CN106379877A - Continuous preparation device of iron phosphate - Google Patents
Continuous preparation device of iron phosphate Download PDFInfo
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- CN106379877A CN106379877A CN201611033719.0A CN201611033719A CN106379877A CN 106379877 A CN106379877 A CN 106379877A CN 201611033719 A CN201611033719 A CN 201611033719A CN 106379877 A CN106379877 A CN 106379877A
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- continuous
- phosphate
- reactor
- iron
- iron phosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a continuous preparation device of iron phosphate (See Figure 1). The continuous preparation device consists of a material cabin, a screw rod feeding device, continuous pipeline reactors, a water pump, a liquid metering material adding pump, a horizontal centrifugal machine and a pipeline. The continuous preparation device has a work process that ferric salts and phosphates are respectively added into the continuous pipeline reactor through the screw rod feeding device and are dissolved into solutions through water addition; the two kinds of solutions proportionally enter the continuous pipeline reactor 1 to take a reaction; in the continuous pipeline reactor 2, the pH is regulated to the neutral state; impurity ions are washed away through the horizontal centrifugal machine; iron phosphate solids are obtained. The continuous preparation device of iron phosphate materials has the advantages that continuous feeding and continuous discharging are realized; the reaction is stable and uniform.
Description
Technical field
The present invention relates to a kind of preparation facilitiess of industrial chemicals, the especially preparation facilitiess of iron phosphate, belong to chemical industry material
Material preparation field.
Background technology
Power lithium ion battery flourishes, and the volume of production of lithium iron phosphate positive material increases quick.LiFePO4
Raw material mostly be iron phosphate, the performance of iron phosphate is very crucial to the LiFePO4 performance of preparation.The main performance bag of iron phosphate
Include ferrum phosphorus ratio, pattern, primary particle size, bulk density, impurity content etc..The preparation method of iron phosphate have multiple, including
Sol-gal process, coprecipitation, mechanical and chemical activation method etc., wherein the more commonly used is coprecipitation, and main process is ferrum
Salt and additive make solution, and phosphate and additive make solution, both hybrid reactions, and adjust pH value and response speed with
And the mixing speed of liquid, iron ion and phosphate radical reaction generation precipitation, filter out precipitate, be neutralized washing and be dried to obtain
Iron phosphate material.
Patent CN200810026602.9 discloses a kind of high-density spherical iron phosphate and preparation method thereof, using co-precipitation
Method.The method is with source of iron and additive as raw material, makes mixed solution A with deionized water dissolving；With phosphate and nertralizer
For raw material, make mixed solution B with deionized water dissolving.A and B solution hybrid reaction, washed and dried to preparing material
Dry-cure, then can get 1.5～5 μm of mean diameter, tap density >=0.95g/cm3, granule dispersion, high density of uniform size
Ball shape ferric phosphate.
Patent CN201010278166.1 discloses a kind of preparation method of iron phosphate, comprises the following steps：Respectively by ferrum
Source, additive are configured to the solution that concentration is 1～3mol/L, are mixed into solution M；Respectively phosphate, nertralizer are configured to dense
Spend the solution for 1～3mol/L, be mixed into solution N；By M: N=1: two kinds of solution are added simultaneously to by the flow-rate ratio of (0.5～3)
In reaction vessel, control pH value 0.5～4.0, the precipitate that reaction generates washs 1～5 with the deionized water of 5～10 times of weight
Secondary, until pH value is more than 6.5；Filtered, filter cake is put in baking oven, baking 5～10 is little at a temperature of 90 DEG C～150 DEG C
When, you can obtain form of spherical particles iron phosphate.Present invention process flow process is simple, operation is few, can effectively control the average of product
Particle diameter in 1～10 μ m, tap density >=0.9g/cm3.
Patent CN201410522113.8 discloses a kind of preparation method of iron phosphate, and ferrous salt solution elder generation acid adding is adjusted by it
Section pH value, is then mixed homogeneously with phosphate mixt with phosphate solution or with phosphoric acid again, is subsequently adding oxidant and carries out instead
Iron phosphate should be generated.The iron phosphate of this invention overcomes the deficiency of existing iron phosphate preparation method well, mixing source of iron and
Just adjust the PH of source of iron before phosphorus source, do not need after mixing to add PH regulator to can reach the PH scope estimating needs, can
Avoid traditional method and produced such as Fe (OH) because alkaline PH regulator local is excessive3Deng impurity, the hydroxide of technical process iron-free
Thing produces, and the iron phosphate purity obtaining is high, removes further after foreign ion through follow-up, it is possible to obtain the iron phosphate of high-quality,
Purity more than 99.8%, stablize in 36.8%-37.2%, and phosphate content is stablized in 62.8%-63.2% by iron content.
Above-mentioned document all to prepare iron phosphate using coprecipitation although emphasis is different, but each for improving product
The stability of item index, does not but have effective means.And the stability of product indices, need the guarantee of process units.
Patent CN201020571412.8 discloses has homodisperse iron phosphate synthesis slurry device, holds including reaction
The relief hole that device and its bottom are provided with, is provided with stirring vane in its reaction vessel, is provided with the top of described stirring vane
It is partitioned into storage cavity and the material leakage disk of mixing chamber is connected with reaction vessel, radially the setting of the reaction vessel positioned at material leakage disk upper end
There is feed pipe.During application, different raw material liq, all add from different feed pipes respectively including alkali liquor, enter storing intracavity
Afterwards, exit into mixing chamber from material leakage disk.The liquid flowing into consumingly is stirred mixing by the agitator of high-speed rotation at once, is thrown to
Impingement mix is once more subjected on the inwall of mixing chamber, then runs down in container along inwall, complete the uniform mixing of slurry, have
Effect ensure that the homogenous material properties in iron phosphate building-up process are consistent.This device has only carried out dispersed in synthesis phase
Guarantee, at aspects such as feed stage, dissolution phase, course of reaction, morphology control, there is no support method.
The present invention is directed to coprecipitation iron phosphate technology of preparing, discloses a kind of new serialization preparation facilitiess, permissible
Effectively improve the stability of iron phosphate.
Content of the invention
The invention discloses a kind of continuous preparation device of iron phosphate (see Fig. 1), this device by feed bin, screw rod charge pump,
Continuous conduit reactor, water pump, liquid meter charge pump and horizontal centrifuge pipeline link together composition.Described water pump
For variable-frequency control pump, its water yield can continuously adjust, and described screw rod charge pump charging rate is continuously adjustable, described
The deflection plate of continuous conduit inside reactor can change different structural shapes.Its work process is：Soluble ferric iron salt is in material
Added in continuous conduit reactor A by screw rod charge pump 1 in storehouse 1, deionized water is injected in continuous conduit reactor A by water pump 1,
Iron salt flows while dissolving formation iron salt solutions in flow reactor；Soluble phosphate in feed bin 2 by screw rod plus
Material pump 2 adds in continuous conduit reactor B, and deionized water is injected in continuous conduit reactor B by water pump 2, and phosphate is continuous
Flow in pipeline reactor while dissolving formation phosphate solution；Iron salt solutions, phosphate solution continuously flow into simultaneously
Carry out reaction in continuous pipeline reactor 1 and generate phosphoric acid iron substance and its by-product, then flow into continuous conduit reactor 2, PH is adjusted
Agent is pumped in continuous conduit reactor 2 according to metered rate, and regulation pH value is predetermined value, and the pasty material separated enters
Horizontal centrifuge, washes away foreign ion, obtains iron phosphate.By the speed of adjusting screw rod charge pump 1 and screw rod charge pump 2, water
The charging rate of pump 1, water pump 2 and liquid meter charge pump, can control addition Fe, P ratio of material and the speed of reaction.
The advantage of the iron phosphate material preparation facilitiess of the present invention is continuous charging continuous discharge, stable reaction, uniformly, for
Specific index parameter can be by the flow velocity pumping into, and screw rod charge pump charging rate, PH regulator add speed, continuous conduit
In reactor, more bringing of deflection plate is accurately controlled, thus improving the stability of iron phosphate quality.
Brief description
Fig. 1 is the continuous preparation device figure of iron phosphate.
Fig. 2 is the installation drawing of the continuous preparation iron phosphate material being designed as source of iron using iron sulfate.
Fig. 3 is the deflection plate layout in continuous conduit reactor.
Specific embodiment
Embodiment 1
The iron sulfate selecting 96% content, as source of iron, selects 96% content NaH2PO4·2H2O as phosphate, with 20% ammonia
Water, as the regulator of pH value, designs the device (see Fig. 2) of a set of continuous preparation iron phosphate material.This device is by feed bin, screw rod
Charge pump, continuous conduit reactor, variable frequency pump, metering diaphragm charge pump, PH sensor, PLC and horizontal centrifuge composition.Should
The work process of device is：Iron sulfate is added in continuous conduit reactor A by screw rod charge pump in feed bin, and deionized water is by water
In pump 1 injection continuous conduit reactor A, form ferrum sulfuricum oxydatum solutum；Sodium phosphate is added continuous pipe by screw rod charge pump in feed bin
In road reactor B, deionized water is injected in continuous conduit reactor B by water pump 2, forms phosphate solution；Two kinds of solution are simultaneously
Flowed in continuous conduit reactor 1 with different in flow rate, carry out reaction and generate iron phosphate and its by-product, then flow into flow reactor
2, ammonia is pumped into by diaphragm metering pump and adjusts pH value in continuous conduit reactor 2 is 6, and the pasty material separated enters sleeping
Formula centrifuge, washes away foreign ion, and waste water is separated, and iron phosphate solid continues output.In all of continuous conduit reactor
Deflection plate layout (see Fig. 3).The charging rate of adjusting screw rod charge pump 1 and screw rod charge pump 2 is respectively 400g/h, 327g/
H, the water yield adjusting water pump 1 is 20L/h, and the water yield adjusting water pump 2 is 10L/h, the material of monitoring continuous conduit discharger 2
PH value is linked with microprocessor pump drive, when pH value is less than 6 increase amounts of pumping into, otherwise then reduces the amount of pumping into.By above measure control
The quality of iron phosphate processed, through detection, the Fe/P in iron phosphate is stable between 0.99～1.01.
Claims (3)
1. a kind of continuous preparation device of iron phosphate, is characterized in that, this device is by feed bin, screw rod charge pump, continuous conduit reaction
Device, water pump, liquid meter charge pump and horizontal centrifuge are connected and composed by pipeline.
2. a kind of continuous preparation device of iron phosphate according to claim 1, is characterized in that, soluble ferric iron salt is in feed bin 1
Middle added in continuous conduit reactor A by screw rod charge pump 1, deionized water by water pump 1 through pipeline inject continuous conduit reactor A
In, iron salt flows in flow reactor and dissolves formation iron salt solutions；Soluble phosphate is in feed bin 2 by screw rod
Charge pump 2 adds in continuous conduit reactor B, and deionized water is injected in continuous conduit reactor B by water pump 2, and phosphate is even
Flow in continuous pipeline reactor while dissolving formation phosphate solution；Iron salt solutions, phosphate solution continuously flow into simultaneously
Carry out reaction in continuous conduit reactor 1 and generate phosphoric acid iron substance and its by-product, then flow into continuous conduit reactor 2, PH adjusts
Section agent is pumped in continuous conduit reactor 2 according to metered rate, and regulation pH value is predetermined value, and the pasty material separated enters
Enter horizontal centrifuge, wash away foreign ion, obtain iron phosphate.
3. a kind of continuous preparation device of iron phosphate according to claim 1, is characterized in that, screw rod charge pump charging rate
It is continuously adjustable, water pump is variable-frequency control pump, and the charging rate of liquid meter charge pump is adjustable.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521094802X | 2015-12-27 | ||
| CN201521094802 | 2015-12-27 |
Publications (1)
| Publication Number | Publication Date |
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| CN106379877A true CN106379877A (en) | 2017-02-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611033719.0A Pending CN106379877A (en) | 2015-12-27 | 2016-11-15 | Continuous preparation device of iron phosphate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809380A (en) * | 2019-03-06 | 2019-05-28 | 深圳海纳百川科技有限公司 | A kind of technique and device of ferrous solution synthesis |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102303858A (en) * | 2011-07-20 | 2012-01-04 | 彩虹集团公司 | Preparation method of nanoscale ferric phosphate for lithium iron phosphate |
| CN202529847U (en) * | 2012-04-06 | 2012-11-14 | 中国电子科技集团公司第十八研究所 | Ferric pyrophosphate powder preparation system with controllable particle size |
| CN203781852U (en) * | 2014-03-17 | 2014-08-20 | 江苏华东锂电技术研究院有限公司 | Lithium iron phosphate continuous preparing device |
| CN203890063U (en) * | 2014-03-17 | 2014-10-22 | 江苏华东锂电技术研究院有限公司 | Continuous lithium iron phosphate preparation device |
-
2016
- 2016-11-15 CN CN201611033719.0A patent/CN106379877A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102303858A (en) * | 2011-07-20 | 2012-01-04 | 彩虹集团公司 | Preparation method of nanoscale ferric phosphate for lithium iron phosphate |
| CN202529847U (en) * | 2012-04-06 | 2012-11-14 | 中国电子科技集团公司第十八研究所 | Ferric pyrophosphate powder preparation system with controllable particle size |
| CN203781852U (en) * | 2014-03-17 | 2014-08-20 | 江苏华东锂电技术研究院有限公司 | Lithium iron phosphate continuous preparing device |
| CN203890063U (en) * | 2014-03-17 | 2014-10-22 | 江苏华东锂电技术研究院有限公司 | Continuous lithium iron phosphate preparation device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809380A (en) * | 2019-03-06 | 2019-05-28 | 深圳海纳百川科技有限公司 | A kind of technique and device of ferrous solution synthesis |
| CN109809380B (en) * | 2019-03-06 | 2020-06-02 | 深圳海纳百川科技有限公司 | Process and device for synthesizing iron solution |
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