CN112047355B - Method for preparing aluminum borate crystal whisker by precipitation method - Google Patents
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Abstract
The invention discloses a method for preparing aluminum borate whisker by a precipitation method, which comprises the following steps: step 1: preparing an aluminum-containing compound into an aluminum-containing solution, and preparing a boron-containing compound into a boron-containing solution; step 2: mixing and stirring the solution uniformly to prepare an aluminum boron mixed solution; and step 3: dropwise adding a precipitator solution into the aluminum boron mixed solution obtained in the step 2, and continuously performing heat preservation reaction after the dropwise adding of the precipitator is finished until a mixed solution containing white precipitates is obtained; and 4, step 4: filtering the mixed solution containing the white precipitate obtained in the step 3, collecting the white precipitate, washing and drying the white precipitate to obtain aluminum borate whisker precursor powder; and 5: and (4) calcining the aluminum borate whisker precursor powder obtained in the step (4) to obtain the aluminum borate whisker powder. The method has the advantages of mild condition, cleanness, short reaction time, easy control, simple process operation, low energy consumption, low cost and environmental protection, and the obtained waste liquid can be recycled and used in the industries of fertilizer, chemical industry and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of nano whisker material products in fine chemical engineering, and relates to a method for preparing aluminum borate whisker by a precipitation method.
Background
Aluminium borate whisker (industrial Al)l8B4O33) Is an important product in boride, has excellent mechanical strength, elastic modulus, heat resistance, neutron absorption, chemical stability, corrosion resistance, electrical insulation and thermal insulation, and has mechanical properties similar to those of high-tech ceramics SiC and Si3N4Compared with the whisker, has the advantage of low cost, and is widely applied to advanced ceramic materialsHigh added value fields such as materials, metal matrix composite materials, aerospace composite materials and the like. In addition, they are also used as reinforcing materials for specialty plastics and polycarbonate resins.
The synthesis method of the aluminum borate whisker comprises a solid phase method, a gas phase method, a fluxing agent method, a melting method, a hydrothermal method, a sol-gel method and the like. In general, the solid phase method is to sinter a mixture of alumina and boron oxide at a certain temperature for a certain time to obtain aluminum borate whiskers; the gas phase method is to obtain the aluminum borate by halide of aluminum and boric acid steam at high temperature; the melting method is that the aluminum oxide and the boron oxide are melted at high temperature and cooled to generate the aluminum borate crystal whisker; the hydrothermal method is that firstly, aluminum borate gel is prepared, and then the gel is subjected to hydrothermal treatment; the sol-gel method is that aluminium salt or alcohol aluminium salt and boric acid are dissolved in water, and through hydrolysis, polymerization and other reactions, certain surfactant is used as guiding agent or template agent to form sol, which is then gelated, dried and calcined to obtain the aluminium borate whisker. The aluminum borate crystal whisker obtained by the solid phase method in the method has poor dispersibility; the growth speed of the vapor phase method is slow; the melting method has high energy consumption; the hydrothermal method has high synthesis temperature and pressure and strict requirements on equipment and other conditions; the sol-gel method has higher cost; these methods are not suitable for mass production. The fluxing agent method has the advantages of easily available raw materials, simple process, simple and convenient operation and the like, and is the main method for the current production.
The preparation of the aluminum borate whisker by the fluxing method is to add a fluxing agent into a compound capable of providing aluminum oxide and boron oxide to prepare the aluminum borate whisker. The alumina source is a substance that can be converted to alumina in a reaction, thereby ensuring that the alumina is fully reacted. As the alumina source, there can be mentioned aluminum sulfate, aluminum nitrate, aluminum chloride, sodium (potassium) aluminum sulfate and the like. The boric oxide source is a substance capable of being converted into boric oxide in a reaction, and optional boric anhydride, boric acid, sodium tetraborate, potassium pyroborate and the like are used. The fluxing agent is used for reducing the melting temperature of the system and providing environmental conditions for whisker growth, and alkali metal sulfate, halide, carbonate, nitrate and the like can be selected. The preparation method comprises the steps of mixing the compounds of the aluminum source and the boron source according to a certain proportion and adding the fluxing agent. The three are crushed and mixed evenly, placed in a crucible, put in a high-temperature furnace to be heated to 900-1200 ℃ for reaction for a certain time, and then cooled and discharged. And crushing, leaching, acidifying, drying and the like are carried out on the cooled material to obtain the final product.
However, in the flux method, the aluminum source is decomposed during the reaction process, and harmful exhaust gases such as sulfur oxide, nitrogen oxide, or chloride are generated in addition to the alumina component required for the reaction, which increases the difficulty of disposing the exhaust gas. In addition, sulfuric acid or hydrochloric acid solution is used in the leaching and acidification processes of the aluminum borate whisker, and the recovery, disposal and discharge of waste liquid of the aluminum borate whisker cause corresponding environmental problems, thereby increasing the product cost.
Disclosure of Invention
The technical problem solved by the invention is as follows: the method for preparing the aluminum borate whisker by the precipitation method has the advantages of mild condition, cleanness, short reaction time, easy control, simple process operation, low energy consumption, low cost and environmental friendliness, and the obtained waste liquid can be recycled and used in the industries of fertilizer, chemical industry and the like.
The technical scheme adopted by the invention is as follows:
a method for preparing aluminum borate whiskers by a precipitation method comprises the following steps:
step 1: preparing an aluminum-containing compound into an aluminum-containing solution, and preparing a boron-containing compound into a boron-containing solution;
step 2: mixing and stirring the solution uniformly to prepare an aluminum boron mixed solution;
and step 3: dropwise adding a precipitator solution into the aluminum boron mixed solution obtained in the step 2, and continuously performing heat preservation reaction after the dropwise adding of the precipitator is finished until a mixed solution containing white precipitates is obtained;
and 4, step 4: filtering the mixed solution containing the white precipitate obtained in the step 3, collecting the white precipitate, washing and drying the white precipitate to obtain aluminum borate whisker precursor powder;
and 5: and (4) calcining the aluminum borate whisker precursor powder obtained in the step (4) to obtain the aluminum borate whisker powder.
Preferably, the aluminum-containing compound comprises any one or more of aluminum nitrate, aluminum sulfate, aluminum ammonium sulfate, aluminum potassium sulfate, aluminum chloride, sodium metaaluminate and aluminum ammonium carbonate. In the present invention, any aluminum-containing compound soluble in water can be used.
Preferably, the boron-containing compound comprises any one or more of boric acid, sodium borate, potassium pyroborate. In the present invention, any boron-containing compound soluble in water can be used.
Preferably, the precipitant is a substance that causes aluminum ions to precipitate to form aluminum hydroxide colloid, and preferably, is one or more of sodium hydroxide, sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, ammonia water, and urea.
Preferably, the aluminum-containing solution in the step 1 is prepared by dissolving aluminum ions with the concentration of 0.01-3 mol/L in water, and the boron-containing solution in the step 1 is prepared by dissolving boron with the concentration of 0.01-1.5 mol/L in water.
Preferably, in the step 2, an aluminum boron mixed solution is obtained by mixing Al, B and (1-6) to (1-4) in the molar ratio of aluminum to boron elements.
Preferably, the molar ratio of the amount of the precipitant used in the step 3 to the aluminum ions in the aluminum-boron mixed solution in the step 2 is 0.1-4.
Preferably, in the step 3, the aluminum-boron mixed solution in the step 2 is heated at 20-100 ℃ for 10-30 minutes, a precipitator is slowly dripped, and after the dripping of the precipitator is completed, the heat preservation reaction is continuously carried out for 1-24 hours to obtain a mixed solution containing white precipitates;
preferably, the drying temperature in the step 4 is 60-200 ℃.
Preferably, the calcining condition in the step 5 is 900-1300 ℃ and calcining time is 1-24 h.
Preferably, the calcination manner in step 5 is calcination in air, in an open container or in a closed container.
The invention adopts a precipitation method process to prepare the aluminum borate whisker, wherein a precipitator firstly reacts with aluminum ions to form aluminum hydroxide colloid (flocculate), the aluminum hydroxide colloid (flocculate) has strong adsorbability, a boron source in a solution is adsorbed in the aluminum hydroxide colloid (flocculate), the colloid (flocculate) gradually forms precipitate along with the prolonging of reaction time, and then an aluminum borate whisker precursor is calcined to obtain an aluminum borate whisker product. In this process the following reactions are completed:
the first stage is as follows: aluminum source + precipitant → Al (OH)3(colloid)
The invention provides a novel green preparation method of aluminum borate whisker, which has the advantages of mild and clean conditions, simple process operation, low energy consumption, short reaction time and easy control. Firstly, uniformly mixing boron-containing solution and aluminum-containing solution, then precipitating the mixed solution by adopting a precipitator to obtain aluminum borate whisker precursor precipitate, and then filtering, washing, drying and calcining the precursor to obtain the aluminum borate whisker. According to the invention, the aluminum borate whisker precursor is prepared by adopting a precipitation method, so that toxic and harmful ions in the raw materials are removed, the emission of toxic and harmful substances to the atmosphere in a high-temperature calcination process is avoided, and the difficulty in tail gas treatment is reduced; the aluminum borate whisker precursor is prepared by a one-step precipitation method, and then the aluminum borate whisker material can be obtained by calcining, so that the procedures of crushing, leaching and acidification are omitted, the process is simple, and the waste liquid is free of pollution; the aluminum borate precursor is prepared by a precipitation method, and the obtained waste liquid can be recycled for industries such as fertilizer, chemical engineering and the like. The aluminum borate whisker prepared by the method has the advantages of complete appearance, good dispersion and high length-diameter ratio.
Drawings
FIG. 1 is an XRD pattern of aluminum borate whiskers prepared in example 1 of the present invention;
figure 2 is an SEM image of aluminum borate whiskers prepared in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following description and examples, including but not limited to the following examples.
Example 1
A method for preparing aluminum borate whiskers by a precipitation method comprises the following steps:
step 1: preparing aluminum-containing solution from aluminum chloride with the concentration of aluminum ions being 1mol/L, and preparing boron-containing solution from boric acid dissolved in water with the concentration of boron being 0.1 mol/L;
step 2: and (3) mixing the solution according to the molar ratio of Al to B as 6: 4, mixing and stirring uniformly to obtain an aluminum boron mixed solution;
and step 3: heating the aluminum boron mixed solution obtained in the step 2 at 80 ℃ for 30min, slowly dropwise adding a precipitator sodium hydroxide solution, wherein the molar ratio of sodium hydroxide to aluminum ions in the mixed solution is 3, and after dropwise adding of the precipitator sodium hydroxide, keeping the temperature to continuously react for 8h to obtain a mixed solution containing white precipitates;
and 4, step 4: filtering the mixed solution containing the white precipitate obtained in the step 3, collecting the white precipitate, washing the white precipitate, and drying at 100 ℃ to obtain aluminum borate whisker precursor powder;
and 5: and (4) putting the aluminum borate whisker precursor powder obtained in the step (4) into an open container for calcination, wherein the calcination temperature is 1000 ℃, and the calcination time is 8 hours, so as to obtain an aluminum borate whisker powder product.
Example 2
A method for preparing aluminum borate whiskers by a precipitation method comprises the following steps:
step 1: preparing aluminum nitrate and aluminum ion with the concentration of 0.01mol/L into an aluminum-containing solution, and dissolving sodium borate in water according to the boron concentration of 0.01mol/L to prepare a boron-containing solution;
step 2: and (3) mixing the solution according to the molar ratio of Al to B as 4: 1, uniformly mixing and stirring to prepare an aluminum boron mixed solution;
and step 3: heating the aluminum-boron mixed solution obtained in the step 2 at 100 ℃ for 10min, slowly dropwise adding a precipitator ammonia water solution, wherein the molar ratio of ammonia water to mixed aluminum ions is 4, and after dropwise adding of the precipitator ammonia water, keeping the temperature to continuously react for 1h to obtain a mixed solution containing white precipitates;
and 4, step 4: filtering the mixed solution containing the white precipitate obtained in the step 3, collecting the white precipitate, washing the white precipitate, and drying at 200 ℃ to obtain aluminum borate whisker precursor powder;
and 5: and (4) putting the aluminum borate whisker precursor powder obtained in the step (4) into a closed container for calcination, wherein the calcination temperature is 900 ℃, and the calcination time is 24 hours, so that the aluminum borate whisker powder product is obtained.
Example 3
A method for preparing aluminum borate whiskers by a precipitation method comprises the following steps:
step 1: preparing aluminum potassium sulfate and aluminum ion with the concentration of 3mol/L into aluminum-containing solution, and dissolving potassium pyroborate in water according to the boron concentration of 1.5mol/L to prepare boron-containing solution;
step 2: and (3) mixing the solution according to the molar ratio of Al to B as 6: 4, mixing and stirring uniformly to prepare an aluminum boron mixed solution;
and step 3: heating the aluminum boron mixed solution obtained in the step 2 at 40 ℃ for 30min, slowly dropwise adding a precipitant sodium bicarbonate solution, wherein the molar ratio of sodium bicarbonate to mixed aluminum ions is 1, and after dropwise adding of the precipitant sodium bicarbonate solution is finished, keeping the temperature to continuously react for 24h to obtain a mixed solution containing white precipitates;
and 4, step 4: filtering the mixed solution containing the white precipitate obtained in the step 3, collecting the white precipitate, washing the white precipitate, and drying at 200 ℃ to obtain aluminum borate whisker precursor powder;
and 5: and (4) putting the aluminum borate whisker precursor powder obtained in the step (4) into a closed container for calcination, wherein the calcination temperature is 1300 ℃, and the calcination time is 1h, so that the aluminum borate whisker powder product is obtained.
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (8)
1. A method for preparing aluminum borate whiskers by a precipitation method is characterized by comprising the following steps:
step 1: preparing an aluminum-containing compound into an aluminum-containing solution, and preparing a boron-containing compound into a boron-containing solution;
step 2: mixing and stirring the solution uniformly to prepare an aluminum boron mixed solution;
and step 3: heating the aluminum-boron mixed solution obtained in the step 2 at 20-100 ℃ for 10-30 minutes, slowly dropwise adding a precipitator, and after dropwise adding the precipitator, continuously preserving heat and reacting for 1-24 hours to obtain a mixed solution containing white precipitates, wherein the precipitator is one or more of sodium hydroxide, sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, ammonia water and urea;
and 4, step 4: filtering the mixed solution containing the white precipitate obtained in the step 3, collecting the white precipitate, washing and drying the white precipitate to obtain aluminum borate whisker precursor powder;
and 5: and (4) calcining the aluminum borate whisker precursor powder obtained in the step (4) to obtain the aluminum borate whisker powder.
2. The method for preparing aluminum borate whiskers by precipitation as claimed in claim 1, wherein the aluminum-containing compound comprises any one or more of aluminum nitrate, aluminum sulfate, aluminum ammonium sulfate, aluminum potassium sulfate, aluminum chloride, sodium metaaluminate and aluminum ammonium carbonate.
3. The method for preparing the aluminum borate whiskers through the precipitation method according to claim 1, wherein the boron-containing compound comprises any one or more of boric acid, sodium borate and potassium pyroborate.
4. The method for preparing the aluminum borate whiskers by the precipitation method according to any one of claims 1 to 3, wherein the aluminum-containing solution in the step 1 is prepared by dissolving 0.01 to 3mol/L of aluminum ions in water, and the boron-containing solution in the step 1 is prepared by dissolving 0.01 to 1.5mol/L of boron in water.
5. The method for preparing the aluminum borate whiskers by the precipitation method according to claim 4, wherein in the step 2, Al, B and (1-6) and (1-4) are mixed according to the molar ratio of aluminum to boron elements to obtain an aluminum-boron mixed solution.
6. The method for preparing the aluminum borate whiskers by the precipitation method according to claim 5, wherein the molar ratio of the amount of the precipitant used in the step 3 to the aluminum ions in the aluminum-boron mixed solution in the step 2 is 0.1-4.
7. The method for preparing the aluminum borate whiskers by the precipitation method according to claim 5, wherein the drying temperature in the step 4 is 60-200 ℃.
8. The method for preparing the aluminum borate whiskers by the precipitation method according to claim 7, wherein the calcination manner in the step 5 is calcination in air, an open container or a closed container, and the calcination condition is 900-1300 ℃ and 1-24 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05117100A (en) * | 1991-07-08 | 1993-05-14 | Otsuka Chem Co Ltd | Production op aluminum borate whisker |
| JP2017031016A (en) * | 2015-08-04 | 2017-02-09 | 国立大学法人室蘭工業大学 | Method for producing aluminum borate whisker |
| CN109423692A (en) * | 2017-08-26 | 2019-03-05 | 慈溪市嘉和新材料科技有限公司 | A kind of synthesis technology of aluminium borate whisker |
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- 2020-07-31 CN CN202010756140.7A patent/CN112047355B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05117100A (en) * | 1991-07-08 | 1993-05-14 | Otsuka Chem Co Ltd | Production op aluminum borate whisker |
| JP2017031016A (en) * | 2015-08-04 | 2017-02-09 | 国立大学法人室蘭工業大学 | Method for producing aluminum borate whisker |
| CN109423692A (en) * | 2017-08-26 | 2019-03-05 | 慈溪市嘉和新材料科技有限公司 | A kind of synthesis technology of aluminium borate whisker |
Non-Patent Citations (3)
| Title |
|---|
| Acid and catalytic properties of nanstoichiometric aluminum borates;Kevin P.Peil等;《Journal of Catalysis》;19890228;第115卷(第2期);第441-451页 * |
| Aluminum borates：synthesis via a precipitation process and study of their formation by DSC analysis;Andre Douy;《Solid State Sciences》;20050131;第7卷(第1期);第117-122页 * |
| The aluminum chemistry and corrosion in alkaline solutions;Jinsuo Zhang等;《Journal of Nuclear Materials》;20091231;第384卷;第175-189页 * |
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