ion battery product form
In ingredient, positive electrode directly determines final secondary cell product in occupation of most important status, the quality of positive electrode
Performance indicator.Positive electrode proportion in battery cost is up to 40% or more.1997, Goodenough was reported for the first time
LiFePO4 (the LiFePO of olivine-type4) it can be used for anode material for lithium-ion batteries.In recent years, from safety and battery cost angle
Degree considers, generally believes LiFePO in the world4It is the best novel anode material of high-energy power battery.LiFePO4, which is used as, most to be had
Wish the anode material of lithium battery applied on high-power power battery, have extra long life, it is safe to use, can be in high current condition
Lower progress fast charging and discharging, high temperature resistant, large capacity, memory-less effect, it is environmentally protective the advantages that.Lithium iron phosphate dynamic battery and its
He compares battery, also has the advantages that be a kind of almost green electricity free from environmental pollution without the poisonous and harmful elements such as lead, cadmium
Pond.
Although the preparation method of LiFePO4 has high temperature solid-state method, hydro-thermal method, microwave method, sol-gel method, coprecipitation
Etc. many kinds, but due to liquid phase method generate the bad processing of industrial wastes, cause material cost to be substantially increased, microwave method can not
Realize large-scale production, therefore in the preparation method of LiFePO4, high temperature solid-state method is still mainstream.But high temperature solid-state method,
Bigger using grain size, the higher Material synthesis of fusing point LiFePO4 actual capacity is lower.The theoretically situation identical in grain size
Under, source of iron is had the following advantages using ferrous oxalate compared with other sources of iron：
1) it is not easily introduced impurity phase in positive electrode building-up process, because ferrous oxalate will produce also in roasting process
Originality gas CO.
2) the lithium iron phosphate positive material crystallinity of ferrous oxalate synthesis is high, bonding force is big, helps to stablize synthetic product
Skeleton structure.
3) ferrous oxalate decomposable process releases gas, and particle agglomeration and crystal grain can be inhibited to grow up.
Chen Hongyan uses the FeC of different-grain diameter2O4·2H2O synthesizing iron lithium phosphates, grain size difference charge and discharge specific volume and efficiency
Also different, grain size is smaller, and electrical property is better.
Therefore positive raw material ferrous oxalate nanosizing, homogenization can significantly improve the charge/discharge capacity of positive electrode and steady
It is qualitative.
The research of Tang Wanjun etc. finds FeC2O4·2H2The thermal decomposition of O is carried out in two steps, 170~200 DEG C of abjection crystallizations water,
200~300 DEG C are gradually oxidized to Fe2O3, it is 158.69KJ.mol to take off crystallization water activation energy-1.This means that the abjection crystallization water
Process need to consume a large amount of energy.
In conclusion preparing, nanoscale anhydrous oxalic acid is ferrous and improve production technology, preparation to LiFePO4 and
The reduction of energy consumption is all of practical significance.
Invention content
The purpose of the present invention provides a kind of production of nanoscale anhydrous oxalic acid ferrous iron aiming at above-mentioned defect
Technique, including two feature process flows：First, producing nanoscale ferrous oxalate dihydrate by ferrous sulfate and oxalic acid；Second is that by receiving
It is ferrous that rice ferrous oxalate dihydrate drying takes off crystallization water production nanometer anhydrous oxalic acid.Energy conservation and environmental protection, energy consumption is than commonly de- crystallization water side
Method saves 20% or so.The granule size of obtained nanometer anhydrous oxalic acid ferrous iron be 10~100nm, have high-specific surface area,
Quantum size effect, the special performance of the nano materials such as small-size effect, purity is high, can be applied to production ferric phosphate lithium cell
Material.
A kind of production Technology scheme of nanoscale anhydrous oxalic acid ferrous iron of the present invention is, including following technological process：
(1) nanoscale ferrous oxalate dihydrate is produced by ferrous sulfate and oxalic acid, while sulfuric acid and deflocculant is added；
(2) by nanometer ferrous oxalate dihydrate by taking off crystallization water preparation with de- crystallization aqueous solvent azeotropic in vacuum environment and receiving
Rice anhydrous oxalic acid is ferrous.
The mass concentration of sulfuric acid is 10~50% in step (1).
Deflocculant is made of deflocculant A and deflocculant B in step (1), and wherein deflocculant A is polyphosphazene polymer
Ether, deflocculant B are alkylsulfonates.
The addition of deflocculant A is the 0.01~1% of ferrous sulfate quality, and the addition of deflocculant B is that sulfuric acid is sub-
The 0.04~4% of weight of iron.
The molar ratio of deflocculant A and deflocculant B is 1:4~4:1.
In step (2), it is dimethylbenzene and water to take off crystallization aqueous solvent, and the dimethylbenzene is ortho-xylene, meta-xylene, right
At least one of dimethylbenzene.
De- crystallization aqueous solvent is dimethylbenzene 62.5~100% by mass percent, and water 0~37.5% forms.
Nanoscale anhydrous oxalic acid ferrous iron particle size is 10~100nm.
By ferrous sulfate, the solution 1 of sulfuric acid, water composition, the solution 2 of the aqueous solution composition containing oxalic acid is according to weight ratio 1:1
Ratio mixing, while deflocculant A and deflocculant B is added, wherein deflocculant A is high molecular polyether, and deflocculant B is
Alkylsulfonate, stirring is warming up to 90 DEG C, and keeps the temperature 3 hours in 90 DEG C, 60 DEG C is cooled to after reaction, by mixture press filtration
Washing, until FeC2O4·2H2Until O filter cakes pH6~7, filter cake is sent to vacuum desiccator, 30~80 DEG C, -0.1~-0.06MPa
Lower drying, by the nanometer Fe C after drying2O4·2H2O is at 95~140 DEG C, under -0.1~-0.06MPa, utilizes dimethylbenzene and water
Azeotropic removes the crystallization water during removing dimethylbenzene.
Mass ratio of each component is ferrous sulfate 20-40%, sulfuric acid 18-20%, water 40-62% in solution 1.
Solution 2 is the aqueous solution that mass percent containing oxalic acid is 14-30%.
Beneficial effects of the present invention are：A kind of production technology of nanoscale anhydrous oxalic acid ferrous iron of the present invention, including two
Feature process flow：First, producing nanoscale ferrous oxalate dihydrate by ferrous sulfate and oxalic acid；Second is that sub- by nanometer oxalic acid dihydrate
It is ferrous that iron drying takes off crystallization water production nanometer anhydrous oxalic acid.Present invention process energy conservation and environmental protection, energy consumption is than commonly de- crystallization water method
Save 20% or so.The granule size of obtained nanometer anhydrous oxalic acid ferrous iron is 10~100nm, has high-specific surface area, amount
Sub- dimensional effect, the special performance of the nano materials such as small-size effect, purity is high, can be applied to production ferric phosphate lithium cell material
Material.
Specific implementation mode：
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but this
Invention is not limited thereto.
Embodiment 1
Sulfur acid ferrous iron 25% is got out, the solution 1 of sulfuric acid 20%, water 55% (the above percentage is mass ratio) is placed in meter
Measuring tank 1；It gets out the aqueous solution ie in solution 2 containing oxalic acid 15% and is placed in measuring tank 2,4 tons of solution 1 and 4 tons of solution 2 are added to instead
Kettle to be answered, while 1 kilogram of deflocculant A and 2 kilograms of deflocculant B is added, stirring is warming up to 90 DEG C, and keeps the temperature 3 hours in 90 DEG C,
It is cooled to 60 DEG C after reaction, and mixture is pumped to a nanometer filter press, filter cake is sent to vacuum and done by pressure filtration washing 5 times
Dry device, it is 80 DEG C, dry under -0.08MPa, by the nanometer Fe C after drying2O4·2H2O is sent by screw conveyor to filling diformazan
The closed two level dewaterer of benzene under -0.1MPa, using the azeotropic of dimethylbenzene and water, removes the mistake of dimethylbenzene at 95~140 DEG C
The crystallization water is removed in journey.Compared with the de- crystallization hydraulic art of conventional thermal decomposition, present invention process energy saving 22%, product anhydrous oxalic acid
Ferrous purity 99.5%, grain size 20~80nm, single crowd of yield 900kg.
Embodiment 2
Sulfur acid ferrous iron 20% is got out, the solution 1 of sulfuric acid 18%, water 62% is placed in measuring tank 1；It is ready to contain oxalic acid
14% aqueous solution ie in solution 2 is placed in measuring tank 2,4 tons of solution 1 and 4 tons of solution 2 is added to reaction kettle, while being added 1 kilogram
Deflocculant A and 4 kilograms of deflocculant B, stirring is warming up to 90 DEG C, and keeps the temperature 3 hours in 90 DEG C, is cooled to 60 after reaction
DEG C, and mixture is pumped to a nanometer filter press, pressure filtration washing 5 times is sent filter cake to vacuum desiccator, 80 DEG C, -0.08MPa
Lower drying, by the nanometer Fe C after drying2O4·2H2O is sent by screw conveyor to the closed two level dewaterer for filling dimethylbenzene,
At 95~140 DEG C, under -0.1MPa, using the azeotropic of dimethylbenzene and water, the crystallization water is removed during removing dimethylbenzene.With it is normal
The de- crystallization hydraulic art of the thermal decomposition of rule is compared, present invention process energy saving 21%, product anhydrous oxalic acid ferrous iron purity 99.6%, grain size
10~60nm, single crowd of yield 705kg.
Embodiment 3
Sulfur acid ferrous iron 30% is got out, the solution 1 of sulfuric acid 20%, water 50% is placed in measuring tank 1；It is ready to contain oxalic acid
20% aqueous solution 2 is placed in measuring tank 2,4 tons of solution As and 4 tons of solution Bs is added to reaction kettle, while 4 kilograms of deflocculations are added
Agent A and 1 kilogram of deflocculant B, stirring are warming up to 90 DEG C, and keep the temperature 3 hours in 90 DEG C, are cooled to 60 DEG C after reaction, and
Mixture is pumped to a nanometer filter press, pressure filtration washing 5 times is sent filter cake to vacuum desiccator, 80 DEG C, is done under -0.08MPa
It is dry, by the nanometer Fe C after drying2O4·2H2O is sent by screw conveyor to the closed two level dewaterer for filling dimethylbenzene, 95
~140 DEG C, under -0.1MPa, using the azeotropic of dimethylbenzene and water, the crystallization water is removed during removing dimethylbenzene.With routine
The de- crystallization hydraulic art of thermal decomposition is compared, present invention process energy saving 25%, product anhydrous oxalic acid ferrous iron purity 99.5%, and grain size 20~
50nm, single crowd of yield 1085kg.
Embodiment 4
Sulfur acid ferrous iron 40% is got out, the solution 1 of sulfuric acid 20%, water 40% is placed in measuring tank 1；It is ready to contain oxalic acid
30% aqueous solution 2 is placed in measuring tank 2,4 tons of solution As and 4 tons of solution Bs is added to reaction kettle, while 3 kilograms of deflocculations are added
Agent A and 2 kilograms of deflocculant B, stirring are warming up to 90 DEG C, and keep the temperature 3 hours in 90 DEG C, are cooled to 60 DEG C after reaction, and
Mixture is pumped to a nanometer filter press, pressure filtration washing 5 times is sent filter cake to vacuum desiccator, 80 DEG C, is done under -0.08MPa
It is dry, by the nanometer Fe C after drying2O4·2H2O is sent by screw conveyor to the closed two level dewaterer for filling dimethylbenzene, 95
~140 DEG C, under -0.1MPa, using the azeotropic of dimethylbenzene and water, the crystallization water is removed during removing dimethylbenzene.With routine
The de- crystallization hydraulic art of thermal decomposition is compared, present invention process energy saving 20%, product anhydrous oxalic acid ferrous iron purity 99.6%, and grain size 30~
70nm, single crowd of yield 1440kg.
Claims (8)
1. a kind of production technology of nanoscale anhydrous oxalic acid ferrous iron, which is characterized in that including following technological process：
（1）Nanoscale ferrous oxalate dihydrate is produced by ferrous sulfate and oxalic acid, while sulfuric acid and deflocculant is added；
（2）By nanometer ferrous oxalate dihydrate by taking off the crystallization water with de- crystallization aqueous solvent azeotropic in vacuum environment and preparing nanometer nothing
Water ferrous oxalate；
Step（1）Middle deflocculant is made of deflocculant A and deflocculant B, and wherein deflocculant A is high molecular polyether, is resisted
Flocculating agent B is alkylsulfonate；
Step（2）In, it is dimethylbenzene or dimethylbenzene and water to take off crystallization aqueous solvent, and the dimethylbenzene is ortho-xylene, diformazan
At least one of benzene, paraxylene.
2. a kind of production technology of nanoscale anhydrous oxalic acid ferrous iron according to claim 1, which is characterized in that step（1）
The mass concentration of middle sulfuric acid is 10 ~ 50%.
3. a kind of production technology of nanoscale anhydrous oxalic acid ferrous iron according to claim 1, which is characterized in that deflocculant
The addition of A is the 0.01 ~ 1% of ferrous sulfate quality, and the addition of deflocculant B is the 0.04 ~ 4% of ferrous sulfate quality.
4. a kind of production technology of nanoscale anhydrous oxalic acid ferrous iron according to claim 1, which is characterized in that deflocculant
The molar ratio of A and deflocculant B is 1:4~4:1.
5. a kind of production technology of nanoscale anhydrous oxalic acid ferrous iron according to claim 1, which is characterized in that the de- crystallization water
Solvent is dimethylbenzene 62.5 ~ 100% by mass percent, and water 0 ~ 37.5% forms.
6. a kind of production technology of nanoscale anhydrous oxalic acid ferrous iron according to claim 1, which is characterized in that nanoscale
Anhydrous oxalic acid ferrous iron particle size is 10 ~ 100nm.
7. a kind of production technology of nanoscale anhydrous oxalic acid ferrous iron according to claim 1, which is characterized in that by sulfuric acid Asia
The solution 1 of iron, sulfuric acid, water composition, the solution 2 of the aqueous solution composition containing oxalic acid is according to weight ratio 1:1 ratio mixing, adds simultaneously
Enter deflocculant A and deflocculant B, wherein deflocculant A is high molecular polyether, and deflocculant B is alkylsulfonate, and stirring rises
Temperature keeps the temperature 3 hours to 90 DEG C, and in 90 DEG C, 60 DEG C is cooled to after reaction, by mixture pressure filtration washing, until FeC2O4•2H2O
Until filter cake pH6 ~ 7, filter cake is sent to vacuum desiccator, 30 ~ 80 DEG C, it is dry under -0.1 ~ -0.06MPa, by the nanometer after drying
FeC2O4•2H2O is at 95 ~ 140 DEG C, under -0.1 ~ -0.06MPa, using the azeotropic of dimethylbenzene and water, during removing dimethylbenzene
Remove the crystallization water.
8. a kind of production technology of nanoscale anhydrous oxalic acid ferrous iron according to claim 7, which is characterized in that in solution 1
Mass ratio of each component is ferrous sulfate 20-40%, sulfuric acid 18-20%, water 40-62%；Solution 2 is that mass percent containing oxalic acid is 14-
30% aqueous solution.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101386575A (en) * | 2008-07-04 | 2009-03-18 | 合肥国轩高科动力能源有限公司 | Method for preparing iron oxalate |
| CN101580464A (en) * | 2009-07-07 | 2009-11-18 | 中南大学 | Method for producing battery-grade ferrous oxalate by using ferrous sulfate as titanium pigment byproduct |
| CN101948379A (en) * | 2010-09-01 | 2011-01-19 | 中国科学院宁波材料技术与工程研究所 | Method for preparing battery-level ferrous oxalate |
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2016
- 2016-10-19 CN CN201610911870.3A patent/CN106356532B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101386575A (en) * | 2008-07-04 | 2009-03-18 | 合肥国轩高科动力能源有限公司 | Method for preparing iron oxalate |
| CN101580464A (en) * | 2009-07-07 | 2009-11-18 | 中南大学 | Method for producing battery-grade ferrous oxalate by using ferrous sulfate as titanium pigment byproduct |
| CN101948379A (en) * | 2010-09-01 | 2011-01-19 | 中国科学院宁波材料技术与工程研究所 | Method for preparing battery-level ferrous oxalate |
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