CN103708565B - Preparation method of FeF3 - Google Patents

Preparation method of FeF3 Download PDF

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CN103708565B
CN103708565B CN201410004861.7A CN201410004861A CN103708565B CN 103708565 B CN103708565 B CN 103708565B CN 201410004861 A CN201410004861 A CN 201410004861A CN 103708565 B CN103708565 B CN 103708565B
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fef
mixture
state
solid
iron ore
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CN103708565A (en
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刘瑞
林乐洪
章林
史春华
龚亚云
李丹阳
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GUIZHOU WANFANG ALUMINUM SCIENCE AND TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

The invention relates to the field of preparation of chemical materials, and particularly relates to a preparation method of FeF3. The method comprises the following step: evenly mixing iron ore or mineral containing Fe2O3 and fluoride, so as to obtain a mixture, and enabling the mixture to react, so as to obtain gaseous FeF3. By adopting the preparation method of the FeF3 disclosed by the invention, the preparation process can be finished by adopting a known reaction device in the field, the production technology is simple in step, and cheap iron ore or mineral containing Fe2O3 and fluoride are adopted as main raw materials, so that the method is low in demands on reaction condition and low in production cost.

Description

FeF 3preparation method
Technical field
The present invention relates to chemical materials preparation field, in particular to FeF 3preparation method.
Background technology
The fluorochemical of iron is owing to having inexpensive, nontoxic, environmental protection, theoretical capacity advantages of higher; And the fluorochemical of iron as the positive electrode material of lithium secondary battery metal fluoride, therefore can receive much attention.In numerous transition metal, Fe element has cheap, rich reserves, advantages of environment protection, therefore, and FeF 3become one of preferred material of reversible chemical transformation mechanism material.FeF 3when being used as positive electrode material, in charge and discharge process, there are two kinds of different storage lithium mechanism: one is typically embedding, de-lithium mechanism, i.e. a Li +at FeF 3embedding reversible in crystalline structure/deviate from, along with Fe 3+/ Fe 2+transformation; Another kind is reversible chemical transformation mechanism, i.e. FeF 3continue and two Li +there is electrochemical reducting reaction, shaping Fe nanoparticle and LiF.
In correlation technique, preparation FeF 3main method have following several: 1, by Fe 2o 3or FeCl 3amorphous FeF is generated with the HF gas effect of drying 3; 2, at high temperature by F 2with metal Fe or Fe 2o 3effect obtains FeF 3; 3, with Fe (OH) 3precipitation and hydrofluoric acid effect, the water that then evaporate to dryness is unnecessary and HF, obtain FeF 3; 4, ionic liquid is utilized to prepare FeF as solvent and fluorine source 3; 5, inorganic molysite is dissolved in alcoholic solvent, obtains the alcoholic solution of iron content; After inorganic fluorine source being distributed to the alcoholic solution of iron content, solution being transferred to thermal treatment in hydrothermal reaction kettle, after cooling, obtain FeF 3.But, adopt aforesaid method to prepare FeF 3, preparation process is complicated, and production cost is high.
Summary of the invention
The object of the present invention is to provide FeF 3preparation method, to solve the above problems.
Provide FeF in an embodiment of the present invention 3preparation method, comprise the steps:
By iron ore or containing Fe 2o 3mineral mix with fluorochemical, obtain mixture;
Make mixture reaction, obtain gaseous state FeF 3.
Furthermore, make mixture reaction, obtain the FeF of gaseous state 3also comprise the steps: after step
To gaseous state FeF 3carry out collecting, cool, purification processes, obtain the FeF that purity is 99% ~ 99.99% 3.
Furthermore, step is by iron ore or containing Fe 2o 3mineral mix with fluorochemical, obtain in mixture, fluorochemical is any one in following solid-state fluoride: NaF, NH 4f, NH 4hF 2, CaF 2and AlF 3, iron ore or containing Fe 2o 3mineral and the particle diameter of solid-state fluoride be all less than 3mm.
Preferably, in step by iron ore or containing Fe 2o 3mineral mix with fluorochemical, obtain in mixture, fluorochemical mass percent is in the mixture 20% ~ 90%.
Preferably, step makes mixture reaction, obtains the FeF of gaseous state 3, specifically comprise the steps:
Mixture is pressed into base;
Pass into air, calcine, obtain gaseous state FeF 3with the mixed gas of other gaseous substance;
Mixed gas is cooled to less than 800 DEG C, obtains solid-state FeF 3with the gas-solid mixture of other gaseous substances;
Gas-solid mixture is separated, obtains solid-state FeF 3;
By solid-state FeF 3gasify, obtain gaseous state FeF 3.
Preferably, pass into air in step, calcine, obtain gaseous state FeF 3with in the mixed gas of other gaseous substance, calcining temperature is 900 DEG C ~ 1300 DEG C, and calcination time is 3h ~ 15h.
Preferably, by solid-state FeF 3gasify, obtain gaseous state FeF 3in, gasification temperature is 1000 DEG C ~ 1400 DEG C.
Furthermore, fluorochemical is hydrofluoric acid, and step is by iron ore or containing Fe 2o 3mineral mix with fluorochemical, the concrete steps obtaining mixture are:
By iron ore or containing Fe 2o 3mineral mix with hydrofluoric acid, obtain mixture, hydrofluoric acid mass percent is in the mixture 20% ~ 90%; The mass concentration of hydrofluoric acid is 20% ~ 40%.
Preferably, step makes mixture reaction, obtains gaseous state FeF 3concrete steps be:
Mixture is under 100 ~ 200 DEG C of conditions, and reaction 3h ~ 15h, generates solid-state FeF 3;
By solid-state FeF 3be warming up to 1000 DEG C ~ 1400 DEG C to gasify, obtain gaseous state FeF 3.
Preferably, iron ore or containing Fe 2o 3mineral be any one in following several material: the silicate mine of bauxitic clay, magnetite, rhombohedral iron ore, limonite, spathic iron ore, pyrites, iron, containing Fe 2o 3waste material.
The FeF of the above embodiment of the present invention 3preparation method, reaction unit well known in the art can be adopted to complete preparation process, and production craft step is simple; And adopt cheap iron ore or contain Fe 2o 3mineral and fluorochemical be main raw material, reaction conditions require low, production cost is low.
Embodiment
Below by specific embodiment, the present invention is described in further detail.
The embodiment provides FeF 3preparation method, comprise the steps:
Step 101: by iron ore or containing Fe 2o 3mineral mix with fluorochemical, obtain mixture;
Step 102: make mixture reaction, obtains gaseous state FeF 3.
The FeF provided in the embodiment of the present invention 3preparation method in, utilize fluorochemical (AF z) in F element and iron ore or contain Fe 2o 3mineral (M xo ynFe 2o 3) in close fluorine element Fe react, its reaction formula is:
M xO y·nFe 2O 3+AF z→M xO y+A 2O z+FeF 3
By above-mentioned reaction, realize to iron ore or containing Fe 2o 3mineral highly fluorinated, generate high-purity FeF of gaseous state 3.The FeF that the present embodiment provides 3preparation method, production craft step simplifies, and adopts cheap iron ore or containing Fe 2o 3mineral and fluorochemical be main raw material, therefore production cost is low.In addition, FeF prepared by the preparation method provided by the present embodiment 3particle diameter is little, inclusion-free, cleanliness factor are high, and reaction process energy consumption is low, does not have poisonous fluorine source in raw material; And require low to reaction conditions and conversion unit.
The FeF that the preparation method provided to improve the present embodiment prepares 3purity, therefore preferably after step 102, also to comprise the steps:
Step 103: to gaseous state FeF 3carry out collecting, cool, purification processes, obtain the FeF that purity is 99% ~ 99.99% 3.
Above-mentioned collection, cooling, method of purification can adopt collection well known in the art, cooling, method of purification and device to realize.
In the present embodiment, the fluorochemical in raw material can be any one in following several solid-state fluoride: NaF, NH 4f, NH 4hF 2, CaF 2and AlF 3, iron ore or containing Fe 2o 3mineral and the particle diameter of solid-state fluoride be all less than 3mm.Due to NaF, NH 4f, NH 4hF 2, CaF 2and AlF 3wide material sources, and cost is low, therefore reduce further preparation FeF 3production cost.In addition, by fluorochemical and iron ore or containing Fe 2o 3the size controlling of mineral at below 3mm, can enable two kinds of solid material compositions mixing, it is more complete that reaction is carried out, and further increases the productive rate of reaction.
When fluorochemical is solid-state fluoride, by iron ore or containing Fe 2o 3mineral and the mixture that forms of fluorochemical in, the massfraction of fluorochemical is preferably 20%-90%.More Fe can be made like this to participate in reaction, contribute to improving productive rate.In addition, in the present embodiment, the FeF of gaseous state is directly generated preferably by the mode improving temperature of reaction 3, preferably, step 102 specifically comprises the steps:
Step 10211: mixture is pressed into base;
Step 10212: pass into air, calcines, and obtains gaseous state FeF 3with the mixed gas of other gaseous substance;
Step 10213: mixed gas is cooled to less than 800 DEG C, obtains solid-state FeF 3with the gas-solid mixture of other gaseous substances;
Step 10214: be separated by gas-solid mixture, obtains solid-state FeF 3;
Step 10215: by solid-state FeF 3gasify, obtain gaseous state FeF 3.
By mixture is pressed into base, the calcining of rear operation can be made more complete, improve preparation FeF 3productive rate.Calcining is directly carried out to solid mixt and obtains gaseous state FeF 3, simplify preparation technology, improve preparation efficiency.By passing into air in calcination process, raw material can be made to calcine fully, react more complete.
In addition, can improve and prepare gaseous state FeF by controlling calcining temperature and calcination time 3purity, preferably, calcining temperature is 900 DEG C ~ 1300 DEG C, and calcination time is 3h ~ 15h.If temperature is lower than 900 DEG C, the FeF of gaseous state possibly cannot be generated 3if temperature higher than 1300 DEG C, then may generate more by product.By controlling the proportioning of calcining temperature, calcination time and raw material, can realize to iron ore or containing Fe 2o 3mineral highly fluorinated, further increase the FeF of preparation 3purity.Gaseous state FeF is finally made in order to improve further 3purity, therefore by solid-state FeF 3at the temperature of 1000 DEG C ~ 1400 DEG C, gasify, by this temperature range to solid-state FeF 3gasify, effectively can improve the gaseous state FeF finally made 3purity.
In another embodiment of the present invention, fluorochemical can also be hydrofluoric acid, and the concrete steps of step 101 are preferably by iron ore or containing Fe 2o 3mineral mix with hydrofluoric acid, obtain mixture.Hydrofluoric acid mass percent is in the mixture 20% ~ 90%.The mass concentration of hydrofluoric acid is 20% ~ 40%.Like this, iron ore can be made or contain Fe 2o 3mineral fully contact with hydrofluoric acid, the reaction making rear operation is more complete, can make iron ore or containing Fe 2o 3mineral highly fluorinated, improve preparation FeF 3productive rate.
Due in the present embodiment, iron ore or containing Fe 2o 3mineral need to react with hydrofluoric acid, particularly, the concrete steps of step 102 are preferably:
Step 10221: mixture is under 100 ~ 200 DEG C of conditions, and reaction 3h ~ 15h, generates solid-state FeF 3.
Step 10222: by solid-state FeF 3be warming up to 1000 DEG C ~ 1400 DEG C to gasify, obtain gaseous state FeF 3.
Temperature of reaction and reaction times are controlled in above-mentioned scope, reaction can be made more complete, improve and prepare gaseous state FeF 3productive rate.
In addition, the iron ore mentioned in the present invention or containing Fe 2o 3mineral can be any one in following several material: the silicate mine of bauxitic clay, magnetite, rhombohedral iron ore, limonite, spathic iron ore, pyrites, iron, containing Fe 2o 3waste material.No matter it should be noted that, raw material used in preparation method provided by the invention, be high-grade iron ore or containing Fe 2o 3mineral be raw material, or low-grade iron ore or containing Fe 2o 3mineral be raw material, all can prepare highly purified FeF 3.
Be below FeF provided by the invention 3the concrete preparation example of preparation method:
Preparation example 1: with rhombohedral iron ore and NH 4f is that high-purity FeF prepared by raw material 3
By rhombohedral iron ore and NH 4f mixes and obtains mixture, rhombohedral iron ore and NH 4the median size of F is below 3mm.NH in mixture 4the mass percent of F is 80%.By mixture 900 DEG C of calcinings 3 hours, generate gaseous state FeF 3with the mixed gas of other gaseous substance, mixed gas is cooled to less than 800 DEG C, obtains solid-state FeF 3with the gas-solid mixture of other gaseous substance.Gas-solid mixture is separated and obtains the higher solid-state FeF of purity 3, then by solid-state FeF 3gasify, gasification temperature is 1050 DEG C, obtains high-purity gaseous state FeF further 3.Due to FeF 3be gaseous state under high temperature, effusion.The FeF generated 3through high-temperature gas collection device, collection device, purifying plant obtains high purity FeF 3.Reaction equation is as follows:
Fe 2O 3+6NH 4F→2FeF 3+6NH 3+3H 2O
Preparation example 2: with limonite and AlF 3for high-purity FeF prepared by raw material 3
By limonite and AlF 3mix and obtain mixture, limonite and AlF 3median size be below 3mm.AlF in mixture 3mass percent be 60%.By mixture 800 DEG C of calcinings 6 hours, generate Al 2o 3with gaseous state FeF 3and the mixed gas of other gaseous substance, mixed gas is cooled to less than 800 DEG C, obtains solid-state FeF 3with the gas-solid mixture of other gaseous substance.Gas-solid mixture is separated and obtains the higher solid-state FeF of purity 3, then by solid-state FeF 3gasify, gasification temperature is 1250 DEG C, obtains high-purity gaseous state FeF further 3.FeF 3be gaseous state under high temperature, overflow from solid.The FeF generated 3high purity FeF is obtained by high-temperature gas collection device, refrigerating unit, purifying plant 3.Reaction equation is as follows:
Fe 2O 3+2AlF 3·3H 2O→Al 2O 3+2FeF 3+6H 2O
Preparation example 3: with spathic iron ore and NH 4hF 2for high-purity FeF prepared by raw material 3
By spathic iron ore and NH 4hF 2mix and obtain mixture, spathic iron ore and NH 4hF 2median size be about 3mm.NH in mixture 4hF 2mass percent be 40%.By the temperature lower calcination 5 hour of mixture at 700 DEG C, generate gaseous state FeF 3with the mixed gas of other gaseous substance, mixed gas is cooled to less than 800 DEG C, obtains solid-state FeF 3with the gas-solid mixture of other gaseous substance.Gas-solid mixture is separated and obtains the higher solid-state FeF of purity 3, then by FeF 3gasify, gasification temperature is 1350 DEG C, obtains high-purity gaseous state FeF further 3.FeF 3be gaseous state under high temperature, overflow from solid.High-temperature gas collection device is crossed by the borontrifluoride Tie Tong generated, refrigerating unit, purifying plant obtain high purity FeF 3.Reaction equation is as follows:
Fe 2O 3+3NH 4HF 2→2FeF 3+3NH 3+3H 2O
Preparation example 4: with magnetite and NaF for high-purity FeF prepared by raw material 3
Mixed with NaF by magnetite and obtain mixture, the median size of magnetite and NaF is about 2.8mm.In mixture, the mass percent of NaF is 35%.By the temperature lower calcination 15 hour of mixture at 1300 DEG C, generate NaOH and gaseous state FeF 3and the mixed gas of other gaseous substance, mixed gas is cooled to less than 800 DEG C, obtains solid-state FeF 3with the gas-solid mixture of other gaseous substance.Gas-solid mixture is separated and obtains the higher FeF of purity 3, then by FeF 3gasify, gasification temperature is 1400 DEG C, obtains high-purity gaseous state FeF further 3.FeF 3be gaseous state under high temperature, overflow from solid.The FeF generated 3high purity FeF is obtained by high-temperature gas collection device, refrigerating unit, purifying plant 3.Reaction equation is as follows:
Fe 2O 3+6NaF+3H 2O→2FeF 3+6NaOH
Preparation example 5: to contain Fe 2o 3waste material and CaF 2for high-purity FeF prepared by raw material 3
Will containing Fe 2o 3waste material and CaF 2mix and obtain mixture, containing Fe 2o 3waste material and CaF 2median size be below 3mm.CaF in mixture 2mass percent be 50%.By the temperature lower calcination 10 hour of mixture at 1000 DEG C, generate CaO and gaseous state FeF 3and the mixed gas of other gaseous substance, mixed gas is cooled to less than 800 DEG C, obtains solid-state FeF 3with the gas-solid mixture of other gaseous substance.Gas-solid mixture is separated and obtains the higher solid-state FeF of purity 3, then by FeF 3gasify, gasification temperature is 1300 DEG C, obtains high-purity gaseous state FeF further 3.FeF 3be gaseous state under high temperature, overflow from solid.The FeF generated 3high purity FeF is obtained by high-temperature gas collection device, refrigerating unit, purifying plant 3.Reaction equation is as follows:
Fe 2O 3+3CaF 2→2FeF 3+3CaO
Following table is the data of each preparation example in the present invention and the data synopsis of comparative example:
Can be found out by upper table, FeF provided by the invention 3preparation method there is the effects such as low cost, high quality, high yield, high purity.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (7)

1.FeF 3preparation method, it is characterized in that, comprise the steps:
Iron ore is mixed with fluorochemical, obtains mixture;
Make described mixture reaction, obtain gaseous state FeF 3;
Described fluorochemical is solid-state fluoride or hydrofluoric acid;
When described fluorochemical is solid-state fluoride, described step makes described mixture reaction, obtains gaseous state FeF 3, specifically comprise the steps: described mixture to be pressed into base; Pass into air, calcine, obtain gaseous state FeF 3with the mixed gas of other gaseous substance, wherein, described calcining temperature is 900 DEG C ~ 1300 DEG C, and calcination time is 3h ~ 15h;
Described mixed gas is cooled to less than 800 DEG C, obtains solid-state FeF 3with the gas-solid mixture of other gaseous substances; Described gas-solid mixture is separated, obtains solid-state FeF 3; By described solid-state FeF 3gasify, obtain gaseous state FeF 3;
When described fluorochemical is hydrofluoric acid, described step makes described mixture reaction, obtains gaseous state FeF 3concrete steps be:
Described mixture is under 100 DEG C ~ 200 DEG C conditions, and reaction 3h ~ 15h, generates solid-state FeF 3;
By described solid-state FeF 3be warming up to 1000 DEG C ~ 1400 DEG C to gasify, obtain gaseous state FeF 3.
2. FeF according to claim 1 3preparation method, it is characterized in that, make described mixture reaction, obtain gaseous state FeF 3also comprise the steps: after step
To described gaseous state FeF 3carry out collecting, cool, purification processes, obtain the FeF that purity is 99% ~ 99.99% 3.
3. FeF according to claim 2 3preparation method, it is characterized in that, iron ore mixes with fluorochemical by described step, obtains in mixture, and described fluorochemical is any one in following solid-state fluoride: NaF, NH 4f, NH 4hF 2, CaF 2and AlF 3, the particle diameter of described iron ore and described solid-state fluoride is all less than 3mm.
4. FeF according to claim 3 3preparation method, it is characterized in that, mixed by iron ore in described step with fluorochemical, obtain in mixture, the mass percent of described fluorochemical in described mixture is 20% ~ 90%.
5. FeF according to claim 1 3preparation method, it is characterized in that, described by described solid-state FeF 3gasify, obtain gaseous state FeF 3in, described gasification temperature is 1000 DEG C ~ 1400 DEG C.
6. FeF according to claim 1 3preparation method, it is characterized in that, described fluorochemical is hydrofluoric acid, and iron ore mixes with fluorochemical by described step, and the concrete steps obtaining mixture are:
Mixed with hydrofluoric acid by iron ore, obtain mixture, the mass percent of described hydrofluoric acid in described mixture is 20% ~ 90%; The mass concentration of described hydrofluoric acid is 20% ~ 40%.
7. the FeF according to any one of claim 1-6 3preparation method, it is characterized in that, described iron ore is any one in following several material: the silicate mine of bauxitic clay, magnetite, rhombohedral iron ore, limonite, spathic iron ore, pyrites, iron.
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CN105336946B (en) * 2015-09-28 2018-09-11 中国船舶重工集团公司第七一二研究所 A kind of preparation method of lithium ion battery ferric fluoride anode material

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