CN109835929B - Method for preparing flaky alpha-alumina powder by sagger calcination - Google Patents
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Abstract
The invention provides a method for preparing flaky alpha-alumina powder by sagger calcination, which relates to the technical field of inorganic nonmetallic materials and comprises the following steps: preparing flaky alumina crystal seeds of boehmite phase; taking aluminum oxide or aluminum oxide hydrate as a raw material, taking seed crystal as a template agent, taking boric acid, fluoride, silicofluoride and alkali metal oxide as mineralizers, mixing and stirring uniformly according to a certain proportion, putting into a saggar, calcining for 5-10 hours at the temperature of 1300-1700 ℃, cooling, and taking out a calcined product from the saggar; grinding and screening the calcined product to obtain the flaky alpha-alumina powder. The alpha-alumina powder prepared by the method has the crystal grain thickness of 1-5 mu m and the diameter of 8-80 mu m, does not introduce other impurities in the preparation process, has simple preparation process, low requirement on equipment and no pollution in the production process, and is very suitable for being used as a grinding and polishing material of monocrystalline silicon and glass products and also can be used as a raw material of refractory materials and toughened ceramics.
Description
Technical Field
The invention relates to the technical field of inorganic non-metallic materials, in particular to a method for preparing flaky alpha-alumina powder by sagger calcination.
Background
The alpha-alumina has excellent performances of high hardness, high melting point, oxidation resistance, high temperature resistance, corrosion resistance, good thermal conductivity, high resistivity and the like. alpha-Al2O3The common crystal morphology of (a) is spheroidal or vermicular. Flaky alumina as special alpha-Al2O3And important powder materials, the crystal morphology of which is a flat sheet. The alumina with the morphology not only has the alpha-Al, but also has special two-dimensional sheet structure and moderate surface activity2O3The high-performance glass fiber reinforced plastic has the advantages of good thermal vibration resistance, good adhesive force and light reflection capability, excellent cutting and polishing capability and obvious electromagnetic wave shielding effect. As a unique property of alpha-Al2O3The flaky alumina is applied to various fields of high-grade refractory materials, toughened ceramics, pigments, paints, cosmetics, grinding and polishing and the like.
At present, the flaky alpha-alumina used in China mainly depends on foreign import. The production method of foreign flaky alpha-alumina is to sinter alumina with mineralizer in a rotary kiln at a high temperature of more than 1500 ℃. Grinding and grading the sintered product to obtain the flaky alpha-alumina. The production method has high requirements on the lining bricks of the rotary kiln and large equipment investment. In the sintering process, because the aluminum oxide is directly contacted with flame and is rapidly melted, the hardness of the material is large, and when the material is used as a grinding and polishing material, the workpiece is easy to scratch.
The patent application No. 200610116360.3 entitled "method for preparing flaky alumina single crystal particles at low temperature", discloses a method for preparing flaky alumina single crystal particles by using calcined Al (OH)3Powder or gamma-Al2O3Amorphous alumina powder generated by the powder is used as a starting material, and then crystal seed alpha-Al is added2O3Powder, the adding amount of which is 5-20% of the total weight; taking molten salt as a synthetic medium, and calculating the dosage according to the weight ratio of 1:1-4:1 of the molten salt to the salt; then calcining the mixture at the temperature of 660-1300 ℃ for 2-8 hours, and then cooling along with the furnace to finally prepare the flaky alumina single crystal particles. In the patent, besides the calcination for 2-8 hours, the seed crystal needs to be pre-sintered for 2 hours, the raw material is ground for 2-3 hours, and the production period is longer. The molten salt is used as a synthetic medium, and the pollution in the production process is serious.
The patent application number is '201210154460.0', the invention name is 'a preparation method of flake alumina with large diameter-thickness ratio', and discloses a method for adding a molten salt, a template agent and a shaping agent into alumina powder and uniformly mixing. Loading the mixture into a crucible with a cover, reacting at a set temperature, washing off soluble salt with hot water, dissolving impurity phase in the sample with hydrofluoric acid solution, washing, and drying to obtain flake aluminum oxide. The template agent is one of kaolin, graphite, calcite and mica, and the shaping agent is one of titanium dioxide, zinc oxide, tin oxide, iron oxide and silicon oxide. The template agent used in the patent can introduce other impurities, such as kaolin and mica can introduce SiO2Carbon is introduced into the graphite, calcium is introduced into the calcite, and the like is reducedThe purity of the alumina. Also, neither the added shaping agent (e.g., titanium dioxide, zinc oxide, iron oxide, silicon oxide) can be dissolved by water, which also affects the purity of the alumina. The use of hydrofluoric acid for dissolution treatment makes the process complicated and requires high equipment. The water is used for washing out soluble salt, a large amount of water is consumed, salt-containing sewage is generated, and the pollution in the production process is serious.
The application number is '201410796522.7', the invention name is 'a method for preparing flake alumina powder', and discloses a method for preparing a green body by using industrial aluminum hydroxide or transition phase alumina powder as a raw material, adding seed crystals and a crystal grain shape control agent into the raw material powder, uniformly mixing the raw material powder and pressing the mixture into a green body. And calcining the blank at high temperature in an atmosphere containing hydrogen halide and a morphology control component, crushing the calcined blank into powder, and calcining at low temperature in an atmosphere containing hydrogen halide with higher concentration after secondary forming to obtain the flaky alumina powder with the thickness of less than 0.2 mu m and the average diameter-thickness ratio of more than 50. This patent requires a blank and two forming operations, followed by calcination and subsequent comminution. The calcination of the green body needs to be carried out in hydrogen halide atmosphere, the requirement on equipment is high, the tail gas treatment is difficult, and the whole process is complex. And the prepared flaky alumina is too thin and easy to break, and can not meet the use requirements of many fields.
Existing flaky alpha-Al2O3The production method has certain problems, if seed crystals, templates and ethanol activators are required to be added, and some calcinations can generate polluting SO3The gases, some of which are calcined in corrosive hydrogen halide atmosphere, some of which need to be presintered or the calcination temperature is too high, the energy consumption is large and the production process is complex.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the shape of the flaky alumina is strictly controlled, the industrial process is simplified, and the cost is reduced, the invention provides the method for preparing the flaky alpha-alumina powder by using the sagger for calcination, the prepared flaky alpha-alumina powder has the advantages that the crystal grain thickness can reach 1-5 mu m, the diameter can reach 8-80 mu m, the shape is uniform, the dispersity is good, the hardness of the flaky crystal is moderate, and the flaky crystal is very suitable for being used as a grinding and polishing material for monocrystalline silicon and glass products.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for preparing flaky alpha-alumina powder by sagger calcination comprises the following steps:
A. uniformly stirring and mixing aluminum hydroxide, fluoride and water according to a certain proportion, injecting the mixture into a reaction kettle, carrying out hydrothermal reaction for 2-7 hours at the temperature of 160-320 ℃, and filtering, drying and crushing the discharged material of the reaction kettle to obtain flaky alumina seed crystals;
B. taking one or more of aluminum oxide or aluminum oxide hydrate as a raw material, taking the seed crystal prepared in the step A as a template agent, taking boric acid, fluoride, silicofluoride and alkali metal oxide as mineralizers, mixing and stirring uniformly according to a certain proportion, putting into a saggar, calcining for 5-10 hours at the temperature of 1300-1700 ℃, cooling, and taking out a calcined product from the saggar;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
Further, the aluminum oxide in step B comprises: one or more of industrial alumina, gamma-alumina, delta-alumina, eta-alumina, theta-alumina and kappa-alumina.
Further, the hydrate of alumina in the step B comprises: one or more of aluminum hydroxide, bayerite and nordstrandite.
Further, the fluoride in step a and step B comprises: NH (NH)4F、NaF、KF、AlF3、LiF、CaF2、HF、ZnF2One or more of them.
Further, the silicofluoride includes: na (Na)2SiF6、CaSiF6、MgSiF6One or more of them.
Further, the alkali metal oxide in step B comprises: na (Na)2O、K2O、MgO、ZnO、Li2And one or more of O.
Further, the addition amount of the mineralizer is 0.5 to 15 percent of the total weight.
Further, the sagger in the step B comprises: clay sagger, corundum sagger and ceramic sagger.
(III) advantageous effects
The invention provides a method for preparing flaky alpha-alumina powder by saggar calcination, the alpha-alumina powder prepared by the method has the crystal grain thickness of 1-5 mu m and the diameter of 8-80 mu m, and flaky alpha-alumina powder with different diameter-thickness ratios can be prepared by adjusting the material proportion, other impurities cannot be introduced in the preparation process, the preparation process is simple, the requirement on equipment is not high, and the production process is pollution-free. The powder has uniform appearance and good dispersibility. The cost is reduced. The flaky crystal has moderate hardness, is very suitable for being used as a grinding and polishing material of monocrystalline silicon and glass products, and can also be used as a raw material of a refractory material and toughened ceramic.
Drawings
FIG. 1 is a scanning electron micrograph of the flaky alpha-alumina obtained in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a method for preparing flaky alpha-alumina powder by sagger calcination comprises the following steps:
A. uniformly mixing aluminum hydroxide, KF, NaF and water according to a certain proportion, injecting the uniformly stirred slurry into a reaction kettle, carrying out hydrothermal reaction for 4 hours at 240 ℃ to generate flaky alumina seed crystals, and filtering, drying and crushing the discharged material of the reaction kettle to prepare powdery flaky alumina seed crystals;
B. taking kappa-alumina, theta-alumina and nordstrandite as raw materials, taking the seed crystal prepared in the step A as a template, and taking boric acid, KF and Na2SiF6、Na2O is a mineralizer, the addition amount of the mineralizer is 10 percent of the total weight, the mixture is uniformly mixed and stirred, the mixture is filled into a clay sagger, the mixture is calcined for 8 hours at the temperature of 1450 ℃, and after cooling, the calcined product is taken out of the clay sagger;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
Example 2:
a method for preparing flaky alpha-alumina powder by sagger calcination comprises the following steps:
A. aluminum hydroxide, NaF and AlF3Uniformly mixing the slurry and water according to a certain proportion, injecting the uniformly stirred slurry into a reaction kettle, carrying out hydrothermal reaction for 6 hours at 180 ℃ to generate flaky alumina seed crystals, and filtering, drying and crushing the discharged material of the reaction kettle to obtain powdery flaky alumina seed crystals;
B. eta-alumina and kappa-alumina are used as raw materials, the seed crystal prepared in the step A is used as a template agent, and boric acid, NaF and CaF are used2、HF、MgSiF6MgO is used as a mineralizer, the addition amount of the mineralizer is 5 percent of the total weight, the mixture is uniformly mixed and stirred, the mixture is put into a corundum sagger and calcined for 10 hours at the temperature of 1400 ℃, and after cooling, the calcined product is taken out of the corundum sagger;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
Example 3:
a method for preparing flaky alpha-alumina powder by sagger calcination comprises the following steps:
A. aluminum hydroxide and NH4F. LiF and water are uniformly mixed according to a certain proportion, the slurry after uniform stirring is injected into a reaction kettle, hydrothermal reaction is carried out for 3 hours at 280 ℃ to generate flaky alumina crystal seeds, and the reaction kettle discharges materials, and the flaky alumina crystal seeds in powder form are prepared after filtration, drying and crushing;
B、using gamma-alumina, theta-alumina and aluminium hydroxide as raw materials, using the crystal seed prepared in the step A as a template agent, and using boric acid and NH4F、AlF3、CaSiF6、K2O is a mineralizer, the addition amount of the mineralizer is 15 percent of the total weight, the mixture is uniformly mixed and stirred, the mixture is put into a ceramic sagger and calcined for 10 hours at the temperature of 1550 ℃, and after cooling, the calcined product is taken out of the ceramic sagger;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
Example 4:
a method for preparing flaky alpha-alumina powder by sagger calcination comprises the following steps:
A. aluminum hydroxide, KF, NaF, LiF and AlF3Uniformly mixing the slurry and water according to a certain proportion, injecting the uniformly stirred slurry into a reaction kettle, carrying out hydrothermal reaction for 2 hours at 320 ℃ to generate flaky alumina seed crystals, and filtering, drying and crushing the discharged material of the reaction kettle to obtain powdery flaky alumina seed crystals;
B. taking industrial alumina, delta-alumina and bayerite as raw materials, taking the crystal seed prepared in the step A as a template, and taking boric acid, NaF, LiF and AlF3、MgSiF6MgO is used as a mineralizer, the addition amount of the mineralizer is 1.5 percent of the total weight, the materials are uniformly mixed and stirred, the mixture is put into a ceramic sagger and calcined for 5 hours at the temperature of 1700 ℃, and after cooling, the calcined product is taken out of the ceramic sagger;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
Example 5:
a method for preparing flaky alpha-alumina powder by sagger calcination comprises the following steps:
A. aluminum hydroxide and NH4F. Uniformly mixing NaF and LiF water according to a certain proportion, injecting the slurry after uniform stirring into a reaction kettle, carrying out hydrothermal reaction for 2.5 hours at 300 ℃ to generate flaky alumina seed crystals, and filtering, drying and crushing the discharged material of the reaction kettle to prepare powdery flaky alumina seed crystals;
B. using delta-alumina, eta-alumina, rho-alumina and nordstrandite as raw materials, using the seed crystal prepared in the step A as a template, and using boric acid and NH4F、NaF、Na2SiF6、Na2O is a mineralizer, the addition amount of the mineralizer is 5% of the total weight, the mixture is uniformly mixed and stirred, the mixture is loaded into a clay sagger, the mixture is calcined for 6 hours at the temperature of 1600 ℃, and after cooling, the calcined product is taken out of the clay sagger;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
Example 6:
a method for preparing flaky alpha-alumina powder by sagger calcination comprises the following steps:
A. aluminum hydroxide, KF, NaF and ZnF2Uniformly mixing the slurry and water according to a certain proportion, injecting the uniformly stirred slurry into a reaction kettle, carrying out hydrothermal reaction for 5 hours at the temperature of 200 ℃ to generate flaky alumina seed crystals, and filtering, drying and crushing the discharged material of the reaction kettle to obtain powdery flaky alumina seed crystals;
B. taking gamma-alumina, delta-alumina, eta-alumina, kappa-alumina and aluminum hydroxide as raw materials, taking the seed crystal prepared in the step A as a template agent, and taking boric acid, KF, NaF and ZnF as2、Na2SiF6、Na2O and MgO are used as mineralizers, the addition amount of the mineralizer is 15% of the total weight, the materials are uniformly mixed and stirred, the materials are put into a clay sagger and are calcined for 5 hours at the temperature of 1450 ℃, and after cooling, the calcined product is taken out of the clay sagger;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
Example 7:
a method for preparing flaky alpha-alumina powder by sagger calcination comprises the following steps:
A. aluminum hydroxide and NH4F and water are mixed evenly according to a certain proportion, the evenly stirred slurry is injected into a reaction kettle, and the hydrothermal reaction is carried out for 4 hours at the temperature of 220 ℃ to generate sheet alumina crystalFiltering, drying and crushing the discharged material of the reaction kettle to prepare powdery flaky alumina crystal seeds;
B. taking industrial alumina, gamma-alumina and bayerite as raw materials, taking the crystal seed prepared in the step A as a template agent, and taking boric acid and NH4F、MgSiF6ZnO is a mineralizer, the addition amount of the mineralizer is 3% of the total weight, the materials are uniformly mixed and stirred, the mixture is filled into a clay sagger, the mixture is calcined for 5 hours at the temperature of 1650 ℃, and after cooling, the calcined product is taken out of the clay sagger;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
In summary, the embodiment of the invention has the following beneficial effects: the alpha-alumina powder prepared by the embodiments 1-7 of the invention has the crystal grain thickness of 1-5 μm and the diameter of 8-80 μm, and has uniform and consistent appearance and good dispersibility. The flaky crystal has moderate hardness, is very suitable for being used as a grinding and polishing material of monocrystalline silicon and glass products, and can also be used as a raw material of a refractory material and toughened ceramic.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for preparing flaky alpha-alumina powder by sagger calcination is characterized by comprising the following steps:
A. uniformly stirring and mixing aluminum hydroxide, fluoride and water according to a certain proportion, injecting the mixture into a reaction kettle, carrying out hydrothermal reaction for 2-7 hours at the temperature of 160-320 ℃, and filtering, drying and crushing the discharged material of the reaction kettle to obtain flaky alumina seed crystals;
B. taking at least one of aluminum oxide or aluminum oxide hydrate as a raw material, taking the seed crystal prepared in the step A as a template agent, taking boric acid, fluoride, silicofluoride and alkali metal oxide as mineralizers, mixing and stirring uniformly according to a certain proportion, putting into a saggar, calcining for 5-10 hours at the temperature of 1300-1700 ℃, cooling, and taking out the calcined product from the saggar;
C. and D, grinding and screening the calcined product obtained in the step B to obtain the flaky alpha-alumina powder.
2. The method of claim 1, wherein the aluminum oxide in step B comprises: at least one of industrial alumina, gamma-alumina, delta-alumina, eta-alumina, theta-alumina and kappa-alumina.
3. The method of claim 1, wherein the hydrate of alumina in step B comprises: at least one of aluminum hydroxide, bayerite and nordstrandite.
4. The method for preparing flaky alpha-alumina powder according to claim 1 by sagger calcinationA method, wherein said fluoride in steps a and B comprises: NH (NH)4F、NaF、KF、AlF3、LiF、CaF2、HF、ZnF2At least one of (1).
5. The method of preparing flaky alpha-alumina powder according to claim 1, wherein the silicofluoride comprises: na (Na)2SiF6、CaSiF6、MgSiF6At least one of (1).
6. The method of claim 1, wherein the alkali metal oxide in step B comprises: na (Na)2O、K2O、Li2At least one of O.
7. The method for preparing flaky alpha-alumina powder by sagger calcination according to any one of claims 1 to 6, wherein the mineralizer is added in an amount of 0.5 to 15% by weight.
8. The method of claim 1, wherein the sagger calcination is used for preparing flaky alpha-alumina powder, the sagger in step B comprises: clay sagger and ceramic sagger.
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| CN112745105B (en) * | 2020-12-24 | 2022-06-14 | 深圳技术大学 | High-sintering-activity alumina ceramic powder and preparation method thereof |
| CN113233488B (en) * | 2021-05-08 | 2023-03-21 | 中铝山东有限公司 | Preparation method of alpha-alumina with narrow primary grain size distribution |
| CN115180641B (en) * | 2022-04-13 | 2023-05-23 | 河南天马新材料股份有限公司 | Method for preparing flaky alumina powder by explosion method |
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