CN102642855A - Preparation method of villiform aluminum fluoride - Google Patents
Preparation method of villiform aluminum fluoride Download PDFInfo
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- CN102642855A CN102642855A CN2012101576546A CN201210157654A CN102642855A CN 102642855 A CN102642855 A CN 102642855A CN 2012101576546 A CN2012101576546 A CN 2012101576546A CN 201210157654 A CN201210157654 A CN 201210157654A CN 102642855 A CN102642855 A CN 102642855A
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- fluoride
- ammonium
- alumnium
- hour
- aluminum
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Abstract
The invention discloses a preparation method of villiform aluminum fluoride, in order to uniformly coat the surface of a coated material with the villiform aluminum fluoride. The preparation method comprises the following operation steps of: carrying out proportioning by a stoichiometric ratio and preparing a solution by taking ammonium fluoride or ammonium fluoaluminate and aluminum salt or aluminum hydroxide as raw materials; respectively putting the solution in reactors with materials to be coated, fully stirring the solution, generating a mixed solution of aluminum fluoride and the like by chemical reaction in the reactors, putting the generated mixed solution together with the coated material in a heating furnace; introducing protective gas such as nitrogen or helium to the furnace; increasing the temperature to 400 DEG C from a room temperature within 2-3 hours and keeping the temperature for 3-5 hours; evaporating the water in the mixed solution at the temperature of about 100 DEG C; and along with the increasing of the temperature, decomposing thermal-decomposition substances into gas in the range of 100-400 DEG C and removing the gas, thus obtaining a villiform aluminum fluoride crystal which can be observed under a scanning electron microscope of fifty thousand times.
Description
Technical field
The present invention relates to a kind of preparation method of fine hair shape ALUMNIUM FLUORIDE; The surface that makes encapsulated material is the villous ALUMNIUM FLUORIDE of coating evenly, is the method for feedstock production fine hair shape ALUMNIUM FLUORIDE with Neutral ammonium fluoride or ammonium aluminum fluoride and aluminium salt (aluminum nitrate, Tai-Ace S 150 or aluminum chloride etc.) or white lake particularly.
Background technology
For battery (like lithium ion battery) positive and negative pole material or detection means; In its work and use; Particularly in the environment that fluoride aqueous solution or gas are arranged; Need with the body of protection battery material or detection means, thereby reach purpose at the material of some protectiveness of surface coated of battery plus-negative plate material or detection means to the modification and the modification of encapsulated material or detection means.General terms of settlement is that material surface is carried out granular coating or film coating at present, makes the permeability of the exchange of substance of body of material and environment for use receive influence like this.The method that adopts fine hair shape ALUMNIUM FLUORIDE to coat; Both can stablize the physico-chemical property of encapsulated material or detection means; Prevent the deterioration of encapsulated material or detection means performance, can solve the permeability problem of the exchange of substance of material or detection means main body and Working environment simultaneously again.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing fine hair shape ALUMNIUM FLUORIDE, the surface that makes encapsulated material is the villous ALUMNIUM FLUORIDE of coating evenly, solves technical problems such as the modification of encapsulated material and modifications.
A kind of preparation method of fine hair shape ALUMNIUM FLUORIDE, the practical implementation step is following:
(1) be raw material with Neutral ammonium fluoride or ammonium aluminum fluoride and aluminium salt or white lake; Said aluminium salt comprises aluminum nitrate, Tai-Ace S 150, aluminum chloride etc.; According to stoichiometric ratio batching and be prepared into solution; Put into respectively to be placed with in the reaction vessel that needs coating material and by abundant and stir, the chemical reaction that in reaction vessel, takes place is:
3 NH
4F + Al
3+ → AlF
3 + 3NH
4 +
3 NH
4F + Al(OH)
3→ AlF
3 + 3NH
3·H
2O
(NH
4)
3AlF
6 + Al
3+ → 2AlF
3 + 3 NH
4 +
(2) with after Neutral ammonium fluoride or ammonium aluminum fluoride and aluminium salt or the white lake hybrid reaction; The mixed solution and the encapsulated material that generate ALUMNIUM FLUORIDE and ammonium salt are put in the process furnace in the lump; Logical all the time nitrogen or helium etc. are made protective gas in the process furnace; In 2-3 hour from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (1) and step (2); Water in the mixed solution evaporates earlier about 100 ℃; While ALUMNIUM FLUORIDE and ammonium salt slowly crystallization form crystal, and along with the rising of temperature, the material an ammonium nitrate of its pyrolytic or ammonium sulfate or ammonium chloride or ammoniacal liquor etc. resolve into gas and are removed in 100-400 ℃ of scope; Thereby make villous aluminum fluoride crystal, this fine hair shape aluminum fluoride crystal can be observed under the ESEM more than 50,000 times.
Beneficial effect of the present invention is: the method that adopts fine hair shape ALUMNIUM FLUORIDE to coat; Both can stablize the physico-chemical property of encapsulated material or detection means; Prevent the deterioration of encapsulated material or detection means performance; Can solve again simultaneously material or detection means main body and Working environment exchange of substance the permeability problem and the ALUMNIUM FLUORIDE on encapsulated material surface evenly is coated with, thereby solution is to technical problems such as the modification of encapsulated material and modifications.The prepared fine hair shape aluminum fluoride crystal of the present invention need be observed under the ESEM more than 50,000 times.
Embodiment
Embodiment 1
A kind of preparation method of fine hair shape ALUMNIUM FLUORIDE makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, is raw material with Neutral ammonium fluoride and aluminum nitrate, specifically comprises the steps:
(1) at room temperature; With Neutral ammonium fluoride and aluminum nitrate is raw material; According to stoichiometric ratio batching and be prepared into solution respectively; Put into respectively then to be placed with in the material reaction vessel that needs to coat and also fully stir, chemical reaction takes place in reaction vessel, generate the mixing solutions of ALUMNIUM FLUORIDE and an ammonium nitrate;
The container that (2) will be loaded with mixed solution and encapsulated material is put in the process furnace, in 2-3 hour from room temperature temperature programming to 400 ℃, and insulation 3-5 hour in the time of 400 ℃;
(3) in step (2); Insulation is 0.5-1 hour in the time of 100 ℃; The water of mixed solution is evaporated earlier, and while ALUMNIUM FLUORIDE and an ammonium nitrate slowly crystallization form crystal, along with the rising of temperature; An ammonium nitrate can resolve into gas and remove in 100-400 ℃ of scope, thereby makes villous aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
Embodiment 2
A kind of method for preparing fine hair shape ALUMNIUM FLUORIDE makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, is raw material with Neutral ammonium fluoride and aluminum chloride, specifically comprises the steps:
(1) at room temperature; With Neutral ammonium fluoride and aluminum chloride raw material according to the stoichiometric ratio batching and be prepared into solution respectively; Put into respectively then to be placed with in the material reaction vessel that needs to coat and also fully stir, chemical reaction takes place in reaction vessel, generate the mixing solutions of ALUMNIUM FLUORIDE and ammonium chloride;
The container that (2) will be loaded with mixed solution and encapsulated material is put in the process furnace, in 2-3 hour from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (2); 100 ℃ of insulations 0.5-1 hour; The water of mixed solution is evaporated earlier, and while ALUMNIUM FLUORIDE and ammonium chloride slowly crystallization form crystal, along with the rising of temperature; Ammonium chloride can resolve into gas and remove in 100-400 ℃ of scope, thereby makes villous aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
Embodiment 3
A kind of method for preparing fine hair shape ALUMNIUM FLUORIDE makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, is raw material with Neutral ammonium fluoride and Tai-Ace S 150, specifically comprises the steps:
(1) at room temperature; With Neutral ammonium fluoride and Tai-Ace S 150 according to the stoichiometric ratio batching and be prepared into solution respectively; Put into respectively then to be placed with in the material reaction vessel that need coat and also fully stir the chemical reaction that in reaction vessel, takes place, the mixing solutions of generation ALUMNIUM FLUORIDE and ammonium sulfate;
The container that (2) will be loaded with mixed solution and encapsulated material is put in the process furnace, in 2-3 hour from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (2); 100 ℃ of insulations 0.5-1 hour; The water of mixed solution is evaporated earlier, and while ALUMNIUM FLUORIDE and ammonium sulfate slowly crystallization form crystal, along with the rising of temperature; Ammonium sulfate can resolve into gas and remove in 100-400 ℃ of scope, thereby makes villous aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
Embodiment 4
A kind of method for preparing fine hair shape ALUMNIUM FLUORIDE makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, is raw material with Neutral ammonium fluoride and white lake, specifically comprises the steps:
(1) at room temperature; Neutral ammonium fluoride and white lake are prepared into solution according to the stoichiometric ratio batching; Put into respectively then to be placed with in the material reaction vessel that needs to coat and and stir, chemical reaction takes place in reaction vessel, generate the mixing solutions of ALUMNIUM FLUORIDE and ammoniacal liquor by abundant;
The container that (2) will be loaded with mixed solution and encapsulated material is put in the process furnace, in 2-3 hour from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (2), 100 ℃ of insulations 0.5-1 hour, the water of mixed solution is evaporated earlier, while ALUMNIUM FLUORIDE and ammoniacal liquor slowly crystallization form crystal.Along with the rising of temperature, ammoniacal liquor can resolve into gas and remove in 100-400 ℃ of scope, thereby makes villous aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
Embodiment 5
A kind of method for preparing fine hair shape ALUMNIUM FLUORIDE makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, is raw material with ammonium aluminum fluoride and Tai-Ace S 150, specifically comprises the steps:
(1) at room temperature; With ammonium aluminum fluoride and Tai-Ace S 150 according to the stoichiometric ratio batching and be prepared into solution respectively; Put into respectively then to be placed with in the material reaction vessel that needs to coat and and stir, chemical reaction takes place in reaction vessel, generate the mixing solutions of ALUMNIUM FLUORIDE and ammonium sulfate by abundant;
The container that (2) will be loaded with solution and encapsulated material is put in the process furnace, in 2-3 hour, and from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (2), 100 ℃ of insulations 0.5-1 hour, the water of mixed solution is evaporated earlier, while ALUMNIUM FLUORIDE and ammonium sulfate slowly crystallization form crystal.Along with the rising of temperature, ammonium sulfate can resolve into gas and remove in 100-400 ℃ of scope, thereby makes fine hair shape aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
Claims (6)
1. the preparation method of a fine hair shape ALUMNIUM FLUORIDE makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, it is characterized in that comprising following operation steps:
(1) be raw material with Neutral ammonium fluoride or ammonium aluminum fluoride and aluminium salt or white lake; Said aluminium salt comprises aluminum nitrate, Tai-Ace S 150, aluminum chloride etc.; According to stoichiometric ratio batching and be prepared into solution; Put into respectively to be placed with in the reaction vessel that needs coating material and by abundant and stir, the chemical reaction that in reaction vessel, takes place is:
3 NH
4F + Al
3+ →AlF
3 +3NH
4 +
3 NH
4F + Al(OH)
3→AlF
3 +3NH
3·H
2O
(NH
4)
3AlF
6+ Al
3+→2AlF
3 +3 NH
4 + ；
(2) with after Neutral ammonium fluoride and aluminium salt or the white lake hybrid reaction; The mixed solution and the encapsulated material that generate ALUMNIUM FLUORIDE and ammonium salt are put in the process furnace in the lump; Protective gas such as logical all the time nitrogen or helium in the process furnace; In 2-3 hour from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (1) and step (2); Water in the mixed solution evaporates earlier about 100 ℃; While ALUMNIUM FLUORIDE and ammonium salt slowly crystallization form crystal, and along with the rising of temperature, the material an ammonium nitrate of its pyrolytic or ammonium sulfate or ammonium chloride or ammoniacal liquor etc. resolve into gas and are removed in 100-400 ℃ of scope; Thereby make fine hair shape aluminum fluoride crystal, this fine hair shape aluminum fluoride crystal can be observed under the ESEM more than 50,000 times.
2. the preparation method of a kind of fine hair shape ALUMNIUM FLUORIDE as claimed in claim 1 makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, it is characterized in that with Neutral ammonium fluoride and aluminum nitrate be raw material, specifically comprises the steps:
(1) at room temperature; With Neutral ammonium fluoride and aluminum nitrate raw material; According to stoichiometric ratio batching and be prepared into solution respectively; Put into respectively then to be placed with in the material reaction vessel that needs to coat and also fully stir, chemical reaction takes place in reaction vessel, generate the mixing solutions of ALUMNIUM FLUORIDE and an ammonium nitrate;
The container that (2) will be loaded with mixed solution and encapsulated material is put in the process furnace, in 2-3 hour from room temperature temperature programming to 400 ℃, and insulation 3-5 hour in the time of 400 ℃;
(3) in step (2); Insulation is 0.5-1 hour in the time of 100 ℃; The water of mixed solution is evaporated earlier, and while ALUMNIUM FLUORIDE and an ammonium nitrate slowly crystallization form crystal, along with the rising of temperature; An ammonium nitrate can resolve into gas and remove in 100-400 ℃ of scope, thereby makes fine hair shape aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
3. the preparation method of a kind of fine hair shape ALUMNIUM FLUORIDE as claimed in claim 1 makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, and it is characterized in that: with Neutral ammonium fluoride and aluminum chloride is raw material, specifically comprises the steps:
(1) at room temperature; With Neutral ammonium fluoride and aluminum chloride raw material according to the stoichiometric ratio batching and be prepared into solution respectively; Put into respectively then to be placed with in the material reaction vessel that needs to coat and also fully stir, chemical reaction takes place in reaction vessel, generate the mixing solutions of ALUMNIUM FLUORIDE and ammonium chloride;
The container that (2) will be loaded with mixed solution and encapsulated material is put in the process furnace, in 2-3 hour from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (2); 100 ℃ of insulations 0.5-1 hour; The water of mixed solution is evaporated earlier, and while ALUMNIUM FLUORIDE and ammonium chloride slowly crystallization form crystal, along with the rising of temperature; Ammonium chloride can resolve into gas and remove in 100-400 ℃ of scope, thereby makes fine hair shape aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
4. the preparation method of a kind of fine hair shape ALUMNIUM FLUORIDE as claimed in claim 1 makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, and it is characterized in that: with Neutral ammonium fluoride and Tai-Ace S 150 is raw material, specifically comprises the steps:
(1) at room temperature; With Neutral ammonium fluoride and Tai-Ace S 150 according to the stoichiometric ratio batching and be prepared into solution respectively; Put into respectively then to be placed with in the material reaction vessel that need coat and also fully stir the chemical reaction that in reaction vessel, takes place, the mixing solutions of generation ALUMNIUM FLUORIDE and ammonium sulfate;
The container that (2) will be loaded with mixed solution and encapsulated material is put in the process furnace, in 2-3 hour from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (2); 100 ℃ of insulations 0.5-1 hour; The water of mixed solution is evaporated earlier, and while ALUMNIUM FLUORIDE and ammonium sulfate slowly crystallization form crystal, along with the rising of temperature; Ammonium sulfate can resolve into gas and remove in 100-400 ℃ of scope, thereby makes fine hair shape aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
5. the preparation method of a kind of fine hair shape ALUMNIUM FLUORIDE as claimed in claim 1 makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, it is characterized in that with Neutral ammonium fluoride and white lake be raw material, specifically comprises the steps:
(1) at room temperature; Neutral ammonium fluoride and white lake are prepared into solution according to the stoichiometric ratio batching; Put into respectively then to be placed with in the material reaction vessel that needs to coat and and stir, chemical reaction takes place in reaction vessel, generate the mixing solutions of ALUMNIUM FLUORIDE and ammoniacal liquor by abundant;
The container that (2) will be loaded with mixed solution and encapsulated material is put in the process furnace, in 2-3 hour from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (2), 100 ℃ of insulations 0.5-1 hour, the water of mixed solution is evaporated earlier, while ALUMNIUM FLUORIDE and ammoniacal liquor slowly crystallization form crystal;
Along with the rising of temperature, ammoniacal liquor can resolve into gas and remove in 100-400 ℃ of scope, thereby makes fine hair shape aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
6. the preparation method of a kind of fine hair shape ALUMNIUM FLUORIDE as claimed in claim 1 makes the surface of encapsulated material evenly be coated with villous ALUMNIUM FLUORIDE, it is characterized in that with ammonium aluminum fluoride and Tai-Ace S 150 be raw material, specifically comprises the steps:
(1) at room temperature; With ammonium aluminum fluoride and Tai-Ace S 150 according to the stoichiometric ratio batching and be prepared into solution respectively; Put into respectively then to be placed with in the material reaction vessel that needs to coat and and stir, chemical reaction takes place in reaction vessel, generate the mixing solutions of ALUMNIUM FLUORIDE and ammonium sulfate by abundant;
The container that (2) will be loaded with solution and encapsulated material is put in the process furnace, in 2-3 hour, and from room temperature temperature programming to 400 ℃, and in 400 ℃ of insulations 3-5 hour;
(3) in step (2), 100 ℃ of insulations 0.5-1 hour, the water of mixed solution is evaporated earlier, while ALUMNIUM FLUORIDE and ammonium sulfate slowly crystallization form crystal;
Along with the rising of temperature, ammonium sulfate can resolve into gas and remove in 100-400 ℃ of scope, thereby makes fine hair shape aluminum fluoride crystal;
(4) in step (2) step (3), protective gas such as logical all the time nitrogen or helium in the process furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101576546A CN102642855A (en) | 2012-05-21 | 2012-05-21 | Preparation method of villiform aluminum fluoride |
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|---|---|---|---|
| CN2012101576546A CN102642855A (en) | 2012-05-21 | 2012-05-21 | Preparation method of villiform aluminum fluoride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107233903A (en) * | 2017-05-18 | 2017-10-10 | 浙江工业大学 | A kind of mechanical mixture roasting preparation method and applications of aluminum fluoride catalyst |
| CN110639463A (en) * | 2019-09-29 | 2020-01-03 | 河南省睿博环境工程技术有限公司 | Intensive fluorination reactor for producing dry-process aluminum fluoride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3941874A (en) * | 1973-02-26 | 1976-03-02 | Anaconda Aluminum Co. | Recovery of aluminum fluoride |
| CN101154727A (en) * | 2007-09-14 | 2008-04-02 | 中南大学 | Coating method of porous clad material for effectively improving rate performance of lithium nickel cobalt manganese oxygen |
-
2012
- 2012-05-21 CN CN2012101576546A patent/CN102642855A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3941874A (en) * | 1973-02-26 | 1976-03-02 | Anaconda Aluminum Co. | Recovery of aluminum fluoride |
| CN101154727A (en) * | 2007-09-14 | 2008-04-02 | 中南大学 | Coating method of porous clad material for effectively improving rate performance of lithium nickel cobalt manganese oxygen |
Non-Patent Citations (3)
| Title |
|---|
| J. M. ZHENG等: "The Effects of AlF3 Coating on the Performance of Li[Li0.2Mn0.54Ni0.13Co0.13]O2 Positive Electrode Material for Lithium-Ion Battery", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 * |
| 林和成等: "AlF3 包覆LiNi0.45Mn0.45Co0.10O2锂离子电池正极材料的结构表征和电化学性能研究", 《化学学报》 * |
| 林和成等: "The effects of quenching treatment and AlF3 coating on LiNi0.5Mn0.5O2 cathode materials for lithium-ion battery", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107233903A (en) * | 2017-05-18 | 2017-10-10 | 浙江工业大学 | A kind of mechanical mixture roasting preparation method and applications of aluminum fluoride catalyst |
| CN107233903B (en) * | 2017-05-18 | 2019-09-17 | 浙江工业大学 | A kind of mechanical mixture roasting preparation method and applications of aluminum fluoride catalyst |
| CN110639463A (en) * | 2019-09-29 | 2020-01-03 | 河南省睿博环境工程技术有限公司 | Intensive fluorination reactor for producing dry-process aluminum fluoride |
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Application publication date: 20120822 |