CN114752352A - High-self-sharpening aluminum oxide abrasive powder and preparation method thereof - Google Patents
High-self-sharpening aluminum oxide abrasive powder and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of inorganic non-metallic materials for abrasive materials, and particularly relates to high-self-sharpening aluminum oxide abrasive powder and a preparation method thereof. The aluminum oxide abrasive powder prepared by the method has the appearance of a sphere-like shape with a surface provided with spikes, the shell spikes are flaky aluminum oxide, and the inner core is fused aluminum oxide, so that the aluminum oxide abrasive powder has high self-sharpening property and can effectively improve the grinding efficiency. The aluminum oxide abrasive with the multilevel morphology is synthesized for the first time, wherein the shell spike shape is synthesized in a potassium sulfate molten salt system by taking sheet-shaped sodium aluminate as a template on the basis of a spherical electric melting aluminum oxide core, and the preparation method is simple and can be industrially produced and applied.
Description
Technical Field
The invention belongs to the technical field of inorganic non-metallic materials for abrasive materials, and particularly relates to high-self-sharpening aluminum oxide abrasive powder and a preparation method thereof.
Background
An abrasive is a sharp, hard material used to make abrasive tools or used directly to abrade a workpiece. In a large family of abrasives, the consumption of corundum abrasives is the largest, and the corundum abrasives mainly comprise brown corundum, white corundum, monocrystalline corundum, chromium corundum, microcrystalline corundum and the like, have high hardness, moderate crushing resistance and self-sharpening property, and good thermal and chemical stability, and mainly comprise spherical alumina. The defects of the prior corundum abrasive are that the sharp end is easy to be abraded and has poor self-sharpening property to cause lower utilization rate of the abrasive, so that the self-sharpening property of the corundum abrasive needs to be improved to improve the grinding efficiency.
Chinese patent CN103013443B discloses an alpha-alumina-based abrasive material containing a sheet-like structure and a preparation method thereof, wherein purified water and a boehmite semi-finished product are added into a stirrer with a vacuumizing function and stirred to prepare slurry; adding dilute nitric acid with the concentration of 20%, and stirring under a vacuum state to gradually form sol and gel; drying and crushing the colloid, and screening out particles on a 120-mesh sieve; calcining the screened particles, and sintering the particles after calcining; and screening to obtain finished granules. The abrasive particles prepared by the invention have the characteristics of good self-sharpening property and long durability, but the preparation process is relatively complex and environment-friendly by adopting a sol-gel method, and Chinese patent CN101691302B discloses a method for preparing the flaky alpha-alumina particles by a molten salt method, wherein an alpha-alumina precursor is prepared by taking industrial-grade sodium aluminate as a raw material, and the flaky alpha-alumina particles are prepared by a sol-gel and ball milling mixing method in the molten salt method. The method has the advantages of simple process, high purity of the prepared product and low preparation cost. In addition, patent CN101182017A describes a method of using hydrous alumina as a raw material, mixing hydrous alumina with a fluoride salt-containing aqueous solution, and then calcining to obtain flaky alumina powder; patent CN101045543A teaches a method for obtaining ultrafine flake alumina by using coal series kaolinite rock or fly ash as raw material and performing wet chemical purification; patent CN101177549A discloses a method for obtaining flake alumina by calcining, grinding and classifying aluminum hydroxide as raw material and magnesium oxide or sodium carbonate as additive. However, due to their smaller thickness to larger aspect ratio, the flake aluminas, although being more self-sharpening, are not suitable for direct use in workpiece grinding, but are used more frequently in fillers and pearlescent pigments.
Chinese patent CN111659317A discloses a method for preparing abrasive material piled up from ultra-hard material with self-sharpening property, which integrates a hollow ceramic ball and the ultra-hard material, the ultra-hard material is in a multi-layer structure on the surface of the hollow ceramic ball, when the sharpness of the ultra-hard material is reduced, the grinding force will be gradually increased, the hollow ceramic ball will be partially broken and removed together with the dull ultra-hard abrasive material, not only the multi-layer structure is introduced into the abrasive particles, but also the self-sharpening property of the ultra-hard material is improved, but the stability of the piled up abrasive material is poor due to the heterogeneity of the ceramic ball and the ultra-hard material, and the whole structure is easy to collapse after being used for a period of time. Chinese patent CN113214790B discloses a method for preparing a hollow alumina ball-based composite abrasive, which utilizes a hollow alumina ball as a substrate, and colloid prepared by a sol-gel process is uniformly coated on the surface of the hollow alumina ball, and ceramic corundum abrasive with a microcrystalline structure is formed on the surface of the hollow alumina ball through drying and high-temperature sintering, so that the grinding performance of the abrasive is improved, and the hollow alumina ball-based composite abrasive has the advantages of extremely high sharpness, good self-sharpening property, strong shape holding power, long service life, small generated grinding heat and the like. However, the distribution preparation procedure of the substrate and the surface microcrystal is complicated, the pore channel of the hollow sphere base is blocked in the preparation process of the surface microcrystal, the appearance of the crystal gradually becomes spheroidal along with the growth of the crystal under the influence of free energy, the heat inside the sphere can not be well dissipated and can not be easily accumulated in the working process, and the hollow sphere base is poor in strength and easy to break in the grinding process.
Therefore, how to use a simple preparation method to improve the strength of the alumina abrasive powder and improve the self-sharpening property thereof is a technical problem to be solved urgently.
Disclosure of Invention
Aiming at the prior art, the invention provides high-self-sharpening aluminum oxide abrasive powder, which is specifically prepared by the following steps:
1) mixing Al (OH)3Mixing the powder and the NaOH solution, adding the mixture into a stirring reaction kettle, heating the mixture to 110-135 ℃, and reacting the mixture for 8 to 12 hours to prepare a sodium metaaluminate solution;
2) adding the sodium metaaluminate solution obtained in the step 1) into alpha-alumina powder and a citric acid solution, continuously reacting until the reaction is finished, heating to 60-80 ℃, and standing and aging for 6-8 h;
3) transferring the aged mixed solution obtained in the step 2) to a vacuum freeze dryer for drying for 12-24h to obtain the flaky sodium aluminate crystal wrapped alumina.
4) And (3) uniformly mixing the product obtained in the step 3) with potassium sulfate powder, then putting the mixture into the corundum box bowl, then placing the corundum box bowl into a high-temperature furnace, heating to 1000 and 1500 ℃, preserving the heat for 1-4h, cooling to room temperature, then taking out the crucible, and washing, filtering and drying the product in the crucible to obtain the target product.
Preferably, in step 1), said Al (OH)3The quantity ratio of Al/Na substances in the powder and NaOH solution is 1:1.1-1.2, Al (OH) 3The content is more than 98.5 percent; the concentration of the NaOH solution is 20-30 wt%.
Preferably, the alpha-alumina powder in the step 2) is fused corundum powder with the granularity of less than 150 mu m and Al2O3The content is more than 99 percent, and the concentration of the citric acid is 1-3 mol/L; sodium metaaluminate solution: electric smelting corundum powder: the mass ratio of the citric acid solution is 1: 0.8-1: 1.
Preferably, in the step 3), the vacuum freezing temperature is-20 to-40 ℃.
Preferably, the mass ratio of the product in the step 4) to the potassium sulfate powder is 1:2, and the potassium sulfate is industrial pure and has the content of more than 98%.
Preferably, the firing temperature in step 4) is 1150-1220 ℃, at which the alpha-alumina phase content is high.
The invention has the beneficial effects that: the aluminum oxide abrasive powder prepared by the method has the appearance of a sphere-like shape with a surface provided with spikes, the shell spikes are flaky aluminum oxide, and the inner core is fused aluminum oxide, so that the aluminum oxide abrasive powder has high self-sharpening property and can effectively improve the grinding efficiency. The aluminum oxide abrasive with the multilevel morphology is synthesized for the first time, wherein the shell spike shape is synthesized in a potassium sulfate molten salt system by taking sheet-shaped sodium aluminate as a template on the basis of a spherical electric melting aluminum oxide core, and the preparation method is simple and can be industrially produced and applied.
Drawings
FIG. 1 is a schematic diagram of a precursor of flaky sodium aluminate crystal-coated alumina in example 1;
FIG. 2 is a TEM image of the high self-sharpening alumina abrasive powder prepared in example 1;
FIG. 3 is a TEM image of a spheroidal alumina abrasive powder prepared in comparative example 1.
Detailed Description
The following examples are intended to illustrate the practice and advantageous effects of the present invention, but are not to be construed as limiting the scope of the present invention.
Example 1
Mixing Al/Na substances in a weight ratio of 1: 1.1 of Al (OH)3Adding the powder and a NaOH solution into a stirring reaction kettle, heating to 120 ℃, and reacting for 8 hours to prepare a sodium metaaluminate solution; weighing the sodium metaaluminate, the alpha-alumina powder and the citric acid solution according to the mass ratio of 1:0.8:1, adding the weighed alpha-alumina powder and citric acid solution into the sodium metaaluminate solution, uniformly stirring, heating to 70 ℃, standing and aging; and then the aged mixed solution is placed in a vacuum freeze dryer to be dried for 24 hours at the temperature of minus 20 ℃ to obtain the flake sodium aluminate crystal coated alumina precursor (see the attached figure 1 of the specification). Uniformly mixing the precursor and potassium sulfate powder in a weight ratio of 1:2, then loading the mixture into a corundum box bowl, then placing the corundum box bowl into a high-temperature furnace, heating to 1180, preserving heat for 3 hours, cooling to room temperature, taking out a crucible, taking out a product in the crucible, and washing, filtering and drying to obtain a target product (see the attached figure 2 of the specification).
Example 2
Mixing Al/Na substances in a mass ratio of 1: 1.2 of Al (OH)3Adding the powder and NaOH solution into a stirring reaction kettle, heating to 120 ℃, and reacting for 8 hours to prepare sodium metaaluminate solution; weighing the sodium metaaluminate, the alpha-alumina powder and the citric acid solution according to the mass ratio of 1:0.9:1, adding the weighed alpha-alumina powder and citric acid solution into the sodium metaaluminate solution, uniformly stirring, heating to 80 ℃, standing and aging; and then placing the aged mixed solution into a vacuum freeze dryer to dry for 24 hours at the temperature of minus 30 ℃ to obtain the flaky sodium aluminate crystal wrapped alumina precursor. Uniformly mixing the precursor and potassium sulfate powder according to the weight ratio of 1:2, then loading the mixture into a corundum box bowl, placing the corundum box bowl into a high-temperature furnace, and heating to 1200 ℃ for preservationAnd after the temperature is kept for 2 hours, cooling to room temperature, taking out the crucible, taking out a product in the crucible, and washing, filtering and drying to obtain the target product.
Example 3
Mixing Al/Na substances in a weight ratio of 1: 1.2 of Al (OH)3Adding the powder and a NaOH solution into a stirring reaction kettle, heating to 120 ℃, and reacting for 8 hours to prepare a sodium metaaluminate solution; weighing the sodium metaaluminate, the alpha-alumina powder and the citric acid solution according to the mass ratio of 1:1:1, adding the weighed alpha-alumina powder and citric acid solution into the sodium metaaluminate solution, uniformly stirring, heating to 80 ℃, standing and aging; and then placing the aged mixed solution into a vacuum freeze dryer to dry for 12 hours at the temperature of minus 40 ℃ to obtain the flaky sodium aluminate crystal wrapped alumina precursor. Uniformly mixing the precursor and potassium sulfate powder in a weight ratio of 1:2, then loading the mixture into a corundum box bowl, placing the corundum box bowl in a high-temperature furnace, heating to 1220, preserving heat for 2 hours, cooling to room temperature, taking out a crucible, taking out a product in the crucible, and washing, filtering and drying to obtain a target product.
Comparative example 1
(1) Preparing gel: weighing 200g of pseudo-boehmite, adding 550ml of deionized water, carrying out ball milling in a ball milling tank for 2h, taking out slurry, heating in a water bath at 75 ℃, slowly adding 80ml of dilute nitric acid (the volume ratio of water to concentrated nitric acid is 1:7, and the concentration of the concentrated nitric acid is 65%), stirring for 20min, and rapidly adding 600 ml of a magnesium nitrate, lanthanum nitrate and iridium nitrate mixed solution (wherein the concentrations of the magnesium nitrate, the lanthanum nitrate and the iridium nitrate are respectively 0.03, 0.01 and 0.01mol/L) to prepare a dilute colloid for later use;
(2) gluing: weighing 1000g of fused corundum powder alpha-alumina powder with the granularity of less than 150 mu m, then weighing 150g of the dilute colloid prepared in the step 1), mixing the dilute colloid and the alumina powder, and finishing the whole gluing process after the colloid is completely adsorbed on the surface of the fused corundum powder;
(3) and (3) drying: putting the colloid-coated fused corundum powder in an enamel tray, drying for 8h in a drying oven at 75 ℃, taking out, checking whether adhesion exists, and screening and separating if adhesion exists. Obtaining the dried electrofusion corundum powder with the colloidal particle adhesion layer;
(4) firing in a furnace: and (2) placing the dried electro-fused corundum powder with the colloidal particle adhesion layer into a muffle furnace for burning, wherein the temperature of the furnace is increased from room temperature to 800 ℃, the temperature increasing speed is 30 ℃/h, the temperature is kept for 2h at 800 ℃, then the temperature is increased to 1300 ℃, the temperature increasing speed is 100 ℃/h, the temperature is kept for 0.5h at 1300 ℃, then the furnace is cooled to room temperature, and the spheroidal alumina is obtained after being taken out of the furnace (see the attached figure 3 of the specification).
Comparative example 2
Mixing Al/Na substances in a mass ratio of 1: 1.1 of Al (OH)3Adding the powder and NaOH solution into a stirring reaction kettle, heating to 120 ℃, and reacting for 8 hours to prepare sodium metaaluminate solution; weighing the sodium metaaluminate, the alpha-alumina powder and the citric acid solution according to the mass ratio of 1:0.1:1, adding the weighed alpha-alumina powder and citric acid solution into the sodium metaaluminate solution, uniformly stirring, and then placing in a vacuum freeze dryer to dry for 24 hours at the temperature of minus 20 ℃ to obtain an alumina precursor. Uniformly mixing the precursor and potassium sulfate powder in a weight ratio of 1:2, then loading the mixture into a corundum box bowl, then placing the corundum box bowl into a high-temperature furnace, heating to 1180, keeping the temperature for 3 hours, cooling to room temperature, taking out a crucible, taking out a product in the crucible, washing with water, performing suction filtration, and drying to obtain a product, namely flaky alumina.
Claims (6)
1. The high-self-sharpening aluminum oxide abrasive powder is prepared by the following steps:
1) mixing Al (OH)3Mixing the powder and a NaOH solution, adding the mixture into a stirring reaction kettle, heating to 110-135 ℃, and reacting for 8-12h to prepare a sodium metaaluminate solution;
2) adding the sodium metaaluminate solution obtained in the step 1) into alpha-alumina powder and a citric acid solution, continuously reacting until the reaction is finished, heating to 60-80 ℃, and standing and aging for 6-8 h;
3) transferring the aged mixed solution obtained in the step 2) to a vacuum freeze dryer for drying for 12-24h to obtain a product, namely flaky sodium aluminate crystal-coated alumina;
4) Uniformly mixing the product obtained in the step 3) with potassium sulfate powder, then putting the mixture into a corundum box bowl, then placing the corundum box bowl in a high-temperature furnace, heating to 1000-1500 ℃, preserving the heat for 1-4h, cooling to room temperature, then taking out the crucible, and washing, filtering and drying the product in the crucible to obtain the target product.
2. The abrasive powder of claim 1, wherein in step 1), the Al (OH) is added3The amount ratio of Al/Na substances in the powder and NaOH solution is 1:1.1-1.2, Al (OH)3，Al(OH)3The content is more than 98.5 percent; the concentration of the NaOH solution is 20-30 wt%.
3. The high self-sharpening aluminum oxide abrasive powder according to claims 1-2, wherein the alpha-aluminum oxide powder in step 2) is fused corundum powder, Al2O3The content is more than 99 percent, and the concentration of the citric acid is 1-3 mol/L; sodium metaaluminate solution: alpha-alumina powder: the mass ratio of the citric acid solution is 1: 0.8-1: 1.
4. The high self-sharpening aluminum oxide abrasive powder according to claims 1 to 3, wherein the vacuum freezing temperature in the step 3) is from-20 ℃ to-40 ℃.
5. The high self-sharpening aluminum oxide abrasive powder as claimed in claims 1 to 4, wherein the mass ratio of the product in the step 3) to the potassium sulfate powder is 1:2, and the potassium sulfate is industrially pure and has a content of more than 98%.
6. The high self-sharpening alumina abrasive powder as defined in claim 1-5, wherein the sintering temperature in step 4) is 1150-1220 ℃, and the alpha-alumina phase content is high.
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