CN103408417A - Preparation method for nanoscale ferrous oxalate - Google Patents
Preparation method for nanoscale ferrous oxalate Download PDFInfo
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Abstract
The invention relates to a preparation method for nanoscale ferrous oxalate. According to the method, ferrous sulfate is used as a raw material, and the product of nanoscale ferrous oxalate is finally obtained through raw material pre-treatment, and synthesis, washing, and drying of nanoscale ferrous oxalate. During the pre-treatment, purified iron powder, a suppressing agent, and an impurity precipitating agent are used to effectively transform iron ions into ferrous ions, and effectively remove impurity metal ions in the raw material; during the synthesis, a thickening agent is used to allow ferrous ions to be presented in the stable dispersion state in a solution; particularly during drying, spray drying is adopted, so that the particle size distribution area of a product is guaranteed to be smaller. The preparation method adopted by the invention is simple and convenient, easy to operate, and suitable for massive industrial production; prepared ferrous oxalate is nanoscale with small particle size distribution area, and has higher purity.
Description
Technical field
The present invention relates to a kind of fine chemical technology field, relate in particular to a kind of preparation method of nano level Ferrox.
Background technology
Lithium ion battery has become the most promising chemical power source at present.Positive electrode material is the key of lithium ion battery, and 1997, J.B.Goodenough found iron lithium phosphate LiFePO first
4In lithium ion have the reversibility that embeds/deviate from, can be used to the positive electrode material of lithium cell.LiFePO
4Have distinctive olivine structural, O and P be with the strong covalent bond mortise, and material is difficult to decompose, and structure and stable not there will be and explodes because of short circuit, and high-temperature behavior and thermal stability obviously are better than the positive electrode material that oneself know other; LiFePO
4Also have excellent cycle performance, discharge and recharge number of times up to more than 1000 times, in addition, LiFePO
4Production starting material wide material sources, cheap, nontoxic.So LiFePO
4Just becoming a kind of novel material that causes the revolution of lithium ion battery industry.
Ferrox, chemical name is the oxalic acid ferrous iron, one of starting material of synthesizing lithium ion battery anode active compound lithium iron phosphate, its purity and particle diameter are most important to the performance of the performance of iron lithium phosphate, because electronics, the ionic conductivity of iron lithium phosphate are very low, solve the low effective ways of ionic conductivity and reduce exactly grain diameter, therefore adopting the Ferrox that particle diameter is little is raw material, can effectively control the particle diameter of iron lithium phosphate.The size of Ferrox also can affect the homogeneity of batch mixing in addition, and particle is less, more is conducive to batch mixing even.Therefore, high, the nanometer particle size of synthetic purity and uniformly Ferrox be the developing direction of production technology.
Summary of the invention
For solving the problem existed in prior art and preparation method, the object of the present invention is to provide the preparation method that the nano level Ferrox that a kind of particle size distribution range is little is provided.
The technical solution adopted in the present invention:
A kind of preparation method of nano level Ferrox comprises the following steps:
(1) pre-treatment of raw material sulphuric acid ferrous iron
The ferrous stainless steel that drops into of raw material sulphuric acid is washed in still, with after the abundant washing and filtering of deionized water, iron powder is reclaimed, ferrous sulfate is moved in the enamel dissolution kettle;
Ferrous sulfate in the enamel dissolution kettle is added to deionized water fully to be dissolved, add again pure iron powder, inhibitor and contamination precipitation agent, regulator solution pH value is 1～4, standingly after fully stirring clarify to solution, proceed in the enamel synthesis reactor ferrous sulfate clear liquor on upper strata standby, the add-on of iron powder is 1%～2% of ferrous sulfate quality, and the add-on of inhibitor is 0.5%～5% of ferrous sulfate quality, and the add-on of contamination precipitation agent is 1%～10% of ferrous sulfate quality;
(2) the nano level Ferrox is synthetic
To 100%～300% the deionized water that adds the precipitation agent quality in precipitation agent, stir and progressively be warming up to 70～90 ℃ standby;
Thickening material is added in the ferrous sulfate clear liquor, stirs and progressively be warming up to 70～90 ℃, the add-on of thickening material is 20%～40% of ferrous sulfate quality;
To heavy in the enamel synthesis reactor, add precipitant solution, precipitation agent and ferrous sulfate mol ratio be (0.6～1): 1, keep homo(io)thermism also to stir 0.5～2h, standing to precipitation fully after, recovery supernatant liquid, gained precipitate and are the nano level Ferrox;
(3) washing of nano level Ferrox
By the nano level Ferrox of gained, after adding deionized water and stirring 3～5min, standing rear filtering separation, repetitive scrubbing is to the check of the barium chloride solution with massfraction 20%～30% nothing precipitation;
(4) drying of nano level Ferrox
Nano level Ferrox after washing is carried out to drying, and gained is the nano level Ferrox.
Inhibitor in step (1) is at least a in monose, oligosaccharides, polysaccharide, polyvalent alcohol.
Contamination precipitation agent in step (1) is at least a in ammoniacal liquor or carbonic acid ammonia or sodium carbonate or sodium bicarbonate or salt of wormwood or saleratus.
Precipitation agent in step (2) is at least a in oxalic acid or oxalic acid ammonia or sodium oxalate or potassium oxalate.
Thickening material in step (2) is at least a in monose or oligosaccharides or polysaccharide or polyvalent alcohol or starch.
The inlet air temperature of the spray-dired arid region in step (4) is 150～450 ℃.
The pressure of the spray-dired arid region in step (4) is-50～-200Nm
-2.
The temperature of the spray-dired dried nano level Ferrox in step (4) is 50～150 ℃.
Beneficial effect of the present invention:
The present invention, when pre-treatment, uses iron powder, inhibitor and contamination precipitation agent, effectively iron ion is converted into to ferrous ion, and has effectively removed the foreign metal ion in the raw material; When synthetic, use thickening material to make ferrous ion in solution, be the stable dispersion state; When drying, select spraying drying, guaranteed that the nanometer particle size of product and distribution range are less.Preparation method of the present invention is easy, easy to operate, is suitable for suitability for industrialized production, and prepared Ferrox is the nano level Ferrox.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment mono-
A kind of preparation method of nano level Ferrox comprises the following steps:
(1) pre-treatment of raw material sulphuric acid ferrous iron
The ferrous stainless steel that drops into of raw material sulphuric acid is washed in still, with after the abundant washing and filtering of deionized water, iron powder is reclaimed, ferrous sulfate is proceeded in the enamel dissolution kettle, ferrous sulfate in the enamel dissolution kettle is added to deionized water dissolving, add again iron powder, oligosaccharides and carbonic acid ammonia, using sulfuric acid or ammoniacal liquor regulator solution pH value is 3, standingly after fully stirring clarify to solution, proceed in the enamel synthesis reactor ferrous sulfate clear liquor on upper strata standby, the add-on of iron powder is 1% of ferrous sulfate quality, the add-on of oligosaccharides is 3% of ferrous sulfate quality, the add-on of carbonic acid ammonia is 5% of ferrous sulfate quality,
(2) the nano level Ferrox is synthetic
In oxalic acid, add deionized water, stir and progressively be warming up to 70 ℃, the add-on of deionized water is 100% of oxalic acid quality; In the enamel synthesis reactor that fills the ferrous sulfate clear liquor, add oligosaccharides, stir and progressively be warming up to 70 ℃, the add-on of oligosaccharides is 20% of ferrous sulfate quality; To heavy in the enamel synthesis reactor, add oxalic acid solution, oxalic acid and ferrous sulfate mol ratio are 0.6: 1, keep homo(io)thermism also to stir 2h, standing to precipitation fully after, reclaim supernatant liquid, gained precipitates and is the nano level Ferrox;
(3) washing of nano level Ferrox
By the nano level Ferrox of gained, after adding deionized water and stirring 5min, standing rear filtering separation, repetitive scrubbing is to the check of the barium chloride solution with massfraction 30% nothing precipitation;
(4) drying of nano level Ferrox
Nano level Ferrox after washing is carried out to drying, and the inlet air temperature of arid region is 450 ℃, and the pressure of arid region is-50Nm
-2, the temperature of the nano level Ferrox of dry rear gained is 150 ℃.
Embodiment bis-
A kind of preparation method of nano level Ferrox comprises the following steps:
(1) pre-treatment of raw material sulphuric acid ferrous iron
The ferrous stainless steel that drops into of raw material sulphuric acid is washed in still, with after the abundant washing and filtering of deionized water, iron powder is reclaimed, ferrous sulfate is proceeded in the enamel dissolution kettle simultaneously, ferrous sulfate in the enamel dissolution kettle is added to deionized water dissolving, add again iron powder, monose and ammoniacal liquor, using acetic acid or sodium hydrate regulator solution pH value is 4, standingly after fully stirring clarify to solution, proceed in the enamel synthesis reactor ferrous sulfate clear liquor on upper strata standby, the add-on of iron powder is 2% of ferrous sulfate quality, the add-on of monose is 3% of ferrous sulfate quality, the add-on of ammoniacal liquor is 6% of ferrous sulfate quality,
(2) the nano level Ferrox is synthetic
In oxalic acid ammonia, add deionized water, stir and progressively be warming up to 80 ℃, the add-on of deionized water is 300% of oxalic acid ammonia quality; In the enamel synthesis reactor that fills the ferrous sulfate clear liquor, add polyvalent alcohol, stir and progressively be warming up to 80 ℃, the add-on of polyvalent alcohol is 40% of ferrous sulfate quality; To heavy in the enamel synthesis reactor, add the oxalic acid ammonia solution, oxalic acid ammonia and ferrous sulfate mol ratio are 1: 1, keep homo(io)thermism also to stir 0.5h, standing to precipitation fully after, reclaim supernatant liquid, gained precipitates and is the nano level Ferrox;
(3) washing of nano level Ferrox
By the Ferrox of gained, after adding deionized water and stirring 3min, standing rear filtering separation, repetitive scrubbing is to the check of the barium chloride solution with massfraction 10% nothing precipitation;
(4) drying of nano level Ferrox
Nano level Ferrox after washing is carried out to drying, and the inlet air temperature of arid region is 150 ℃, and the pressure of arid region is-200Nm
-2, after drying, obtaining temperature is 50 ℃.The nano level Ferrox.
Embodiment tri-
A kind of preparation method of nano level Ferrox comprises the following steps:
(1) pre-treatment of raw material sulphuric acid ferrous iron
The ferrous stainless steel that drops into of raw material sulphuric acid is washed in still, with after the abundant washing and filtering of deionized water, iron powder is reclaimed, ferrous sulfate is proceeded in the enamel dissolution kettle, ferrous sulfate in the enamel dissolution kettle is added to deionized water dissolving, add again iron powder, polysaccharide and sodium carbonate, using sulfuric acid or potassium hydroxide regulator solution pH value is 1, standingly after fully stirring clarify to solution, proceed in the enamel synthesis reactor ferrous sulfate clear liquor on upper strata standby, the add-on of iron powder is 1% of ferrous sulfate quality, the add-on of polysaccharide is 0.5% of ferrous sulfate quality, the add-on of sodium carbonate is 10% of ferrous sulfate quality,
(2) the nano level Ferrox is synthetic
In sodium oxalate, add deionized water, stir and progressively be warming up to 90 ℃, the add-on of deionized water is 200% of sodium oxalate quality; In the enamel synthesis reactor that fills the ferrous sulfate clear liquor, add thickening material, stir and progressively be warming up to 90 ℃, the add-on of thickening material is 30% of ferrous sulfate quality; To heavy in the enamel synthesis reactor, add sodium oxalate solution, sodium oxalate and ferrous sulfate mol ratio are 0.8: 1, keep homo(io)thermism also to stir 1h, standing to precipitation fully after, reclaim supernatant liquid, gained precipitates and is the nano level Ferrox;
(3) washing of nano level Ferrox
By the nano level Ferrox of gained, after adding deionized water and stirring 4min, standing rear filtering separation, repetitive scrubbing is to the check of the barium chloride solution with massfraction 20% nothing precipitation;
(4) drying of nano level Ferrox
Nano level Ferrox after washing is carried out to drying, and the inlet air temperature of arid region is 300 ℃, and the pressure of arid region is-100Nm
-2, dry rear gained temperature is the nano level Ferrox of 100 ℃.
Embodiment tetra-
A kind of preparation method of nano level Ferrox comprises the following steps:
(1) pre-treatment of raw material sulphuric acid ferrous iron
The ferrous stainless steel that drops into of raw material sulphuric acid is washed in still, with after the abundant washing and filtering of deionized water, iron powder is reclaimed, ferrous sulfate is proceeded in the enamel dissolution kettle, ferrous sulfate in the enamel dissolution kettle is added to deionized water dissolving, add again iron powder, monose and ammoniacal liquor, using sulfuric acid or ammoniacal liquor regulator solution pH value is 2, standingly after fully stirring clarify to solution, proceed in the enamel synthesis reactor ferrous sulfate clear liquor on upper strata standby, the add-on of iron powder is 2% of ferrous sulfate quality, the add-on of monose is 5% of ferrous sulfate quality, the add-on of ammoniacal liquor is 1% of ferrous sulfate quality,
(2) the nano level Ferrox is synthetic
In potassium oxalate, add deionized water, stir and progressively be warming up to 80 ℃, the add-on of deionized water is 200% of potassium oxalate quality; In the enamel synthesis reactor that fills the ferrous sulfate clear liquor, add polysaccharide, stir and progressively be warming up to 80 ℃, the add-on of polysaccharide is 20% of ferrous sulfate quality; To heavy in the enamel synthesis reactor, add Potassium Oxalate Solution, potassium oxalate and ferrous sulfate mol ratio are 0.6: 1, keep homo(io)thermism also to stir 2h, standing to precipitation fully after, reclaim supernatant liquid, gained precipitates and is the nano level Ferrox;
(3) washing of nano level Ferrox
By the nano level Ferrox of gained, after adding deionized water and stirring 5min, standing rear filtering separation, repetitive scrubbing is to the check of the barium chloride solution with massfraction 10% nothing precipitation;
(4) drying of nano level Ferrox
Nano level Ferrox after washing is carried out to drying, and the inlet air temperature of arid region is 200 ℃, and the pressure of arid region is-150Nm
-2, the temperature of the nano level Ferrox of dry rear gained is 100 ℃.
Embodiment five
A kind of preparation method of nanometer ferrous sulfate comprises the following steps:
(1) pre-treatment of raw material sulphuric acid ferrous iron
The ferrous stainless steel that drops into of raw material sulphuric acid is washed in still, with after the abundant washing and filtering of deionized water, iron powder is reclaimed, ferrous sulfate is proceeded in the enamel dissolution kettle, ferrous sulfate in the enamel dissolution kettle is added to deionized water dissolving, add again iron powder, polyvalent alcohol and salt of wormwood, using acetic acid or sodium hydrate regulator solution pH value is 4, standingly after fully stirring clarify to solution, proceed in the enamel synthesis reactor ferrous sulfate clear liquor on upper strata standby, the add-on of iron powder is 1% of ferrous sulfate quality, the add-on of polyvalent alcohol is 4% of ferrous sulfate quality, the add-on of salt of wormwood is 3% of ferrous sulfate quality,
(2) the nano level Ferrox is synthetic
In sodium oxalate, add deionized water, stir and progressively be warming up to 70 ℃, the add-on of deionized water is 150% of sodium oxalate quality; In the enamel synthesis reactor that fills the ferrous sulfate clear liquor, add oligosaccharides, stir and progressively be warming up to 70 ℃, the add-on of oligosaccharides is 30% of ferrous sulfate quality; To heavy in the enamel synthesis reactor, add sodium oxalate solution, sodium oxalate and ferrous sulfate mol ratio are 0.7: 1, keep homo(io)thermism also to stir 1.5h, standing to precipitation fully after, reclaim supernatant liquid, gained precipitates and is the nano level Ferrox;
(3) washing of nano level Ferrox
By the nano level Ferrox of gained, after adding deionized water and stirring 3min, standing rear filtering separation, repetitive scrubbing is to the check of the barium chloride solution with massfraction 20% nothing precipitation;
(4) drying of nano level Ferrox
Nano level Ferrox after washing is carried out to drying, and the inlet air temperature of arid region is 400 ℃, and the pressure of arid region is-150Nm
-2, the temperature of the nano level Ferrox of dry rear gained is 150 ℃.
Embodiment six
A kind of preparation method of nanometer ferrous sulfate comprises the following steps:
(1) pre-treatment of raw material sulphuric acid ferrous iron
The ferrous stainless steel that drops into of raw material sulphuric acid is washed in still, with after the abundant washing and filtering of deionized water, iron powder is reclaimed, ferrous sulfate is proceeded in the enamel dissolution kettle, ferrous sulfate in the enamel dissolution kettle is added to deionized water dissolving, add again iron powder, monose and sodium bicarbonate, using sulfuric acid or regulator solution pH value is 2, standingly after fully stirring clarify to solution, proceed in the enamel synthesis reactor ferrous sulfate clear liquor on upper strata standby, the add-on of iron powder is 1% of ferrous sulfate quality, the add-on of monose is 3% of ferrous sulfate quality, the add-on of sodium bicarbonate is 5% of ferrous sulfate quality,
(2) the nano level Ferrox is synthetic
In oxalic acid, add deionized water, stir and progressively be warming up to 80 ℃, the add-on of deionized water is 100% of oxalic acid quality; In the enamel synthesis reactor that fills the ferrous sulfate clear liquor, add monose, stir and progressively be warming up to 70 ℃, the add-on of monose is 40% of ferrous sulfate quality; To heavy in the enamel synthesis reactor, add oxalic acid solution, oxalic acid and ferrous sulfate mol ratio are 0.9: 1, keep homo(io)thermism also to stir 0.5h, standing to precipitation fully after, reclaim supernatant liquid, gained precipitates and is the nano level Ferrox;
(3) washing of nano level Ferrox
By the nano level Ferrox of gained, after adding deionized water and stirring 3min, standing rear filtering separation, repetitive scrubbing is to the check of the barium chloride solution with massfraction 30% nothing precipitation;
(4) drying of nano level Ferrox
Nano level Ferrox after washing is carried out to drying, and the inlet air temperature of arid region is 250 ℃, and the pressure of arid region is-100Nm
-2, dry temperature is the nano level Ferrox of 100 ℃.
Claims (8)
1. the preparation method of a nano level Ferrox is characterized in that: comprise the following steps:
(1) pre-treatment of raw material sulphuric acid ferrous iron
The ferrous stainless steel that drops into of raw material sulphuric acid is washed in still, with after the abundant washing and filtering of deionized water, iron powder is reclaimed, ferrous sulfate is moved in the enamel dissolution kettle;
Ferrous sulfate in the enamel dissolution kettle is added to deionized water fully to be dissolved, add again pure iron powder, inhibitor and contamination precipitation agent, regulator solution pH value is 1～4, standingly after fully stirring clarify to solution, proceed in the enamel synthesis reactor ferrous sulfate clear liquor on upper strata standby, the add-on of iron powder is 1%～2% of ferrous sulfate quality, and the add-on of inhibitor is 0.5%～5% of ferrous sulfate quality, and the add-on of contamination precipitation agent is 1%～10% of ferrous sulfate quality;
(2) the nano level Ferrox is synthetic
To the deionized water that adds precipitation agent quality 100%～300% in precipitation agent, stir and progressively be warming up to 70～90 ℃ standby;
Thickening material is added in the ferrous sulfate clear liquor, stirs and progressively be warming up to 70～90 ℃, the add-on of thickening material is 20%～40% of ferrous sulfate quality;
In the enamel synthesis reactor, add precipitant solution, precipitation agent and ferrous sulfate mol ratio are (0.6～1): 1, and keep homo(io)thermism and stir 0.5～2h, after standing extremely precipitation is complete, reclaim supernatant liquid, the gained precipitation is the nano level Ferrox;
(3) washing of nano level Ferrox
By the nano level Ferrox of gained, after adding deionized water and stirring 3～5min, standing rear filtering separation, repetitive scrubbing is to the check of the barium chloride solution with massfraction 20%～30% nothing precipitation;
(4) drying of nano level Ferrox
Nano level Ferrox after washing is carried out to drying, and gained is the nano level Ferrox.
2. the preparation method of nanometer ferrous sulfate according to claim 1 is characterized in that: the inhibitor in described step (1) is at least a in monose, oligosaccharides, polysaccharide, polyvalent alcohol.
3. the preparation method of nano level Ferrox according to claim 1 is characterized in that: the contamination precipitation agent in described step (1) is at least a in ammoniacal liquor, carbonic acid ammonia, sodium carbonate, sodium bicarbonate, salt of wormwood, saleratus.
4. the preparation method of nanometer ferrous sulfate according to claim 1 is characterized in that: the precipitation agent in described step (2) is at least a in oxalic acid, oxalic acid ammonia, sodium oxalate, potassium oxalate.
5. the preparation method of nanometer ferrous sulfate according to claim 1 is characterized in that: the thickening material in described step (2) is at least a in monose, oligosaccharides, polysaccharide, polyvalent alcohol, starch.
6. the preparation method of nanometer ferrous sulfate according to claim 1, it is characterized in that: the inlet air temperature of the spray-dired arid region in described step (4) is 150～450 ℃.
7. the preparation method of nanometer ferrous sulfate according to claim 1 is characterized in that: the pressure of the spray-dired arid region in described step (4) is-50～-200Nm
-2.
8. the preparation method of nanometer ferrous sulfate according to claim 1, it is characterized in that: the temperature of the nano level Ferrox after the spraying drying in described step (4) is 50～150 ℃.
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Cited By (1)
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Application publication date: 20131127 |