CN107473196A - A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate - Google Patents
A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate Download PDFInfo
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- CN107473196A CN107473196A CN201710923708.8A CN201710923708A CN107473196A CN 107473196 A CN107473196 A CN 107473196A CN 201710923708 A CN201710923708 A CN 201710923708A CN 107473196 A CN107473196 A CN 107473196A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate, including：Preparation iron salt concentration is 0.05 2.0mol/L, and trivalent iron salt is 1 with sour mol ratio：0.1 5.0, as raw material A；Preparation phosphate concn is 0.05 2.0mol/L, as raw material B；The mol ratio of phosphorus and iron in raw material A is 1.0 2.0 in raw material B phosphate, is transported in first stage micro passage reaction and quickly mixes, and precipitation reaction occurs, obtains ferric phosphate precursor pulp C;Precursor pulp C is delivered to two level continuous hydrothermal crystallization in second stage microchannel by pump, obtains nano ferric phosphate slurry D;Nano ferric phosphate slurry D is filtered, and by washing of precipitate, drying, obtains nano ferric phosphate.Present invention process is simple, investment and floor space are small, production efficiency is high, product purity is high, magnetic foreign body risk is small, granularity is small and it is uniform, monodispersity is good, the LiFePO4 compacted density for preparing as raw material is high, good product consistency.
Description
Technical field
The invention belongs to chemical technology field, and in particular to a kind of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate
Method.
Background technology
With becoming increasingly conspicuous for energy and environment problem, lithium ion battery is close constantly to high-energy as secondary cell
Degree, high security, long-life and inexpensive direction are developed, to meet electric automobile, solar energy and wind energy energy-storage system and intelligence
The field such as peak load regulation network application requirement, so as to which the performance of the critical material to forming battery proposes requirements at the higher level.Therefore, study
Exploitation turns into the focus of Study on Li-ion batteries with high-energy-density, good circulation performance and safe cheap positive electrode
Problem.
The positive electrode that power lithium-ion battery can be done in theory has a lot, but most study be lithium transition oxidation
Thing LiCoO2/LiNiO2/LiMn2O4（LiAlO2）Ternary material and LiFePO4.Ternary material has energy density height, still
Due to structure change caused by its pyrolysis so as to bringing safety issue.Since the phosphorus of olivine structural in 1997
Sour iron lithium（LiFePO4）It has been reported since it is up to 170 mAh/g theoretical capacities, because it has a safety feature, stable circulation
Property high, environment-friendly, low cost and other advantages, and one of study hotspot as current anode material for lithium-ion batteries.
Li+ in LiFePO4 with olivine structural almost can all reversible insertions or deintercalation, actual capacity
Close to the mAh/g of theoretical capacity 170, up to 95% or so, and iron is cheap, non-toxic.It is successfully electric for one
Key factor is synthetic method for the material of pole, and synthetic method can control form, particle size and cation sequence.
LiFePO4Have a safety feature, have extended cycle life, raw material sources extensively, the remarkable advantage such as non-environmental-pollution, as electric automobile
With electrokinetic cell first choice positive electrode, need not doubt.In fact, the LiFePO 4 material of excellent performance is prepared, just first
High performance presoma must be prepared.Sour iron lithium has an outstanding advantage as a kind of anode material for lithium-ion batteries, ferric phosphate because
Similarity in structure be present with LiFePO4 and turn into a kind of important presoma.Pass through the different synthesis of current LiFePO 4 material
Technique is contrasted, and finds there is lot of advantages as the presoma that LiFePO 4 material synthesizes using ferric phosphate.
Compared with ternary material, the major defect of LiFePO4 is that high rate performance is relatively low at present, and existing outstanding problem is just
It is that particle diameter is larger and skewness influences its electronic conductivity and ionic conductance.On the other hand, can by adulterate conductive materials,
The compacted density for reduce particle size, improving battery improves its energy density.Research finds, by particle size nanosizing,
The compacted density of battery can be improved, so as to improve battery capacity density.Obtain that spherical particle diameter is smaller and the phosphorus of narrow distribution
Sour iron lithium, should just prepare that spherical particle diameter is smaller and the ferric phosphate of narrow distribution first.
Ferric phosphate（FePO4）A kind of rice white or pale powder, initial research mainly agricultural, glass-ceramic,
The field such as steel and surface passivation, found that ferric phosphate had unique catalysis characteristics, ion-exchange capacity and electrochemistry later
Can, novel battery positive electrode is alternatively arranged as, is to prepare anode material for lithium-ion batteries.Ferric phosphate（FePO4）As synthesis phosphorus
The important source material of sour iron lithium, preparing phosphoric acid has a variety of methods：Including hydro-thermal method, liquid-phase precipitation method, sol-gel process, air
Oxidizing process, microemulsion method, microwave radiation crystallization method etc..The preparation method of industrial generally use is liquid-phase precipitation method at present, is
Prepared using trivalent, divalent iron salt and phosphoric acid, phosphate, generally require exacting terms, high is required to equipment material, reaction
Time is grown, and granularity is difficult to control, less stable between batch, and low production efficiency, and production cost is also higher, therefore seeks
Economic, gentle, easy to operate preparation method is significant.
Liquid-phase precipitation control crystallisation can control the Fe/P ratios of ferric phosphate well, realize the spheroidization of ferric phosphate.
For particle size and its distribution problem, the troubled water of the material in preparation process is reacted is depended on, is particularly being divided
Mixing on sub- yardstick.Conventional production method is batch production, and the ferric ion aqueous solution and aqueous phosphatic are anti-
Answer mixing, heat temperature raising in kettle to react, obtain the ferric phosphate precursor pulp that granularity is larger and granularity is uneven, gained
To precursor can just access ferric phosphate after prolonged insulation ageing.The mixed effect of traditional reactor is poor, up to not
To the other mixed effect of molecular level, process regulation is not accurate enough, therefore resulting product granularity is uneven, uniformity
Difference, and because mass-and heat-transfer efficiency is low, whole course of reaction duration length, low production efficiency.Battery material is different to magnetic
Thing requires high, therefore requires high to reactor material, and equipment early investment is big.
The content of the invention
It is an object of the invention to a kind of technique for overcoming disadvantages mentioned above and providing is simple, investment and floor space are small, life
Produce that efficiency high, product purity are high, magnetic foreign body risk is small, granularity is small and it is uniform, monodispersity is good, the phosphorus that is prepared as raw material
Sour iron lithium compacted density is high, the method for the continuous production LITHIUM BATTERY high compacted density nano ferric phosphate of good product consistency.
A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate of the present invention, comprises the following steps：
（1）Prepare the mixed aqueous solution of trivalent iron salt and acid, iron salt concentration 0.05-2.0mol/L；Trivalent iron salt rubs with acid
You are than being 1：0.1-5.0, as raw material A；
（2）Prepare the phosphatic aqueous solution, phosphate concn 0.05-2.0mol/L, as raw material B；
（3）The mol ratio of phosphorus and iron in raw material A is 1.0-2.0 in raw material B phosphate, by being pumped into first stage microchannel
Quickly mixed in reactor, 50-100 DEG C of mixing temperature, incorporation time 1-5min, precipitation reaction occurs, obtains ferric phosphate forerunner
Body slurry C;
（4）Precursor pulp C is delivered to two level continuous hydrothermal crystallization in second stage microchannel, hydrothermal crystallizing temperature by pump
110-180 DEG C, crystallization time 1-30min, obtain nano ferric phosphate slurry D;
（5）Nano ferric phosphate slurry D is filtered, and by washing of precipitate, drying, obtains nano ferric phosphate.
The raw material A trivalent iron salt is ferric nitrate, ferric sulfate, iron chloride or their hydrate.
Acid is nitric acid, sulfuric acid, hydrochloric acid or their mixture in the raw material A.
The raw material B phosphate is ammonium phosphate, sodium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium dihydrogen phosphate, phosphoric acid
Disodium hydrogen or their mixture.
The present invention compared with prior art, has obvious beneficial effect, as can be known from the above technical solutions：The present invention uses
The efficient mixing of micro passage reaction and mass-transfer performance ensure that the microreaction environment of precipitation reaction and hydrothermal crystallization process is tight
Lattice are controllable, enable the ferric ion aqueous solution with aqueous phosphatic in consistent reaction density, suitable and uniform pH
The lower fully precipitation of value obtains the good nano ferric phosphate precursor pulp of homogeneous grain diameter, monodispersity, at the same in liquid phase iron content
It is relatively low, improve conversion ratio and product yield.Resulting nano ferric phosphate precursor pulp is carried out in micro passage reaction
Two level continuous hydrothermal crystallization, directly by nano ferric phosphate precursor pulp converted in-situ, so as to obtain, purity is high, granularity is equal
First, the good nano ferric phosphate of monodispersity.
The present invention can be significantly using the continuous impinging stream reaction coupling microchannel continuous hydrothermal crystallisation technique in microchannel
It is strictly controllable to improve the microreaction environment of precipitation reaction and hydrothermal crystallization process, and hydro-thermal reaction is carried out in microchannel,
Mass-and heat-transfer is fast, can greatly shorten reaction and digestion time, improves stability and uniformity between batch.Due to whole mistake
Journey is successive reaction, and required equipment volume and production area are small, and production efficiency is high, and process materials are few, can quickly, accurately adjust
Whole process conditions, and the material of microreactor can select pure titanium, polyether-ether-ketone, polyester, polyimides, glass, ceramics etc.
There is no the material of magnetic risk, further lift product quality.Used microreactor has special structure (patent application
Number：201610036471.7), easily cleared up, solve the shortcomings that traditional microreactor easily blocks up, be easy to industry amplification life
Production.Have that process is simple, investment and floor space are small, production efficiency is high, product is pure using the nano ferric phosphate for preparing of the present invention
Degree is high, magnetic foreign body risk is small, granularity is small and it is uniform, monodispersity is good, prepared LiFePO4 compacted density is high, product one
The advantages that cause property is good.
Embodiment
Embodiment 1
A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate, comprises the following steps：
0.5mol/L containing ferric nitrate, the phosphoric acid 0.05mol/L aqueous solution are configured, obtains raw material A.Configure 0.5mol/L di(2-ethylhexyl)phosphate
Hydrogen aqueous ammonium, obtain raw material B.Two phase materials press 1:1 volume flow ratio is pumped into microreactor by measuring pump and reacted, and obtains
To ferric phosphate precursor pulp C.Ferric phosphate precursor pulp C is pumped into progress continuous hydrothermal crystallization in one-level micro passage reaction
Reaction, first order hydrothermal crystallizing temperature are 110 DEG C, crystallization time 5 minutes, are then pumped into two level micro passage reaction and carry out the
Secondary continuous hydrothermal crystallization, first order hydrothermal crystallizing temperature are 120 DEG C, crystallization time 9 minutes, obtain white ferric phosphate slurry
Expect D.Slurry D filters out precipitation, and precipitation is washed, dried, obtains nano ferric phosphate, average grain diameter about 50nm.
Embodiment 2
A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate, comprises the following steps：
1mol/L containing ferric nitrate, the phosphoric acid 0.05mol/L aqueous solution are configured, obtains raw material A.Configure 1mol/L sodium dihydrogen phosphate
The aqueous solution, obtain raw material B.Two phase materials press 1:1 volume flow ratio is pumped into microreactor by measuring pump and reacted, and obtains phosphorus
Sour iron precursor pulp C.It is anti-that ferric phosphate precursor pulp C is pumped into progress continuous hydrothermal crystallization in one-level micro passage reaction
Should, first order hydrothermal crystallizing temperature is 120 DEG C, crystallization time 7 minutes, is then pumped into two level micro passage reaction and carries out second
Secondary continuous hydrothermal crystallization, first order hydrothermal crystallizing temperature are 150 DEG C, crystallization time 9 minutes, obtain white ferric phosphate slurry
D.Slurry D filters out precipitation, and precipitation is washed, dried, obtains nano ferric phosphate, average grain diameter about 70nm.
Embodiment 3
A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate, comprises the following steps：
Sulfur acid iron 0.5mol/L, the phosphoric acid 0.25mol/L aqueous solution are configured, obtains raw material A.Configure 0.5mol/L sodium phosphate
The aqueous solution, obtain raw material B.Two phase materials press 1:1 volume flow ratio is pumped into microreactor by measuring pump and reacted, and obtains phosphorus
Sour iron precursor pulp C.It is anti-that ferric phosphate precursor pulp C is pumped into progress continuous hydrothermal crystallization in one-level micro passage reaction
Should, first order hydrothermal crystallizing temperature is 110 DEG C, crystallization time 5 minutes, is then pumped into two level micro passage reaction and carries out second
Secondary continuous hydrothermal crystallization, first order hydrothermal crystallizing temperature are 120 DEG C, crystallization time 9 minutes, obtain white ferric phosphate slurry
D.Slurry D filters out precipitation, and precipitation is washed, dried, obtains nano ferric phosphate, average grain diameter about 80nm.
Embodiment 4
A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate, comprises the following steps：
Chloride containing iron 1mol/L, the hydrochloric acid 0.1mol/L aqueous solution are configured, obtains raw material A.Configure 1mol/L ammonium dihydrogen phosphate
The aqueous solution, obtain raw material B.Two phase materials press 1:1 volume flow ratio is pumped into microreactor by measuring pump and reacted, and obtains phosphorus
Sour iron precursor pulp C.It is anti-that ferric phosphate precursor pulp C is pumped into progress continuous hydrothermal crystallization in one-level micro passage reaction
Should, first order hydrothermal crystallizing temperature is 120 DEG C, crystallization time 7 minutes, is then pumped into two level micro passage reaction and carries out second
Secondary continuous hydrothermal crystallization, first order hydrothermal crystallizing temperature are 125 DEG C, crystallization time 7 minutes, obtain white ferric phosphate slurry
D.Slurry D filters out precipitation, and precipitation is washed, dried, obtains nano ferric phosphate, average grain diameter about 50nm.
Embodiment 5
A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate, comprises the following steps：
Sulfur acid iron 1mol/L, the phosphoric acid 0.1mol/L aqueous solution are configured, obtains raw material A.Configure 1mol/L ammonium dihydrogen phosphate
The aqueous solution, obtain raw material B.Two phase materials press 1:1 volume flow ratio is pumped into microreactor by measuring pump and reacted, and obtains phosphorus
Sour iron precursor pulp C.It is anti-that ferric phosphate precursor pulp C is pumped into progress continuous hydrothermal crystallization in one-level micro passage reaction
Should, first order hydrothermal crystallizing temperature is 120 DEG C, crystallization time 5 minutes, is then pumped into two level micro passage reaction and carries out second
Secondary continuous hydrothermal crystallization, first order hydrothermal crystallizing temperature are 140 DEG C, crystallization time 9 minutes, obtain white ferric phosphate slurry
D.Slurry D filters out precipitation, and precipitation is washed, dried, obtains nano ferric phosphate, average grain diameter about 60nm.
Embodiment 6
A kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate, comprises the following steps：
Sulfur acid iron 1mol/L, the phosphoric acid 0.5mol/L aqueous solution are configured, obtains raw material A.Configure 1mol/L diammonium hydrogen phosphate
The aqueous solution, obtain raw material B.Two phase materials press 1:1 volume flow ratio is pumped into microreactor by measuring pump and reacted, and obtains phosphorus
Sour iron precursor pulp C.It is anti-that ferric phosphate precursor pulp C is pumped into progress continuous hydrothermal crystallization in one-level micro passage reaction
Should, first order hydrothermal crystallizing temperature is 120 DEG C, crystallization time 5 minutes, is then pumped into two level micro passage reaction and carries out second
Secondary continuous hydrothermal crystallization, first order hydrothermal crystallizing temperature are 160 DEG C, crystallization time 9 minutes, obtain white ferric phosphate slurry
D.Slurry D filters out precipitation, and precipitation is washed, dried, obtains nano ferric phosphate, average grain diameter about 80nm.
The principle of the present invention：（1）By be previously added into the trivalent iron salt aqueous solution configured appropriate phosphoric acid, sulfuric acid or
Nitric acid controls the pH value of iron salt solutions and reaction system, and the hydrolysis for suppressing iron ion avoids producing iron hydroxide, while suitably
PH value can ensure the abundant precipitation of iron ion in reaction system；（2）By measuring pump by the trivalent iron salt aqueous solution and phosphoric acid
Saline solution is pumped into progress rapid precipitation reaction in one-level micro passage reaction by a certain percentage, strengthens because microreactor has
Mass transfer and mixed effect, its monodispersity is preferable in nano particle state for obtained ferric phosphate presoma slurry material；（3）From micro- anti-
Answer the ferric phosphate presoma slurry viscosity of outflow in device slightly larger, channel blockage is easily caused if being directly entered in converter, therefore increase
If buffer tank stores ferric phosphate precursor pulp；（4）Ferric phosphate precursor pulp in buffer tank is stored in again by pump by its pump
Enter and continuous hydrothermal crystallization carried out in two-stage micro passage reaction, make ferric phosphate precursor in situ be continuously converted to high-purity,
Good dispersion, even-grained nano ferric phosphate particle.
The above described is only a preferred embodiment of the present invention, any formal limitation, Ren Hewei not are made to the present invention
Disengaging technical solution of the present invention content, any simple modification made according to technical spirit of the invention to above example, etc.
With change and modification, in the range of still falling within technical solution of the present invention.
Claims (4)
1. a kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate, comprises the following steps：
（1）Prepare the mixed aqueous solution of trivalent iron salt and acid, iron salt concentration 0.05-2.0mol/L；Trivalent iron salt rubs with acid
You are than being 1：0.1-5.0, as raw material A；
（2）Prepare the phosphatic aqueous solution, phosphate concn 0.05-2.0mol/L, as raw material B；
（3）The mol ratio of phosphorus and iron in raw material A is 1.0-2.0 in raw material B phosphate, by being pumped into first stage microchannel
Quickly mixed in reactor, 50-100 DEG C of mixing temperature, incorporation time 1-5min, precipitation reaction occurs, obtains ferric phosphate forerunner
Body slurry C;
（4）Precursor pulp C is delivered to two level continuous hydrothermal crystallization in second stage microchannel, hydrothermal crystallizing temperature by pump
110-180 DEG C, crystallization time 1-30min, obtain nano ferric phosphate slurry D;
（5）Nano ferric phosphate slurry D is filtered, and by washing of precipitate, drying, obtains nano ferric phosphate.
2. a kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate as claimed in claim 1, wherein：Raw material
A trivalent iron salts are ferric nitrate, ferric sulfate, iron chloride or their hydrate.
3. a kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate as claimed in claim 1, wherein：Raw material
Acid is nitric acid, sulfuric acid, hydrochloric acid or their mixture in A.
4. a kind of method of continuous production LITHIUM BATTERY high compacted density nano ferric phosphate as claimed in claim 1, wherein：Raw material
B phosphate is ammonium phosphate, sodium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate or theirs is mixed
Compound.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108117055A (en) * | 2017-12-30 | 2018-06-05 | 彩客化学（东光）有限公司 | The preparation method and process units of a kind of battery-grade iron phosphate |
| CN108878822A (en) * | 2018-06-22 | 2018-11-23 | 宜春学院 | Coat the preparation method of nano ferric phosphate composite material |
| CN111252751A (en) * | 2018-12-03 | 2020-06-09 | 成都市银隆新能源有限公司 | Microfluidic droplet forming structural component and method for preparing solid spherical lithium iron phosphate |
| CN112876681A (en) * | 2021-02-04 | 2021-06-01 | 武汉柔显科技股份有限公司 | Preparation method for preparing polyimide precursor and film thereof by using impinging stream reactor |
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| CN108878822A (en) * | 2018-06-22 | 2018-11-23 | 宜春学院 | Coat the preparation method of nano ferric phosphate composite material |
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| CN111252751A (en) * | 2018-12-03 | 2020-06-09 | 成都市银隆新能源有限公司 | Microfluidic droplet forming structural component and method for preparing solid spherical lithium iron phosphate |
| CN112876681A (en) * | 2021-02-04 | 2021-06-01 | 武汉柔显科技股份有限公司 | Preparation method for preparing polyimide precursor and film thereof by using impinging stream reactor |
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