CN110255521A - A kind of method of titanium white by product object ferrous sulfate synthesis ferric phosphate - Google Patents
A kind of method of titanium white by product object ferrous sulfate synthesis ferric phosphate Download PDFInfo
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- CN110255521A CN110255521A CN201910481016.1A CN201910481016A CN110255521A CN 110255521 A CN110255521 A CN 110255521A CN 201910481016 A CN201910481016 A CN 201910481016A CN 110255521 A CN110255521 A CN 110255521A
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- ferrous sulfate
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of methods of titanium white by product object ferrous sulfate synthesis ferric phosphate, comprising the following steps: reduced iron powder is added in titanium white by product object ferrous sulfate solution, after reaction, flocculant solution is added, filters to obtain ferrous sulfate solution A；It takes microcosmic salt solution that excessive hydrogen peroxide is added and obtains microcosmic salt solution B after pH is adjusted to 6.5~8.5 after mixing evenly；Solution B is added into solution A, after the reaction was completed adjusts pH to 1.8~3.2, obtains suspension C；Filtering, after being washed with water, pulp obtains pure suspension D；Phosphoric acid is added, the total iron and total phosphorus ratio for controlling reaction system are 1:1~1.3, obtain ferric phosphate intermediate after the reaction was completed, obtain suspension E after aged, crystallization；Filtering, refilters after being washed with water, and repeated washing filter operation collects ferric phosphate filter cake up to conductivity≤1000 μ s/cm of the water filtered out；Calcining obtains anhydrous iron phosphate finished product.
Description
Technical field
The present invention relates to lithium ion battery material technical fields, and in particular to a kind of titanium white by product object ferrous sulfate synthesis phosphorus
The method of sour iron.
Background technique
Presoma of the ferric phosphate as LiFePO4, purity, structure and pattern have very the performance of LiFePO4 product
Big influence, the electrochemical performances of lithium iron phosphate that different phosphoric acid iron materials synthesize differ greatly.Ferric phosphate is usually by sulfuric acid Asia
Prepared by iron and phosphate reaction, major part ferric phosphate manufacturer, generallys use the high-purity iron sheet of sulfuric acid dissolution or high purity iron at present
Powder prepares the ferrous sulfate of high-purity, and this method can generate a large amount of hydrogen during molten iron, and safety is lower, therefore, raw
Plant area's fire prevention, explosive-proof grade are required during production stringent, while high-purity iron sheet and iron powder are expensive, cause production cost compared with
It is high.Iron sheet and iron powder are substituted as source of iron using titanium white by product object ferrous sulfate, are that current ferric phosphate manufacturer reduces iron
One of source cost way.
During production of titanium dioxide by sulfuric acid method, every production 1t titanium dioxide product can generate 3.5~4.0t by-product, seven water sulfuric acid
Ferrous (being commonly called as green vitriol), by this estimation, the every annual meeting in China generates by-product ferrous sulfate object about 700kt because producing titanium dioxide.
However, due in titanium white by product object ferrous sulfate impurity element Ti, Mg, Al and Mn content it is higher, it is difficult to be used directly, cause
Titanium white by product object in the prior art is usually stacked everywhere, not only seriously pollutes environment, but also result in waste of resources, and is influenced
The economic benefit of enterprise.Therefore, the comprehensive utilization of titanium white by product object ferrous sulfate is imperative.
To the phosphorus using titanium white by product object ferrous sulfate large-scale production high-purity, high compacted density and excellent electrical property
Sour iron, it is necessary to find a kind of effective titanium white by product object ferrous sulfate removal of impurities and matched ferric phosphate preparation process.In
State invention patent application document CN106892415A discloses a kind of method that byproduct ferrous sulfate of titanium dioxide prepares ferric phosphate,
It specifically discloses by blasting air after heating, sulphur acid for adjusting pH value is added, after flocculant filtering is added, adds di(2-ethylhexyl)phosphate
Removal of impurities ferrous sulfate is obtained by filtration after hydrogen sodium, flocculant, adds sodium phosphate, phposphate reacts and ferric phosphate is made.This method
It is higher to control titanium white by product object ferrous sulfate temperature, while after blasting air, ferrous ion is easy a large amount of hydrolytic precipitations, causes iron
It loses more serious, after sulfuric acid is added, causes sulfur content in finished product ferric phosphate higher, while needing in back segment reaction excessive very much
Phosphoric acid can just be converted to ferric phosphate to control pH value, cause Fe/P in finished product lower, while ferric phosphate lmpurities element M g,
Al, Mn are higher, and wherein Mg, Mn can reach 150ppm or more, and impurity removal process is complicated in the technique, to raw material titanium white by product object
Impurity requires stringent in ferrous sulfate, prepares that leaching requirement in ferric phosphate washing process is big, and the quality of ferric phosphate is more difficult to control.This
Outside, it is ultra-fine to disclose a kind of titanium white by product object ferrous sulfate preparation LITHIUM BATTERY by Chinese invention patent application file CN107857243A
The method of ferric phosphate is flocculated by the way that ferric iron in phosphoric acid and solution is added and is formed after ferric phosphate colloid absorbed portion impurity to be added
Agent after sedimentation filtration, is added ammonium hydroxide, converts iron hydroxide for ferrous sulfate, then fill into phosphoric acid, be converted into ferric phosphate.The work
The colloid adsorbing contaminant that phosphoric acid is formed is added in skill, although the removal effect to Ti is good, not to the adsorption effect of Mn, Al and Cr
It is good.Be added ammonium hydroxide after, these impurity easily with iron co-precipitation bring into iron hydroxide, after being converted to ferric phosphate, cause ferric phosphate at
After impurity element Mg, Al, Mn are higher in product, while the stage that cleans in the technique exists because introducing phosphoric acid, iron loss is serious, simultaneously
Phosphoric acid amount is added during back segment ferric phosphate conversion reaction to cause phosphorus source metering inaccurate because of the phosphoric acid that the removal of impurities stage brings into
Really, Fe/P is difficult to control, and is had an adverse effect to finished product electrical property.
Based on this, still need to further develop utilization titanium white by product object ferrous sulfate synthesis easy to operate and high controllability
The technique of ferric phosphate.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of titanium white by product object sulfuric acid easy to operate and high controllability
The method of ferrous iron synthesis ferric phosphate.
In order to solve the above-mentioned technical problem, a kind of the technical solution adopted by the present invention are as follows: titanium white by product object ferrous sulfate conjunction
At the method for ferric phosphate, comprising the following steps:
S1, under stirring by reduced iron powder be added titanium white by product object ferrous sulfate solution in, control reaction system
Temperature is 50~85 DEG C, after the reaction was completed, flocculant solution is added, the ferrous sulfate solution A of primary purification is obtained by filtration；
It takes microcosmic salt solution that excessive hydrogen peroxide is added and obtains microcosmic salt solution after pH is adjusted to 6.5~8.5 after mixing evenly
B；
S2, microcosmic salt solution B is added in ferrous sulfate solution A, is reacted under stiring, after the reaction was completed by pH adjust to
1.8~3.2, obtain flaxen ferric phosphate intermediate suspension C；
S3, the flaxen ferric phosphate intermediate suspension C is filtered, after being washed with water, pulp obtains pure suspended
Liquid D；
Phosphoric acid is added in S4, Xiang Suoshu suspension D, the total iron and total phosphorus ratio for controlling reaction system are 1:1~1.3,
Heating temperature is 88~100 DEG C, reacts under conditions of stirring, obtains faint yellow ferric phosphate intermediate after the reaction was completed, will be yellowish
Color ferric phosphate intermediate is aged, the ferric phosphate suspension E of white is obtained after crystallization；
S5, ferric phosphate suspension E is filtered into repeated washing filter operation up to conductivity≤1000 μ s/ of the water filtered out
Cm collects ferric phosphate filter cake and calcines up to anhydrous iron phosphate finished product.
Preferably, the mixing speed in the step S1 is 40~400r/min.
Preferably, the reaction time in the step S1 is 120~360min.
Further, the reduced iron powder in the step S1 is high-purity reduced iron powder, iron powder in high-purity reduced iron powder
Purity be 98% or more.
Preferably, the dosage of the reduced iron powder in the step S1 be titanium white by product object ferrous sulfate quality 0.05%~
0.1%, reaction temperature is 50~70 DEG C, and stirring rate is 40r~300r/min, and the reaction time is 2~4h.
Preferably, flocculant described in the step S1 is cationic polyacrylamide (cationic
Polyacrylamide, CPAM), the mass concentration of CPAM is 0.01% in the flocculant solution.
Preferably, in the step S1, the whole mass concentration in the reaction system of flocculant is 0.01%.
Preferably, the volume additional amount of the flocculant solution be titanium white by product put ferrous sulfate solution volume 0.01~
0.1 times.
Preferably, microcosmic salt described in the step S1 includes ammonium dihydrogen phosphate, sodium dihydrogen phosphate, diammonium hydrogen phosphate, phosphoric acid
At least one of disodium hydrogen, potassium dihydrogen phosphate or dipotassium hydrogen phosphate.
Preferably, in the step S1, the reagent for adjusting pH value is phosphoric acid, ammonium hydroxide, sodium hydroxide or sodium carbonate.
Further, the amount of the substance of hydrogen peroxide is 1.05~1.5 times of molysite reaction meterings mole in the step S1.
Further, in the step S2, the concentration of microcosmic salt solution and ferrous sulfate solution is controlled as 0.5~
1.5mol/L。
Further, in the step S2, the feed time of microcosmic salt solution is 30~180min.
Preferably, in the step S2, microcosmic salt solution B additional amount according to molysite and microcosmic salt mole metering than be 1:0.65~
0.95 is added.
Further, in the step S2, reaction temperature is 25~60 DEG C, and the reaction time is 20~80min.
Preferably, in the step S2, pH to 1.8~3.2 is adjusted by phosphoric acid, ammonium hydroxide or sodium hydroxide.
Preferably, the washing step in the step S3, conductivity≤2200 μ s/cm when reaching washing terminal, pulp obtain
To suspension in solid-liquid mass volume ratio be 1:0.5~10.
Preferably, the mixing speed in the step S4 is 30~500r/min；Preferably, the reaction in the step S4
Time is 120~300min.
Further, ferric phosphate filter cake is calcined at 550 DEG C~750 DEG C in the step S5,2~5h obtains anhydrous phosphorus
Sour iron finished product.
The beneficial effects of the present invention are: the present invention program is by being added reduced iron powder into titanium dioxide ferrous sulfate solution
And heating stirring is reacted, and is restored impurity using reduced iron powder, while iron powder is oxidized to ferrous ion and enters in solution, both may be used
The impurity in solution is preferably removed, and can avoid introducing new impurity；Iron powder can also consume byproduct ferrous sulfate of titanium dioxide
In residual acid, the pH value of reaction iron series can be improved, the titanium in titanium dioxide ferrous sulfate hydrolyzes to form precipitating, and filtering separates titanium
And precipitation adsorption partial impurities, the present invention program quantity of slag in dedoping step is few, the smaller utilization of iron loss in easy filtering and solution
Rate is high；It is selective good in precipitation process to be made by control reaction condition (such as pH, temperature), and iron precipitates completely prior to impurity,
It is not yet co-precipitated with iron using impurity, then by washing, it can be directly further by separation of foreign elements, to obtain pure phosphorus
Sour iron, the program can preferably overcome byproduct ferrous sulfate of titanium dioxide impurity removal process in the prior art and subsequent phosphoric acid iron
Waste residue present in standby technical process is more, iron loss vector is big, is difficult to filter, and finished product impurity element Mn, Al, Cr is higher, sulfur content
The technologies such as higher, finished product Fe/P is difficult to control, and requirement to titanium white by product object ferrous sulfate impurity is stringent not in, the present invention program
Simple process and parameters are easily controllable, requires the titanium white by product object ferrous sulfate as raw material low, is suitble to extensive raw
It produces.
Detailed description of the invention
Fig. 1 is the SEM figure of the ferric phosphate prepared in the embodiment of the present invention 1.
Fig. 2 is the XRD diagram of the ferric phosphate prepared in the embodiment of the present invention 1.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is given below in conjunction with embodiment and attached drawing
With explanation.
The embodiment of the present invention one are as follows: a kind of method of titanium white by product object ferrous sulfate synthesis ferric phosphate, including following step
It is rapid:
(1) weigh the by-product ferrous sulfate generated during certain plant produced titanium dioxide of 4673.83g be configured to it is molten
Liquid is dissolved in water to 9L, high-purity reduced iron powder of 4.67g 99% is added, and is 40r/min in revolving speed, heating temperature is 50 DEG C
Under the conditions of react 2h, into solution be added 0.01%CPAM solution, wherein the volume additional amount of CPAM solution be titanium white by product object
0.1 times of ferrous sulfate solution volume, is obtained by filtration the ferrous sulfate solution of primary purification.
(2) 1635.16g PHOSPHORIC ACID TECH.GRADE ammonium dihydrogen (w%=99%) is weighed, is dissolved in water, adds and is measured with molysite
The hydrogen peroxide of molar ratio excessive 20%, is diluted with water to 10L, and ammonium hydroxide is added, microcosmic salt pH value is adjusted to 8.5.
(3) ferrous sulfate solution is diluted to 1.5mol/L, treated that microcosmic salt solution 30min uniformly adds by step (2)
It is 50 DEG C in heating temperature, the feed time of stirring rate 30r/min, microcosmic salt are in ferrous sulfate after adding to dilution
Ammonium hydroxide is added in 30min, reaction time 20min, and pH is adjusted to 3.2, is obtained in flaxen ferric phosphate after first step reaction
Mesosome suspension.
(4) ferric phosphate intermediate suspension is filtered, washed (due to solubility product Ksp=1.3 × 10 of ferric phosphate-22Pole
Small, when pH is 1.8~3.2, iron is preferentially formed with phosphate radical and is precipitated, and other impurities element, as calcium, magnesium, manganese, zinc phosphoric acid
Salt solubility product cannot form greatly precipitating, form precipitating and need higher pH value, therefore, these impurity elements are in the form of soluble salt
In the presence of be filtered, washed and solution in main anion sulfate acid radical ion can also be washed), washing terminal conductivity be
2000μs/cm.Water slurry filter cake is added to obtain pure ferric phosphate intermediate suspension, the solid-liquid mass volume ratio of suspension is 1:
0.5。
(5) phosphoric acid is added in the suspension obtained to aforesaid operations (4), so that in reaction system, the ratio of total iron and total phosphorus
Example is 1:1.3, is 88 DEG C in heating temperature, under conditions of stirring rate is 500r/min, reaction time 120min is obtained white
The ferric phosphate suspension of color.
(6) white ferric phosphate suspension is filtered, washed, washing terminal conductivity is 960 μ s/cm, obtains ferric phosphate filter
Cake.
(7) filter cake is calcined into 5h at 550 DEG C, obtains anhydrous phosphoric acid iron powder body.
Ferric phosphate made from aforesaid operations is taken to be scanned Electronic Speculum (scanning electron microscope, SEM)
It is analyzed with X-ray diffractometer (X-Ray Diffractometer, XRD), it is as a result as depicted in figs. 1 and 2 respectively.It can be with from Fig. 1
Find out, ferric phosphate pattern made from the embodiment of the present invention 1 is in honeycomb, and about at 0.1 μm or so, partial size divides the partial size of primary particle
Cloth is uniform.As can be seen from Figure 2 the diffraction maximum of ferric phosphate made from the embodiment of the present invention 1 and standard phosphate iron card (29-
0715) characteristic diffraction peak in is compared, and peak shape, peak position fit like a glove and free from admixture peak, meanwhile, the embodiment of the present invention system
The diffraction maximum of the ferric phosphate obtained is sharp, and halfwidth is narrow, and being indicated above ferric phosphate made from the embodiment of the present invention 1 is pure phase and crystallization
Spend good ferric phosphate.
The embodiment of the present invention two are as follows: a kind of method of titanium white by product object ferrous sulfate synthesis ferric phosphate, including following step
It is rapid:
(1) it weighs 9347.66g by-product of white titanium pigment and prepares ferrous sulfate solution, be dissolved in water to 20L, 4.67g high is added
Pure reduced iron powder is 300r/min in revolving speed, and heating temperature is 70 DEG C, and after reacting 4h, titanium white by product object sulphur is added into solution
0.05 times of 0.01%CPAM solution of sour ferrous iron solution volume, is obtained by filtration the ferrous sulfate solution of primary purification.
(2) 2568.73g diammonium hydrogen phosphate is weighed, is dissolved in water, is added double with molysite stoichiometric mole ratio excessive 50%
Oxygen water adds water and is diluted to 20L, and phosphoric acid is added, microcosmic salt solution ph is adjusted to 6.5.
(3) ferrous sulfate solution is diluted to 1mol/L, then microcosmic salt solution 90min is uniformly added in ferrous sulfate,
It is 25 DEG C, stirring rate 500r/min, reaction time 80min in heating temperature, phosphoric acid is added, pH is adjusted to 2.2, the
Flaxen ferric phosphate intermediate suspension is obtained after single step reaction.
(4) ferric phosphate intermediate suspension is filtered, washed, washing terminal conductivity is 1500 μ s/cm.Water slurryization is added to filter
Cake obtains pure ferric phosphate intermediate suspension, and the solid-liquid mass volume ratio of suspension is 1:10.
(5) phosphoric acid is added into above-mentioned steps (4) treated suspension, so that in reaction system, total iron and total phosphorus
Ratio is 1:1.1, is 100 DEG C, stirring rate 30r/min, reaction time 300min in heating temperature, obtains the phosphorus of white
Sour iron suspension.
(6) white ferric phosphate suspension is filtered, washed, washing terminal conductivity is 570 μ s/cm, obtains ferric phosphate filter
Cake.
(7) filter cake is calcined into 2h at 750 DEG C, obtains anhydrous phosphoric acid iron powder body.
The embodiment of the present invention three are as follows: a kind of method of titanium white by product object ferrous sulfate synthesis ferric phosphate, including following step
It is rapid:
(1) it weighs 7809.10g byproduct ferrous sulfate of titanium dioxide and is prepared into solution, be dissolved in water to 40L, add 6.5g high
Pure reduced iron powder is 150r/min in revolving speed, and heating temperature is 60 DEG C, reacts 3h, titanium white by product object sulfuric acid is added into solution
0.01 times of 0.01%CPAM solution of ferrous iron solution volume, is obtained by filtration the ferrous sulfate solution of primary purification.
(2) 2700.00g disodium hydrogen phosphate is weighed, is dissolved in water, is added double with molysite stoichiometric mole ratio excessive 5%
Oxygen water adds water and is diluted to 50L, and phosphoric acid is added, microcosmic salt solution ph is adjusted to 7.0.
(3) ferrous sulfate solution is diluted to 0.5mol/L, then microcosmic salt solution 180min is uniformly added in ferrous sulfate,
It is 25 DEG C, stirring rate 500r/min, reaction time 80min in heating temperature, ammonium hydroxide is added, pH is adjusted to 1.8, the
Flaxen ferric phosphate intermediate suspension is obtained after single step reaction.
(4) ferric phosphate intermediate suspension is filtered, washed, washs 1000 μ s/cm of terminal conductivity.Add water slurry filter cake
Pure ferric phosphate intermediate suspension is obtained, the solid-liquid mass volume ratio of suspension is 1:0.2.
(5) phosphoric acid is added into above-mentioned steps (4) treated suspension, so that in reaction system, total iron and total phosphorus
Ratio is 1:10, is 92 DEG C, stirring rate 150r/min, reaction time 180min in heating temperature, obtains the phosphorus of white
Sour iron suspension.
(6) white ferric phosphate suspension is filtered, washed, washing terminal conductivity is 160us/cm, obtains ferric phosphate filter
Cake.
(7) filter cake is calcined into 3h at 650 DEG C, obtains anhydrous phosphoric acid iron powder body.
Anhydrous phosphoric acid iron powder body made from above-described embodiment 1~3 is taken to carry out physical and chemical index test, and by test result and city
Conventional phosphoric acid iron is sold to compare, as a result as shown in table 1 below:
1 physical and chemical index comparing result table of table
As can be seen from the above table, ferric phosphate Fe/P made from the embodiment of the present invention is higher than commercially available phosphoric acid up to 0.98 or more
Iron, impurity content are lower than the impurity of commercially available ferric phosphate, and especially content is higher miscellaneous in raw material titanium white by product object ferrous sulfate
Prime element Mg, Al, Mn are in 10ppm hereinafter, reach ferric phosphate lithium cell standard.
Take anhydrous phosphoric acid iron powder body made from above-described embodiment 1~3 and commercially available conventional phosphoric acid iron under the same conditions according to
Routine techniques in the prior art is prepared into LiFePO4, carries out compacted density and electric performance test to LiFePO4 obtained,
As a result as shown in table 2 below:
2 compacted density of table and electrical property testing result contrast table
As can be seen from the above table, the powder compacted density of the LiFePO4 of ferric phosphate synthesis is made using the embodiment of the present invention
And electrical property is superior to the LiFePO4 of commercially available ferric phosphate synthesis, is indicated above ferric phosphate made from the present invention program in lithium battery
Preparation field has a good application prospect.
Titanium white by product object ferrous sulfate raw material sources used in above-described embodiment are identical, to being made in the embodiment of the present invention
Titanium white by product object ferrous sulfate raw material carries out composition detection, as a result as shown in table 3 below:
3 ferrous sulfate material composition table of table
As can be seen from the above table, the iron content in the raw material is not high and impurity content is higher, therefore, in conjunction with above-mentioned table
It is not high that sign data can be seen that requirement of the present invention program to raw material.
Feed time is controlled in the embodiment of the present invention so that preparation ferric phosphate uniform particle diameter and appropriate
In range, can preferably it be applied in lithium electricity production process.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (10)
1. a kind of method of titanium white by product object ferrous sulfate synthesis ferric phosphate, it is characterised in that: the following steps are included:
S1, under stirring by reduced iron powder be added titanium white by product object ferrous sulfate solution in, control the temperature of reaction system
It is 50~85 DEG C, after the reaction was completed, flocculant solution is added, the ferrous sulfate solution A of primary purification is obtained by filtration；
It takes microcosmic salt solution that excessive hydrogen peroxide is added and obtains microcosmic salt solution B after pH is adjusted to 6.5~8.5 after mixing evenly；
S2, microcosmic salt solution B is added in ferrous sulfate solution A, is reacted under stiring, after the reaction was completed adjust pH to 1.8
~3.2, obtain flaxen ferric phosphate intermediate suspension C；
S3, the flaxen ferric phosphate intermediate suspension C is filtered, after being washed with water, pulp obtains pure suspension D；
Phosphoric acid is added in S4, Xiang Suoshu suspension D, the total iron and total phosphorus ratio for controlling reaction system are 1:1~1.3, are being heated
Temperature is 88~100 DEG C, reacts under conditions of stirring, obtains faint yellow ferric phosphate intermediate after the reaction was completed, by faint yellow phosphorus
Sour iron intermediate is aged, the ferric phosphate suspension E of white is obtained after crystallization；
S5, ferric phosphate suspension E is filtered to repeated washing filter operation up to conductivity≤1000 μ s/cm of the water filtered out, received
Collection ferric phosphate filter cake is calcined up to anhydrous iron phosphate finished product.
2. the method for titanium white by product object ferrous sulfate synthesis ferric phosphate according to claim 1, it is characterised in that: the step
Mixing speed in rapid S1 is 40~400r/min.
3. the method for titanium white by product object ferrous sulfate synthesis ferric phosphate according to claim 1, it is characterised in that: the step
Reduced iron powder in rapid S1 is high-purity reduced iron powder, and the purity of iron powder is 98% or more in high-purity reduced iron powder.
4. the method for titanium white by product object ferrous sulfate synthesis ferric phosphate according to claim 1, it is characterised in that: the step
The dosage of reduced iron powder in rapid S1 is the 0.05%~0.1% of titanium white by product object ferrous sulfate quality, reaction temperature is 50~
70 DEG C, stirring rate is 40r~300r/min, and the reaction time is 2~4h.
5. the method for titanium white by product object ferrous sulfate synthesis ferric phosphate according to claim 1, it is characterised in that: the step
Flocculant described in rapid S1 is CPAM, and the mass concentration of CPAM is 0.01% in the flocculant solution.
6. the method for titanium white by product object ferrous sulfate synthesis ferric phosphate according to claim 1, it is characterised in that: the wadding
The volume additional amount of solidifying agent solution is 0.01~0.1 times that titanium white by product puts ferrous sulfate solution volume.
7. the method for titanium white by product object ferrous sulfate synthesis ferric phosphate according to claim 1, it is characterised in that: the step
In rapid S1, the reagent for adjusting pH value is phosphoric acid, ammonium hydroxide, sodium hydroxide or sodium carbonate.
8. the method for described in any item titanium white by product object ferrous sulfate synthesis ferric phosphates, feature exist according to claim 1~7
In: in the step S2, the microcosmic salt solution B additional amount is according to molysite and microcosmic salt mole metering than being that 1:0.65~0.95 adds
Enter.
9. the method for described in any item titanium white by product object ferrous sulfate synthesis ferric phosphates, feature exist according to claim 1~7
In: in the step S2, by microcosmic salt solution and ferrous sulfate solution, concentration is controlled as 0.5~1.5mol/L respectively.
10. the method for described in any item titanium white by product object ferrous sulfate synthesis ferric phosphates according to claim 1~7, feature
It is: the washing step in the step S3, conductivity≤2200 μ s/cm when reaching washing terminal, the suspension that pulp obtains
Middle solid-liquid mass volume ratio is 1:0.5~10.
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| CN115140721A (en) * | 2022-05-24 | 2022-10-04 | 抚州润泰药业有限公司 | Method for synthesizing battery-grade iron phosphate from byproduct ferrous sulfate and byproduct phosphoric acid |
| CN115140721B (en) * | 2022-05-24 | 2024-03-12 | 抚州润泰药业有限公司 | Method for synthesizing battery grade ferric phosphate from byproduct ferrous sulfate and byproduct phosphoric acid |
| CN115108543A (en) * | 2022-05-31 | 2022-09-27 | 丁兴立 | Method for synthesizing battery-grade iron phosphate |
| CN115124010A (en) * | 2022-07-15 | 2022-09-30 | 湖北万润新能源科技股份有限公司 | Manganese (II) phosphate nanosheet and lithium iron manganese phosphate cathode material and preparation method thereof |
| CN115124010B (en) * | 2022-07-15 | 2023-05-30 | 湖北万润新能源科技股份有限公司 | Manganese (II) phosphate nanosheet, lithium manganese iron phosphate positive electrode material and preparation method thereof |
| WO2024027214A1 (en) * | 2022-08-03 | 2024-02-08 | 宜都兴发化工有限公司 | Method for preparing mesoporous iron phosphate by induction by block copolymer |
| CN115403021A (en) * | 2022-09-08 | 2022-11-29 | 云南纳诺电子新材料有限公司 | Method for preparing lithium iron phosphate from titanium dioxide byproduct ferrous sulfate |
| CN115535985B (en) * | 2022-09-22 | 2023-11-21 | 云南云天化股份有限公司 | Method for synthesizing battery-grade ferric phosphate by oxidation and precipitation integrated process |
| CN115535985A (en) * | 2022-09-22 | 2022-12-30 | 云南云天化股份有限公司 | Method for synthesizing battery-grade iron phosphate by oxidation and precipitation integrated process |
| CN115701828A (en) * | 2022-11-25 | 2023-02-14 | 宁波新福钛白粉有限公司 | Quasi-continuous method for preparing battery-grade anhydrous iron phosphate by using ferrous sulfate |
| CN115784186A (en) * | 2022-12-16 | 2023-03-14 | 河南龙佰新材料科技有限公司 | Preparation method of spherical iron phosphate |
| CN116534820A (en) * | 2023-03-30 | 2023-08-04 | 新洋丰农业科技股份有限公司 | Method for preparing high-compaction ferric phosphate from industrial monoammonium phosphate and ferrous sulfate |
| CN116534820B (en) * | 2023-03-30 | 2023-11-24 | 新洋丰农业科技股份有限公司 | Method for preparing high-compaction ferric phosphate from industrial monoammonium phosphate and ferrous sulfate |
| CN116621141A (en) * | 2023-04-25 | 2023-08-22 | 浙江友山新材料有限公司 | Preparation method of low-manganese magnesium ferric phosphate |
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