CN106986545B - Method for preparing sintered glass ceramics by non-melting process - Google Patents
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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Abstract
A method for preparing sintered glass ceramics by a non-melting process, belonging to the technical field of glass ceramics preparation. The invention adopts non-melting, spray drying and dry powder granulation processes, and prepares sintered glass ceramics by cooperating with iron phosphate obtained by recovering sodium/potassium feldspar and lithium iron phosphate, and the processes comprise acid leaching, lithium precipitation and filtration, spray drying, dry powder granulation, cloth sintering and the like. Compared with the prior art, the invention has good energy-saving effect because of adopting processes of no melting, spray drying, dry powder granulation and the like, and simultaneously solves the problems of solid waste and waste liquid disposal in the recovery process of the lithium iron phosphate because the invention adopts the recovered iron phosphate and the mixed sodium salt of the lithium iron phosphate as the raw materials of the microcrystalline glass, thereby having good environmental benefit.
Description
Technical Field
The invention belongs to the technical field of microcrystalline glass preparation, and particularly relates to a method for preparing sintered microcrystalline glass by using non-melting, spray drying and dry powder granulation processes in cooperation with ferric phosphate obtained after recovery of sodium/potassium feldspar and lithium iron phosphate.
Background
The microcrystal glass is also called glass ceramic and is a kind of polycrystal solid material containing a great deal of microcrystal phase and glass phase, which is prepared by controlling crystallization of base glass with specific composition in the heating process. Although the structure, performance and production method of the glass ceramics are different from those of glass and ceramics, the glass ceramics integrates the characteristics of glass and ceramics, not only has the basic performance of glass, but also has the polycrystalline characteristic of ceramics, and becomes a unique novel material. The microcrystalline glass has many excellent properties, low thermal expansion coefficient, high mechanical strength, high hardness, good wear resistance, and can adapt to severe environment.
The microcrystalline glass is developed to date, and a plurality of preparation methods are adopted, and a rolling method and a sintering method are generally adopted. The melting method melts the batch containing the crystal nucleus agent into glass, and then carries out nucleation and crystallization treatment to obtain the microcrystalline glass. The main process is that a certain amount of crystal nucleus agent is added into slag, the slag is melted at 1400-1500 ℃, the glass melt is formed after homogenization, and the finished product is prepared by nucleation and crystallization through an annealing process. Sintering is the process of heating a powder or powder compact to a temperature below the melting point of the essential components therein, and then cooling to room temperature at a certain rate and method. As a result of sintering, bonding between the powder particles occurs, the strength of the sintered body increases, and the agglomerates of the powder particles become agglomerates of grains, thereby obtaining the desired physical and mechanical properties of the article or material. The sintering method has the advantages of solving the problems of inseparable melting and forming, difficult control of high-temperature forming and the need of adding a crystal nucleus agent in the melting method, and being convenient for industrial production. It can adopt the traditional low-temperature forming method of ceramics to prepare products with various shapes; the water quenched glass has a high specific surface area and is more susceptible to bulk crystallization than glass made by a fusion process.
At present, solid wastes and non-metallic ores are basically adopted as raw materials of amorphous glass in China, and in order to obtain qualified microcrystalline glass products, both a rolling method and a sintering method need to melt main and auxiliary materials, and a large amount of energy is consumed in the process.
With the development of new energy automobiles in China, particularly the breakthrough of the preparation technology of lithium ion batteries, the lithium ion batteries become the main power source of the new energy automobiles. Lithium iron phosphate materials are widely applied to the fields of energy storage equipment of solar and wind power generation systems, light electric vehicles such as electric locomotives, electric bicycles, recreational vehicles, golf carts, electric boosters, cleaning vehicles and Hybrid Electric Vehicles (HEV), small-sized equipment such as electric wheelchair vehicles, electric scooter and toys (remote control electric planes, vehicles and ships), and the like. The lithium iron phosphate is the safest lithium ion battery anode material at present, and does not contain any heavy metal elements harmful to human bodies. However, the recycling value of the lithium iron phosphate battery is not high, and particularly, the problems of iron phosphate after lithium is recycled by a wet method and the disposal of sewage generated in the recycling process always become limitations on the popularization and application of the lithium iron phosphate battery.
Disclosure of Invention
The invention aims to mainly solve the defect that high energy consumption is caused by high-temperature melting of main and auxiliary materials in the traditional rolling method and sintering method, iron phosphate and mixed sodium salt generated after recovery of low-melting-point non-metallic ore and lithium iron phosphate are combined to be used as the main and auxiliary materials for producing the microcrystalline glass, advanced preparation processes such as atomization drying and dry powder granulation are adopted, and a non-melting process is adopted to prepare the microcrystalline glass product. The process not only reduces consumption, but also solves the problems of solid waste and solid-liquid disposal after the recovery of the lithium iron phosphate, synergistically promotes the development of the lithium iron phosphate battery industry, and has the advantages of short treatment process flow, simple equipment, less investment, quick implementation and obvious energy-saving effect.
A method for preparing sintered glass ceramics by a non-melting process is characterized by comprising the following specific steps:
(1) acid leaching: performing acid leaching and filtering treatment on the lithium iron phosphate to obtain acid leaching solution and acid leaching residue;
(2) lithium deposition and filtration: performing lithium precipitation and filtration on the pickle liquor obtained in the step (1) to obtain lithium slag and a lithium precipitation liquid, and returning the lithium slag to lithium for recovery;
(3) spray drying: respectively carrying out spray drying on the acid leaching residue obtained in the step (1) and the lithium precipitation solution obtained in the step (2) to obtain iron phosphate powder and mixed sodium salt;
(4) dry powder granulation: granulating the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder obtained in the step (3) in a dry powder granulator to obtain raw material granules, wherein the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder are all-300 meshes;
(5) and (3) cloth sintering: and (4) distributing the raw material particles obtained in the step (4) by using a distributing machine, and then sintering to obtain the sintered black glass ceramics.
Further, in the acid leaching process in the step (1), the mass ratio of water to the lithium iron phosphate powder is 2-3: 1, the amount of the added nitric acid is 3-5 mol/L, the amount of the added 30% hydrogen peroxide is 3-5 ml:1g of lithium iron phosphate powder, the leaching temperature is 30-60 ℃, and the leaching time is 12-36 hours.
Further, in the lithium precipitation and filtration process in the step (2), sodium bicarbonate is added as a lithium precipitation agent until no precipitation is generated in the solution, the lithium precipitation temperature is 70-90 ℃, and the lithium precipitation stirring time is 0.5-2 hours.
In the further step (4), in the dry powder granulation process, 15-30 parts of iron phosphate powder, 5-10 parts of mixed sodium salt, 10-20 parts of fluorite powder and 0.5-2 parts of cobalt oxide powder, and the balance of sodium/potassium feldspar powder, wherein the mass of the iron phosphate powder, the mixed sodium salt, the fluorite powder, the cobalt oxide powder and the sodium/potassium feldspar powder is 100 parts in total.
Further, in the sintering process in the step (5), the temperature is raised to 550-600 ℃ at a rate of 30-50 ℃/min, the temperature is maintained for 1-2 hours, and then the temperature is raised to 1100-1200 ℃ at a rate of 150-200 ℃/hour, and the temperature is maintained for 0.5-2 hours.
Compared with the prior art, the invention has good energy-saving effect because of adopting processes of no melting, spray drying, dry powder granulation and the like, and simultaneously solves the problems of solid waste and waste liquid disposal in the recovery process of the lithium iron phosphate because the invention adopts the recovered iron phosphate and the mixed sodium salt of the lithium iron phosphate as the raw materials of the microcrystalline glass, thereby having good environmental benefit.
Drawings
FIG. 1 shows a flow chart of a process for preparing sintered glass-ceramics by a non-melting process.
Detailed Description
Example 1
Performing acid leaching and filtering treatment on lithium iron phosphate to obtain acid leaching solution and acid leaching slag, wherein in the acid leaching process, the mass ratio of water to lithium iron phosphate powder is 2:1, the amount of added nitric acid is 3mol/L, the amount of added 30% hydrogen peroxide is 3ml, and the amount of added hydrogen peroxide is 1g, the leaching temperature is 30 ℃, and the leaching time is 12 hours; performing lithium precipitation and filtration on the acid leaching solution obtained by acid leaching to obtain lithium slag and a lithium precipitation solution, returning the lithium slag to lithium recovery, adding sodium bicarbonate as a lithium precipitation agent in the lithium precipitation and filtration process until the solution does not generate precipitation, wherein the lithium precipitation temperature is 70 ℃, and the lithium precipitation stirring time is 0.5 hour; respectively carrying out spray drying on acid leaching residues obtained by acid leaching and lithium precipitation liquid obtained by filtering lithium precipitation to obtain iron phosphate powder and mixed sodium salt; granulating iron phosphate powder, mixed sodium salt, cobalt oxide powder, sodium/potassium feldspar powder and fluorite powder which are respectively obtained by spray drying in a dry powder granulator to obtain raw material granules, wherein the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder are all-300 meshes, and the iron phosphate powder is 15 parts, the mixed sodium salt is 5 parts, the fluorite powder is 10 parts, the cobalt oxide powder is 0.5 part, and the sodium/potassium feldspar powder is 69.5 parts; distributing the raw material particles by using a distributing machine, sintering to obtain sintered black glass ceramics, heating to 550 ℃ at a speed of 30 ℃/min in the sintering process, preserving heat for 1 hour, heating to 1100 ℃ at a speed of 150 ℃/hour, and preserving heat for 0.5 hour.
Example 2
Performing acid leaching and filtering treatment on lithium iron phosphate to obtain acid leaching solution and acid leaching slag, wherein in the acid leaching process, the mass ratio of water to lithium iron phosphate powder is 3:1, the amount of added nitric acid is 5mol/L, the amount of added 30% hydrogen peroxide is 5ml:1g, the leaching temperature is 60 ℃, and the leaching time is 36 hours; performing lithium precipitation and filtration on the acid leaching solution obtained by acid leaching to obtain lithium slag and a lithium precipitation solution, returning the lithium slag to lithium recovery, adding sodium bicarbonate as a lithium precipitation agent in the lithium precipitation and filtration process until the solution does not precipitate, wherein the lithium precipitation temperature is 90 ℃, and the lithium precipitation and stirring time is 2 hours; respectively carrying out spray drying on acid leaching residues obtained by acid leaching and lithium precipitation liquid obtained by filtering lithium precipitation to obtain iron phosphate powder and mixed sodium salt; granulating iron phosphate powder, mixed sodium salt, cobalt oxide powder, sodium/potassium feldspar powder and fluorite powder which are respectively obtained by spray drying in a dry powder granulator to obtain raw material granules, wherein the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder are all-300 meshes, and the iron phosphate powder is 30 parts, the mixed sodium salt is 10 parts, the fluorite powder is 20 parts, the cobalt oxide powder is 2 parts, and the sodium/potassium feldspar powder is 38 parts; distributing the raw material particles by using a distributing machine, then sintering to obtain the sintered black microcrystalline glass, heating to 600 ℃ at a speed of 50 ℃/min in the sintering process, preserving heat for 2 hours, heating to 1200 ℃ at a speed of 200 ℃/hour, and preserving heat for 2 hours.
Example 3
Performing acid leaching and filtering treatment on lithium iron phosphate to obtain acid leaching solution and acid leaching slag, wherein in the acid leaching process, the mass ratio of water to lithium iron phosphate powder is 2.5:1, the amount of added nitric acid is 4mol/L, the amount of added 30% hydrogen peroxide is 4ml:1g of lithium iron phosphate powder, the leaching temperature is 40 ℃, and the leaching time is 24 hours; performing lithium precipitation and filtration on the acid leaching solution obtained by acid leaching to obtain lithium slag and a lithium precipitation solution, returning the lithium slag to lithium recovery, adding sodium bicarbonate as a lithium precipitation agent in the lithium precipitation and filtration process until the solution does not precipitate, wherein the lithium precipitation temperature is 80 ℃, and the lithium precipitation and stirring time is 1 hour; respectively carrying out spray drying on acid leaching residues obtained by acid leaching and lithium precipitation liquid obtained by filtering lithium precipitation to obtain iron phosphate powder and mixed sodium salt; granulating iron phosphate powder, mixed sodium salt, cobalt oxide powder, sodium/potassium feldspar powder and fluorite powder which are respectively obtained by spray drying in a dry powder granulator to obtain raw material granules, wherein the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder are all-300 meshes, and the iron phosphate powder is 20 parts, the mixed sodium salt is 8 parts, the fluorite powder is 15 parts, the cobalt oxide powder is 1 part, and the sodium/potassium feldspar powder is 56 parts; distributing the raw material particles by a distributing machine, sintering to obtain sintered black microcrystalline glass, heating to 580 ℃ at 40 ℃/min in the sintering process, preserving heat for 1.5 hours, heating to 1150 ℃ at 180 ℃/hour, and preserving heat for 1 hour.
Example 4
Performing acid leaching and filtering treatment on lithium iron phosphate to obtain acid leaching solution and acid leaching slag, wherein in the acid leaching process, the mass ratio of water to lithium iron phosphate powder is 2.3:1, the amount of added nitric acid is 3.5mol/L, the amount of added 30% hydrogen peroxide is 4.5ml:1g of lithium iron phosphate powder, the leaching temperature is 50 ℃, and the leaching time is 30 hours; performing lithium precipitation and filtration on the acid leaching solution obtained by acid leaching to obtain lithium slag and a lithium precipitation solution, returning the lithium slag to lithium recovery, adding sodium bicarbonate as a lithium precipitation agent in the lithium precipitation and filtration process until the solution does not precipitate, wherein the lithium precipitation temperature is 85 ℃, and the lithium precipitation and stirring time is 1.5 hours; respectively carrying out spray drying on acid leaching residues obtained by acid leaching and lithium precipitation liquid obtained by filtering lithium precipitation to obtain iron phosphate powder and mixed sodium salt; granulating iron phosphate powder, mixed sodium salt, cobalt oxide powder, sodium/potassium feldspar powder and fluorite powder which are respectively obtained by spray drying in a dry powder granulator to obtain raw material granules, wherein the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder are all-300 meshes, and 25 parts of iron phosphate powder, 5 parts of mixed sodium salt, 15 parts of fluorite powder, 1.5 parts of cobalt oxide powder and 53.5 parts of sodium/potassium feldspar powder are obtained; distributing the raw material particles by using a distributing machine, then sintering to obtain the sintered black microcrystalline glass, heating to 560 ℃ at a speed of 45 ℃/min in the sintering process, preserving heat for 1 hour, heating to 1180 ℃ at a speed of 190 ℃/hour, and preserving heat for 1.5 hours.
Example 5
Performing acid leaching and filtering treatment on lithium iron phosphate to obtain acid leaching solution and acid leaching slag, wherein in the acid leaching process, the mass ratio of water to lithium iron phosphate powder is 2.2:1, the amount of added nitric acid is 3.8mol/L, the amount of added 30% hydrogen peroxide is 4.2ml:1g of lithium iron phosphate powder, the leaching temperature is 45 ℃, and the leaching time is 20 hours; performing lithium precipitation and filtration on the acid leaching solution obtained by acid leaching to obtain lithium slag and a lithium precipitation solution, returning the lithium slag to lithium recovery, adding sodium bicarbonate as a lithium precipitation agent in the lithium precipitation and filtration process until the solution does not precipitate, wherein the lithium precipitation temperature is 85 ℃, and the lithium precipitation and stirring time is 1 hour; respectively carrying out spray drying on acid leaching residues obtained by acid leaching and lithium precipitation liquid obtained by filtering lithium precipitation to obtain iron phosphate powder and mixed sodium salt; granulating iron phosphate powder, mixed sodium salt, cobalt oxide powder, sodium/potassium feldspar powder and fluorite powder which are respectively obtained by spray drying in a dry powder granulator to obtain raw material granules, wherein the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder are all-300 meshes, 28 parts of iron phosphate powder, 6 parts of mixed sodium salt, 12 parts of fluorite powder, 0.7 part of cobalt oxide powder and 53.3 parts of sodium/potassium feldspar powder; distributing the raw material particles by using a distributing machine, then sintering to obtain the sintered black microcrystalline glass, heating to 570 ℃ at 42 ℃/min in the sintering process, preserving heat for 1.5 hours, heating to 1150 ℃ at 170 ℃/hour, and preserving heat for 1 hour.
Example 6
Performing acid leaching and filtering treatment on lithium iron phosphate to obtain acid leaching solution and acid leaching slag, wherein in the acid leaching process, the mass ratio of water to lithium iron phosphate powder is 2.8:1, the amount of added nitric acid is 3.5mol/L, the amount of added 30% hydrogen peroxide is 3.5ml:1g of lithium iron phosphate powder, the leaching temperature is 45 ℃, and the leaching time is 18 hours; performing lithium precipitation and filtration on the acid leaching solution obtained by acid leaching to obtain lithium slag and a lithium precipitation solution, returning the lithium slag to lithium recovery, adding sodium bicarbonate as a lithium precipitation agent in the lithium precipitation and filtration process until the solution does not precipitate, wherein the lithium precipitation temperature is 85 ℃, and the lithium precipitation and stirring time is 1 hour; respectively carrying out spray drying on acid leaching residues obtained by acid leaching and lithium precipitation liquid obtained by filtering lithium precipitation to obtain iron phosphate powder and mixed sodium salt; granulating iron phosphate powder, mixed sodium salt, cobalt oxide powder, sodium/potassium feldspar powder and fluorite powder which are respectively obtained by spray drying in a dry powder granulator to obtain raw material granules, wherein the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder are all-300 meshes, and the iron phosphate powder, the mixed sodium salt, the fluorite powder and the fluorite powder are 18 parts, 8 parts, 12 parts, 1.2 parts and 60.8 parts respectively; distributing the raw material particles by using a distributing machine, then sintering to obtain the sintered black microcrystalline glass, heating to 600 ℃ at a speed of 35 ℃/min in the sintering process, preserving heat for 1.5 hours, heating to 1200 ℃ at a speed of 200 ℃/hour, and preserving heat for 1 hour.
Claims (1)
1. A method for preparing sintered glass ceramics by a non-melting process is characterized by comprising the following specific steps:
(1) acid leaching: performing acid leaching and filtering treatment on the lithium iron phosphate to obtain acid leaching solution and acid leaching residue;
(2) lithium deposition and filtration: performing lithium precipitation and filtration on the pickle liquor obtained in the step (1) to obtain lithium slag and a lithium precipitation liquid, and returning the lithium slag to lithium for recovery;
(3) spray drying: respectively carrying out spray drying on the acid leaching residue obtained in the step (1) and the lithium precipitation solution obtained in the step (2) to obtain iron phosphate powder and mixed sodium salt;
(4) dry powder granulation: granulating the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder obtained in the step (3) in a dry powder granulator to obtain raw material granules, wherein the iron phosphate powder, the mixed sodium salt, the cobalt oxide powder, the sodium/potassium feldspar powder and the fluorite powder are all-300 meshes; the mixture ratio: 15-30 parts of iron phosphate powder, 5-10 parts of mixed sodium salt, 10-20 parts of fluorite powder and 0.5-2 parts of cobalt oxide powder, wherein the balance is sodium/potassium feldspar powder, and the mass of the iron phosphate powder, the mixed sodium salt, the fluorite powder, the cobalt oxide powder and the sodium/potassium feldspar powder is 100 parts in total;
(5) and (3) cloth sintering: distributing the raw material particles obtained in the step (4) by using a distributing machine, and then sintering to obtain sintered black microcrystalline glass; in the sintering process, heating to 550-600 ℃ at a speed of 30-50 ℃/min, preserving heat for 1-2 hours, heating to 1100-1200 ℃ at a speed of 150-200 ℃/hour, and preserving heat for 0.5-2 hours;
in the acid leaching process in the step (1), the mass ratio of water to the lithium iron phosphate powder is 2-3: 1, the amount of added nitric acid is 3-5 mol/L, the amount of added 30% hydrogen peroxide is 3-5 ml:1g of lithium iron phosphate powder, the leaching temperature is 30-60 ℃, and the leaching time is 12-36 hours;
and (3) adding sodium bicarbonate as a lithium precipitation agent in the lithium precipitation and filtration process in the step (2), adding the sodium bicarbonate until the solution does not produce precipitation, wherein the lithium precipitation temperature is 70-90 ℃, and the lithium precipitation stirring time is 0.5-2 hours.
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