CN108997010B - Zero-emission oxide ceramic powder preparation method and production system thereof - Google Patents
Zero-emission oxide ceramic powder preparation method and production system thereof Download PDFInfo
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Abstract
The invention discloses a preparation method and a production system of zero-emission oxide ceramic powder.A precursor raw material and a corresponding solvent A are placed in a reaction kettle to be heated and stirred to prepare a precursor mixed solution or sol; then adding a certain amount of precipitator to precipitate the precursor solution, or converting the precursor sol into gel through polycondensation; after the reaction is finished, adding a non-aqueous high-boiling-point solvent, distilling and recovering a low-boiling-point byproduct to obtain a mixed solution of the high-boiling-point non-aqueous solvent and the precursor precipitate or gel; finally, the target powder precipitate or xerogel is obtained through reduced pressure drying, the high boiling point non-aqueous solvent B is recovered, and the final powder is obtained through calcination. The invention has the outstanding characteristics of full recovery of byproducts, zero discharge in the whole process, simple operation and the like, thereby having wide application prospect.
Description
Technical Field
The invention belongs to the technical field of oxide ceramic powder preparation, and particularly relates to a zero-emission oxide ceramic powder preparation method and a zero-emission oxide ceramic powder production system.
Background
The oxide ceramic material generally has a series of excellent performances such as high melting point, corrosion resistance, good electrical insulation, strong oxidation resistance and the like, can be used for preparing ceramic cutters, valves, bearings, teeth, lamp covers, liquid lifting pipes, fuel cells and the like, and is widely applied in the fields of petroleum, chemical industry, food, medicine, electronics, mechanical manufacturing, architectural decoration, aerospace and the like. The ceramic technology is basically characterized in that powder is used as a raw material and is formed and sintered to form a polycrystalline sintered body. Therefore, the preparation of high quality oxide powders is a prerequisite and basis for obtaining high performance oxide ceramics.
The preparation method of the oxide ceramic powder mainly comprises a solid phase method, a liquid phase method and a gas phase method. Wherein the solid phase method has high synthesis temperature, which causes the activity of the powder to be reduced and the final quality to be poor; the gas phase method has higher requirements on equipment, and is not convenient for large-scale production; the liquid phase method is widely used because the prepared oxide ceramic powder has the advantages of uniform particle size distribution, accurate chemical components, high purity and the like. The liquid phase methods currently applied to the industrial production of oxide ceramic powder mainly include a precipitation method, a hydrolysis method and a hydrothermal method, particularly the latter two methods are currently available in mass production and can prepare high-quality powder, but unfortunately, the raw materials used in the methods usually contain chloride ions, and the chloride can cause the salt bridge effect of powder particles in the calcining process and hinder the sintering of the ceramic. In the prior art, two impurity removal methods for preparing oxide ceramic powder by using chlorine-containing raw materials are available. One is the by-product of consuming a large amount of water or alcohol for washing to remove the chlorine, which wastes not only water resources (see Journal of Alloys and Compounds 2006, volume 69-75) or consumes a large amount of alcohol (see ZL 200610005316.5), but also produces a waste liquid which seriously pollutes the environment; in addition, the salt is not formed as a by-product, and the by-product is directly removed by evaporation. The method usually has high requirements on equipment and is difficult to realize industrialization (see Journal of the American Ceramic Society, 2000, No. 83: No. 9: No. 2196,2202.), and moreover, the method has low heat transfer efficiency of solid precipitation due to the absence of a liquid phase at the later stage of evaporation, and at the moment, the precipitation activity is high, and a large amount of byproducts are adsorbed in the solid precipitation and are difficult to remove completely. Therefore, the efficient zero emission industrialization of the oxide ceramic powder prepared by using the chlorine-containing raw materials is difficult to realize.
Disclosure of Invention
The invention aims to provide a preparation method and a production system of zero-emission oxide ceramic powder, which have the advantages of simple process, environmental protection, short synthesis time and high byproduct recovery rate.
In order to solve the technical problems, the technical scheme of the invention is as follows: a preparation method of zero-emission oxide ceramic powder is characterized by comprising the following steps:
the method comprises the following steps: putting the precursor raw material and a corresponding solvent A into a reaction kettle, heating and stirring to prepare a precursor mixed solution or sol;
step two: adding a certain amount of precipitator to precipitate the precursor solution or change the precursor sol into gel through polycondensation;
step three: adding a high-boiling-point non-aqueous solvent B into the precipitate or gel obtained in the step two, and recovering a low-boiling-point byproduct after distillation to obtain a mixed solution of the high-boiling-point non-aqueous solvent B and the precursor precipitate or gel;
step four: finally, obtaining a precipitation product or xerogel of the target powder through reduced pressure drying, recovering the high-boiling point non-aqueous solvent B, and calcining to obtain the oxide ceramic powder.
In the first step, the precursor raw material is one or the combination of two of soluble salts of zirconium, yttrium, aluminum, titanium, silicon, iron and barium metals.
In the first step, the corresponding solvent A is water or a non-aqueous organic solvent with the boiling point lower than 120 ℃, and the heating and stirring temperature is 60-110 ℃. The non-aqueous organic solvent is one of ethanol, isopropanol and n-butanol.
In the second step, the precipitant is one of carbonic acid, oxalic acid and maleic acid,
in the third step, the high-boiling point non-aqueous solvent B is one of o-xylene, n-octanol, n-butyl ether and phthalic acid. The addition amount of the high-boiling point non-aqueous solvent B in the third step is as follows: and controlling the solid content of the high-boiling-point non-aqueous solvent B and the precursor precipitate or gel mixed solution to be 5-30%.
The boiling point of the low-boiling-point by-product in the third step is lower than 120 ℃, and the distillation temperature is 80-120 ℃. The boiling point of the high boiling point nonaqueous solvent B in the third step is higher than 140 ℃.
In the fourth step, the reduced pressure drying temperature is 120-140 ℃, and the calcining temperature is 650-1200 ℃.
The production system for preparing the zero-emission oxide ceramic powder is characterized in that: the production system consists of a reaction system, a slurry conveying pump, a drying system, a powder conveying belt, a calcining system and a connecting pipeline, wherein the reaction system is connected with the drying system through the slurry conveying pump, and the drying system is connected with the calcining system through the powder conveying belt; the reaction system consists of a reaction kettle, a condenser, a byproduct recovery tank, a vacuum pump and a buffer tank; the drying system consists of a dryer, a condenser, a solvent recovery tank, a vacuum unit and a buffer tank; the calcining system consists of a kiln and a flue gas treatment system.
The equipment of the production system is coated with acid corrosion resistant coating on the parts directly contacting with the raw materials.
The invention provides a novel technology for preparing oxide ceramic powder with zero emission and a production system thereof for the first time at home and abroad. There are three outstanding advantages: washing with water or alcohol is not needed. Avoids the consumption of water resource and alcohol raw material, has no waste liquid discharge and protects the environment. The bottlenecks of water resource consumption, environmental pollution and the like in the powder preparation industry are solved, and the sustainable development of the industry is realized. ② zero discharge. The byproducts and the solvent are completely recovered and are more thorough. By optimizing the precipitator, the precursor cations are precipitated, and meanwhile, byproducts such as chlorine can be evaporated and recovered along with the low-temperature solvent; the preferred high boiling point solvent does not chemically react with other materials in the system, but ensures that the temperature field of the precipitate during the removal of the by-product is uniform in the liquid phase environment of the whole system. This makes it possible to utilize the characteristic of the by-product being more volatile than the high-boiling solvent, so that the by-product can be removed by distillation. Then, the volatilization temperature of the high boiling point solvent is effectively reduced through reduced pressure drying, and the high boiling point solvent is convenient to recover. Meanwhile, the innovative scheme design greatly reduces the flammable and explosive risks of the organic solvent. ③ the recovered high boiling point solvent can be directly recycled. Really realizes the green and safe production of the oxide ceramic powder, thereby having wide market prospect.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a block diagram of a production system of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example 1 preparation of yttrium-stabilized zirconia powder
Adding 4.8kg of zirconium oxychloride, 0.098kg of yttrium oxide and 11.5L of deionized water into an enamel reaction kettle of the reaction system, dissolving at 60 ℃, adding 0.05kg of zirconium oxide seed crystal, and boiling for 5 days until gel particles are generated; then adding 13L of high-boiling point solvent o-xylene; after distillation at 110 ℃, recycling byproducts mainly comprising hydrogen chloride and deionized water to a byproduct recycling tank through a condenser, a vacuum pump and a buffer tank, so that the material does not contain harmful substances such as chloride ions and the like, and a mixed solution of o-xylene and precursor material gel particles is left; then transferring the mixed solution to an enamel double-cone dryer of a drying system through a slurry transfer pump, drying at 140 ℃ under reduced pressure, and recovering o-xylene to a solvent recovery tank by combining a condenser, a vacuum unit and a buffer tank to obtain a precursor of the stabilized zirconia powder; then the powder is sent to a kiln of a calcining system through a powder conveyer belt, heat treatment is carried out at 800 ℃ to obtain stable zirconia powder, and dust is treated through a flue gas treatment system.
Example 2 preparation of alumina powder
Weighing 10L of isopropanol, placing the isopropanol into an enamel reaction kettle of a reaction system, weighing 2kg of aluminum trichloride hexahydrate, adding the aluminum trichloride hexahydrate, heating at 110 ℃, stirring, refluxing for 4 hours, adding 10 g of PEG600 dispersant, fully stirring uniformly, and slowly adding 1.57kg of oxalic acid to generate precipitate; then adding 5L of high boiling point solvent n-butyl ether; after distillation at 120 ℃, recovering byproducts mainly comprising hydrogen chloride and isopropanol to a byproduct recovery tank through a condenser, a vacuum pump and a buffer tank; so that the material is free of harmful substances such as chloride ions and the like, and a mixed solution of n-butyl ether and precursor material gel particles is left; then transferring the mixed solution to an enamel double-cone dryer of a drying system through a slurry transfer pump, drying under reduced pressure at 130 ℃, and recovering n-butyl ether to a solvent recovery tank by combining a condenser, a vacuum unit and a buffer tank to obtain a precursor of the stable alumina powder; then the powder is conveyed to a kiln of a calcining system through a powder conveying belt, heat treatment is carried out for 2 hours at 1000 ℃ to obtain stable alumina powder, and dust is treated through a flue gas treatment system.
EXAMPLE 3 preparation of aluminum titanate powder
Measuring 10L of absolute ethyl alcohol, placing the absolute ethyl alcohol into an enamel reaction kettle of a reaction system, respectively measuring 0.55L of titanium tetrachloride and 1.334 Kg of anhydrous aluminum trichloride, heating and dissolving the titanium tetrachloride and the anhydrous aluminum trichloride in the enamel reaction kettle, and refluxing the mixture at 80 ℃ for 12 hours until gel particles are generated; then adding 5L of phthalic acid which is a high-boiling-point solvent; after distillation at 100 ℃, recycling byproducts mainly comprising hydrogen chloride and ethanol to a byproduct recycling tank through a condenser, a vacuum pump and a buffer tank, so that the materials do not contain harmful substances such as chloride ions and the like, and mixed solution of phthalic acid and precursor material gel particles is left; then transferring the mixed solution to an enamel double-cone dryer of a drying system through a slurry transfer pump, drying at 120 ℃ under reduced pressure, and recovering phthalic acid to a solvent recovery tank by combining a condenser, a vacuum unit and a buffer tank to obtain a precursor of the stable aluminum titanate powder; then the powder is sent to a kiln of a calcining system through a powder conveyer belt, heat treatment is carried out at 750 ℃ to obtain stable aluminum titanate powder, and dust is treated through a flue gas treatment system.
EXAMPLE 4 preparation of mullite powder
Measuring 20L of absolute ethyl alcohol, placing the absolute ethyl alcohol into an enamel reaction kettle of a reaction system, respectively measuring 1.12L of ethyl orthosilicate and 2.001Kg of anhydrous aluminum trichloride, heating and dissolving the ethyl orthosilicate and the anhydrous aluminum trichloride in the enamel reaction kettle, and refluxing for 12 hours at 80 ℃ until gel particles are generated; then adding 15L of high-boiling-point solvent n-butyl ether; after distillation at 80 ℃, recovering byproducts mainly comprising hydrogen chloride, ethanol and chloroethane to a byproduct recovery tank through a condenser, a vacuum pump and a buffer tank, so that the materials are free of harmful substances such as chloride ions and the like, and a mixed solution of n-butyl ether and precursor material gel particles is left; then transferring the mixed solution to an enamel double-cone dryer of a drying system through a slurry transfer pump, drying under reduced pressure at 130 ℃, and recovering n-butyl ether to a solvent recovery tank by combining a condenser, a vacuum unit and a buffer tank to obtain a precursor of the stable mullite powder; then the powder is sent to a kiln of a calcining system through a powder conveyer belt, heat treatment is carried out at 900 ℃ to obtain stable mullite powder, and dust is treated through a flue gas treatment system.
Example 5 preparation of zirconium silicate powder
Measuring 15L of n-butanol, putting the n-butanol into an enamel reaction kettle of a reaction system, respectively measuring 1.68L of ethyl orthosilicate, 0.06Kg of mineralizer lithium fluoride and 1.748Kg of anhydrous zirconium tetrachloride, heating and dissolving the mixture in the enamel reaction kettle, and refluxing the mixture at 90 ℃ for 12 hours until gel particles are generated; then adding n-octanol (5L) serving as a high-boiling-point solvent; after distillation at 110 ℃, recovering byproducts mainly comprising hydrogen chloride, n-butanol and chloroethane to a byproduct recovery tank through a condenser, a vacuum pump and a buffer tank, so that the materials do not contain harmful substances such as chloride ions and the like, and a mixed solution of n-octanol and precursor material gel particles is left; then transferring the mixed solution to an enamel double-cone dryer of a drying system through a slurry transfer pump, drying at 120 ℃ under reduced pressure, and recovering n-octanol to a solvent recovery tank by combining a condenser, a vacuum unit and a buffer tank to obtain a precursor of the stable zirconium silicate powder; then the powder is sent to a kiln of a calcining system through a powder conveyer belt, heat treatment is carried out at 650 ℃ to obtain stable zirconium silicate powder, and dust is treated through a flue gas treatment system.
Claims (6)
1. A preparation method of zero-emission oxide ceramic powder is characterized by comprising the following steps:
the method comprises the following steps: putting the precursor raw material and a corresponding solvent A into a reaction kettle, heating and stirring to prepare a precursor mixed solution or sol;
step two: adding a certain amount of precipitator to precipitate the precursor solution or change the precursor sol into gel through polycondensation;
step three: adding a high-boiling-point non-aqueous solvent B into the precipitate or gel obtained in the step two, and recovering a low-boiling-point byproduct through distillation to obtain a mixed solution of the high-boiling-point non-aqueous solvent B and the precursor precipitate or gel;
step four: finally, obtaining precipitate or xerogel of target powder through reduced pressure drying, simultaneously recovering the high-boiling point non-aqueous solvent B, and then obtaining oxide ceramic powder through calcination;
in the second step, the precipitator is one of carbonic acid, oxalic acid and maleic acid; in the third step, the high-boiling point non-aqueous solvent B is one of o-xylene, n-octanol, n-butyl ether and phthalic acid;
in the first step, the precursor raw material is one or the combination of two of soluble salts of zirconium, yttrium, aluminum, titanium, silicon, iron and barium metals;
in the first step, the corresponding solvent A is water or a non-aqueous organic solvent with the boiling point lower than 120 ℃, and the heating and stirring temperature is 60-110 ℃;
the non-aqueous organic solvent is one of ethanol, isopropanol and n-butanol.
2. The method for preparing zero-emission oxide ceramic powder according to claim 1, characterized in that: the addition amount of the high-boiling point non-aqueous solvent B in the third step is as follows: and controlling the solid content of the high-boiling-point non-aqueous solvent B and the precursor precipitate or gel mixed solution to be 5-30%.
3. The method for preparing zero-emission oxide ceramic powder according to claim 1, characterized in that: the boiling point of the low-boiling-point by-product in the third step is lower than 120 ℃, and the distillation temperature is 80-120 ℃; the boiling point of the high boiling point nonaqueous solvent B in the third step is higher than 140 ℃.
4. The method for preparing zero-emission oxide ceramic powder according to claim 1, characterized in that: in the fourth step, the temperature of the reduced pressure drying is 120-140 ℃, and the temperature of the calcining is 650-1200 ℃.
5. The production system of the zero-emission oxide ceramic powder production method according to claim 1, characterized in that: the production system consists of a reaction system, a slurry delivery pump, a drying system, a powder conveying belt, a calcining system and a connecting pipeline, wherein the reaction system consists of a reaction kettle, a condenser, a byproduct recovery tank, a vacuum pump and a buffer tank; the drying system consists of a dryer, a condenser, a solvent recovery tank, a vacuum unit and a buffer tank; the calcining system consists of a kiln and a flue gas treatment system.
6. The production system of the zero-emission oxide ceramic powder production method according to claim 5, characterized in that: the equipment of the production system is coated with acid corrosion resistant coating on the parts directly contacting with the raw materials.
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| JP2006322052A (en) * | 2005-05-19 | 2006-11-30 | Noritake Co Ltd | Method for producing metal powder |
| CN103087338A (en) * | 2013-01-18 | 2013-05-08 | 淮安科润膜材料有限公司 | Device and method for manufacturing composite perfluorinated ion exchange membrane for vanadium battery |
| CN105502492A (en) * | 2015-12-18 | 2016-04-20 | 景德镇陶瓷学院 | Method for preparing stable zirconia ultrafine powder through novel non-water-precipitation method |
| CN106365198A (en) * | 2016-09-06 | 2017-02-01 | 景德镇陶瓷大学 | Method for preparing titanium oxide nano powder at low temperature by non-water-precipitation process |
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| CN103588246A (en) * | 2012-08-13 | 2014-02-19 | 南宁市鼎发粉末冶金有限责任公司 | Preparation process for nano zirconia powder |
| CN108483492A (en) * | 2018-04-18 | 2018-09-04 | 南京工业大学 | Preparation method of zirconia aerogel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006322052A (en) * | 2005-05-19 | 2006-11-30 | Noritake Co Ltd | Method for producing metal powder |
| CN103087338A (en) * | 2013-01-18 | 2013-05-08 | 淮安科润膜材料有限公司 | Device and method for manufacturing composite perfluorinated ion exchange membrane for vanadium battery |
| CN105502492A (en) * | 2015-12-18 | 2016-04-20 | 景德镇陶瓷学院 | Method for preparing stable zirconia ultrafine powder through novel non-water-precipitation method |
| CN106365198A (en) * | 2016-09-06 | 2017-02-01 | 景德镇陶瓷大学 | Method for preparing titanium oxide nano powder at low temperature by non-water-precipitation process |
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