CN115321943A - Ceramic composite grinding medium and preparation method thereof - Google Patents
Ceramic composite grinding medium and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ceramic composite grinding medium and a preparation method thereof, relating to the field of ceramic composite grinding media, wherein the ceramic composite grinding medium is obtained by taking a metal grinding medium as a metal core, grinding the outer surface of the metal core, coating a composite ceramic layer on the outer surface of the ground metal core, putting the metal core into a ball forming machine, rolling to form a ball, polishing, drying and sintering, and the problems of high manufacturing cost and lower hardness of the existing grinding medium are solved; use of a metal core increases the hardness of the ceramic composite grinding media, with Si0 dispersed in the grinding media 2 Absorbable grinding mediumImpact energy of micro cracks in the ceramic body, crack expansion is prevented, and B is in the process of sintering and temperature rising 4 C is oxidized to generate chemical bonding force with high bonding energy, and B is generated in a molten state 2 0 3 Can flow to the crack of the ceramic interface to inhibit the crack from diffusing, so that the ceramic interface is more densified, thereby achieving the aim that the grinding medium is not easy to crack in the grinding process.
Description
Technical Field
The invention relates to the field of ceramic composite grinding media, in particular to a ceramic composite grinding medium and a preparation method thereof.
Background
Along with the requirement on the fineness of materials, the use of sand mills is more and more common, the types of grinding media in the market are more, and the grinding media can be divided into glass grinding media, ceramic grinding media, steel grinding media and the like according to different materials, wherein the ceramic grinding media have the advantages of high mechanical strength, high hardness, high density, good high-temperature performance, no pollution to materials, strong acid-base corrosion resistance, excellent wear resistance and the like, so that the ceramic grinding media occupy a very important place in the field of grinding media and are widely applied to the related fine processing fields of mineral products, chemical industry, paint, mechanical electronics and the like;
the ceramic grinding medium mainly comprises zirconium silicate grinding medium, zirconium dioxide grinding medium, aluminum dioxide grinding medium, rare earth metal stabilized zirconium dioxide bead grinding medium, silicon carbide grinding medium and the like, but the existing grinding medium is high in price, high in manufacturing cost, free of market advantage, low in wear resistance and hardness and prone to cracking in the grinding process.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a ceramic composite grinding medium and a preparation method thereof:
(1) The metal grinding medium is used as a metal core, the outer surface of the metal core is ground, the ground outer surface of the metal core is coated with a composite ceramic layer, the metal core is put into a ball forming mill to be rolled into a ball shape, polished and dried, pressed into a blank by isostatic pressing, and put into a high-temperature kiln to obtain the ceramic composite grinding medium, so that the problems that the existing grinding medium is high in price, high in manufacturing cost, free of market advantage and low in hardness are solved;
(2) Adding 2, 3-diaminotoluene into a three-neck flask, adding solvent N, N-dimethylacetamide, adding dried pyromellitic dianhydride to obtain an intermediate A, and adding SiO 2 And B 4 C, uniformly mixing, adding a silane coupling agent, and adding a solvent ethanol to obtain an intermediate BThe intermediate B is added into the intermediate A and sintered to obtain the sintering aid, so that the problems that the existing grinding medium is low in hardness and easy to crack in the grinding process are solved;
(3) Adding a catalyst into a high-pressure reaction kettle, adding 3-methyl-3-butylene-1-alcohol, adding 1, 2-butylene oxide and ethylene oxide to obtain an intermediate C, adding acetic anhydride into the intermediate C, adding an antioxidant to obtain an intermediate D, adding high-hydrogen silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane into a round-bottom flask, adding a catalyst, adding sodium bicarbonate to obtain an intermediate E, performing low-boiling-point substance removal pretreatment on the intermediate E, adding the intermediate D, the catalyst and the antioxidant into the round-bottom flask, and dropwise adding the intermediate E to obtain the dispersing agent.
The purpose of the invention can be realized by the following technical scheme:
a ceramic composite grinding medium, prepared by the following steps:
s1: taking a metal grinding medium as a metal core, and grinding the outer surface of the metal core;
s2: coating the outer surface of the polished metal core with a composite ceramic layer, stirring and dispersing for 1-2h at the rotation speed of 800-1000r/min, putting into a ball forming mill, rolling to form a ball, polishing, and drying for 1-2h at 40-50 ℃;
s3: pressing into a blank by adopting isostatic pressing, placing the blank into a high-temperature kiln, firing at the heating rate of 5-10 ℃/min, keeping the temperature for 1-2h when the temperature is raised to 800-1000 ℃, then firing at the heating rate of 3-5 ℃/min, keeping the temperature for 0.1-0.5h when the temperature is raised to 1200-1250 ℃, and naturally cooling and annealing to obtain the ceramic composite grinding medium;
the composite ceramic layer in the step S2 comprises the following components in parts by weight:
10-20 parts of kaolin, 10-20 parts of silicon carbide, 10-20 parts of feldspar, 3-5 parts of wollastonite, 5-7 parts of calcium oxide, 10-15 parts of zirconia, 2-3 parts of sodium dodecyl benzene sulfonate, 5-8 parts of a dispersing agent, 5-10 parts of a sintering aid, 3-5 parts of polyvinyl alcohol and 40-60 parts of water;
the sintering aid is prepared by the following steps:
s11: adding 2, 3-diaminotoluene into a three-neck flask, controlling the temperature at 10-11 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 5-6 hours to obtain an intermediate A;
s12: mixing SiO 2 And B 4 C, uniformly mixing, adding a silane coupling agent, adding a solvent ethanol, stirring for 1.5-2.5h, performing ultrasonic dispersion for 0.5-2h, and transferring to a drying oven at 85-95 ℃ for drying for 3-4h to obtain an intermediate B;
s13: and adding the intermediate B into the intermediate A, stirring for 1-2h, heating to 180-190 ℃ at the speed of 5 ℃/min, preserving heat for 1-1.5h, heating to 260-270 ℃ at the speed of 1-3 ℃/min, preserving heat for 1.5-2.5h, and naturally cooling to room temperature to obtain the sintering aid.
As a further scheme of the invention: the molar ratio of the 2, 3-diaminotoluene to the pyromellitic dianhydride in step S11 is 1.2-1.3:1.
as a further scheme of the invention: siO in step S12 2 、B 4 The using ratio of C to the silane coupling agent is 10g:10g:1g, wherein the dosage ratio of the intermediate A to the intermediate B in the step S13 is 1g:1g of the total weight of the composition.
As a further scheme of the invention: the dispersant is prepared by the following steps:
s41: adding a catalyst into a high-pressure reaction kettle, adding 3-methyl-3-butene-1-ol, pumping out air in the kettle at room temperature, adding 1, 2-epoxybutane, reacting at 110-120 ℃ for 3-5h, adding ethylene oxide, reacting at 100-110 ℃ for 2-3h, cooling after complete reaction, and discharging to obtain an intermediate C;
the chemical reaction formula is as follows:
s42: adding acetic anhydride into the intermediate C, heating to 140-145 ℃, and reacting2-3h, after the reaction is finished, N is used 2 Vacuum stripping, removing residual anhydride, adding antioxidant, reacting at 80-95 deg.C for 1-3h, and performing antioxidant treatment to obtain intermediate D;
the chemical reaction formula is as follows:
s43: adding high hydrogen-containing silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane into a round-bottom flask, adding a catalyst, stirring for reaction for 3-5h, standing, separating out the catalyst at the lower layer, adding sodium bicarbonate, and stirring for reaction for 0.5-1.5h at room temperature to obtain an intermediate E;
s44: and (2) carrying out low-boiling-point substance removal pretreatment on the intermediate E, adding the intermediate D, a catalyst and an antioxidant into a round-bottom flask with an electric stirrer and a thermometer, uniformly mixing, heating to 40-50 ℃, dropwise adding the intermediate E, controlling the dropwise adding speed to be 1-2 drops/s, carrying out reaction heat release after an induction period of 10-15min, and controlling the system temperature to be 65-70 ℃ for carrying out heat preservation reaction for 2-2.5h to obtain the dispersing agent.
As a further scheme of the invention: in step S41, the catalyst is potassium hydroxide, the catalyst is 0.3-0.4% of the total mass of the 3-methyl-3-butene-1-ol, the 1, 2-butylene oxide and the ethylene oxide, and the molar ratio of the 4-pentene-1-ol, the 1, 2-butylene oxide and the ethylene oxide is 1:1.5:1.
as a further scheme of the invention: in the step S42, the antioxidant is an aromatic amine antioxidant, the dosage of the antioxidant is 0.3 percent of the total mass of acetic anhydride and the intermediate E, and the molar ratio of the acetic anhydride to the intermediate C is 1:1.
as a further scheme of the invention: in the step S43, the catalyst is concentrated sulfuric acid with a mass fraction of 98%, the usage amount of the catalyst is 2% of the total mass of the high hydrogen-containing silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane, the usage amount of the sodium bicarbonate is 1% of the total mass of the high hydrogen-containing silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane, and the usage amount ratio of the high hydrogen-containing silicone oil, the octamethylcyclotetrasiloxane and the hexamethyldisiloxane is 19.1g:78.4g:1.5g.
As a further scheme of the invention: in the step S44, the catalyst is chloroplatinic acid, the antioxidant is an aromatic amine antioxidant, the dosage of the catalyst is 11% of the total mass of the intermediate D and the intermediate E, the dosage of the antioxidant is 1% of the total mass of the intermediate D and the intermediate E, and the dosage ratio of the intermediate D to the intermediate E is 25g:11g.
A preparation method of a ceramic composite grinding medium comprises the following steps:
s1: taking a metal grinding medium as a metal core, and grinding the outer surface of the metal core;
s2: coating the outer surface of the polished metal core with a composite ceramic layer, stirring and dispersing for 1-2h at the rotation speed of 800-1000r/min, then putting into a ball forming mill, rolling to form balls, polishing, and drying for 1-2h at 40-50 ℃;
s3: pressing into a blank by isostatic pressing, placing the blank into a high-temperature kiln, firing at the heating rate of 5-10 ℃/min, keeping the temperature for 1-2h when the temperature is raised to 800-1000 ℃, then firing at the heating rate of 3-5 ℃/min, keeping the temperature for 0.1-0.5h when the temperature is raised to 1200-1250 ℃, and naturally cooling and annealing to obtain the ceramic composite grinding medium.
The invention has the following beneficial effects:
(1) The metal grinding medium is used as a metal core, the outer surface of the metal core is ground, the ground outer surface of the metal core is coated in a composite ceramic layer, the metal core is placed in a ball forming mill to be rolled to form a ball, the ball is polished and dried, a blank is formed by isostatic pressing, the blank is placed in a high-temperature kiln, the ceramic composite grinding medium is obtained, the hardness of the ceramic composite grinding medium is increased by using the metal core, and the compactness and the wear resistance of the ceramic composite grinding medium are improved by adding a sintering aid and a dispersing agent;
(2) Adding 2, 3-diaminotoluene into a three-neck flask, adding solvent N, N-dimethylacetamide, adding dried pyromellitic dianhydride to obtain an intermediate A, and adding SiO 2 And B 4 C, uniformly mixing, adding a silane coupling agent, adding a solvent ethanol to obtain an intermediate B,adding the intermediate B into the intermediate A, sintering to obtain the sintering aid, and adding the small-size nano Si0 2 are uniformly dispersed In the grinding medium, the dispersion strengthening effect is realized in the grinding medium, and when the grinding medium is impacted and rubbed during grinding work, si0 dispersed in the grinding medium 2 Can absorb the impact energy of the microcracks in the grinding medium and prevent the cracks from expanding, thereby enhancing the mechanical property of the system and hindering the slippage between polymer chain segments, thereby improving the bonding strength, and B is used in the process of sintering and heating 4 C is oxidized to generate chemical bonding force with high bonding energy, and B is generated in a molten state 2 0 3 The grinding medium can flow to the crack of the ceramic interface to inhibit crack diffusion, so that the ceramic interface is more densified, and the aim that the grinding medium is not easy to crack in the grinding process is fulfilled;
(3) Adding a catalyst into a high-pressure reaction kettle, adding 3-methyl-3-butylene-1-alcohol, adding 1, 2-butylene oxide, adding ethylene oxide to obtain an intermediate C, adding acetic anhydride into the intermediate C, adding an antioxidant to obtain an intermediate D, adding high hydrogen-containing silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane into a round-bottom flask, adding a catalyst, adding sodium bicarbonate to obtain an intermediate E, performing low-boiling-point substance removal pretreatment on the intermediate E, adding the intermediate D, the catalyst and the antioxidant into the round-bottom flask, and dropwise adding the intermediate E to obtain the dispersing agent, wherein the dispersing agent is formed by connecting a polyether chain segment and a polysiloxane chain segment through a Si-C chemical bond, and the polysiloxane main chain is used as a hydrophobic group to endow the product with excellent temperature resistance, ageing resistance, electric insulation, softness and the like, and the hydrophilic polyether chain segment enables the product to have good surface activity, and the hydrophilic lipophilic property can be effectively adjusted by introducing the main ethylene oxide and 1, 2-butylene oxide chain segment to obtain the performances of lubrication, emulsification, foam stabilization and defoaming, so that the components of the grinding medium are dispersed more uniformly and more compact.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the 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:
this example is a ceramic composite grinding media prepared by the steps of:
s1: taking a metal grinding medium as a metal inner core, and grinding the outer surface of the metal grinding medium;
s2: coating the outer surface of the polished metal core with a composite ceramic layer, stirring and dispersing for 1h at the rotating speed of 800r/min, then putting into a ball forming mill, rolling to form a ball, polishing, and drying for 1h at 40 ℃;
s3: pressing into a blank by isostatic pressing, placing the blank into a high-temperature kiln, firing at the heating rate of 5 ℃/min, keeping the temperature for 1h when the temperature is raised to 800 ℃, firing at the heating rate of 3 ℃/min, keeping the temperature for 0.1h when the temperature is raised to 1200 ℃, and naturally cooling and annealing to obtain the ceramic composite grinding medium;
the composite ceramic layer comprises the following components in parts by weight:
10 parts of kaolin, 10 parts of silicon carbide, 10 parts of feldspar, 3 parts of wollastonite, 5 parts of calcium oxide, 10 parts of zirconia, 2 parts of sodium dodecyl benzene sulfonate, 5 parts of a dispersing agent, 5 parts of a sintering aid, 3 parts of polyvinyl alcohol and 40 parts of water;
the sintering aid is prepared by the following steps:
s11: adding 2, 3-diaminotoluene into a three-neck flask, controlling the temperature at 10 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 5 hours to obtain an intermediate A;
s12: mixing SiO 2 And B 4 C, uniformly mixing, adding a silane coupling agent, adding a solvent ethanol, stirring for 1.5h, performing ultrasonic dispersion for 0.5h, and transferring to a drying oven at 85 ℃ for drying for 3h to obtain an intermediate B;
s13: and adding the intermediate B into the intermediate A, stirring for 1h, heating to 180 ℃ at the speed of 5 ℃/min, preserving heat for 1h, heating to 260 ℃ at the speed of 1 ℃/min, preserving heat for 1.5h, and naturally cooling to room temperature to obtain the sintering aid.
The dispersing agent is prepared by the following steps:
s41: adding a catalyst into a high-pressure reaction kettle, adding 3-methyl-3-butene-1-ol, pumping out air in the kettle at room temperature, adding 1, 2-epoxybutane, reacting for 3 hours at 110 ℃, adding ethylene oxide, reacting for 2 hours at 100 ℃, cooling and discharging after complete reaction to obtain an intermediate C;
s42: adding acetic anhydride into the intermediate C, heating to 140 ℃, reacting for 2h, and reacting with N after the reaction is finished 2 Vacuum stripping, removing residual anhydride, adding an antioxidant, reacting at 80 ℃ for 1h, and performing antioxidant treatment to obtain an intermediate D;
s43: adding high hydrogen-containing silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane into a round-bottom flask, adding a catalyst, stirring for reaction for 3 hours, standing, separating out the catalyst at the lower layer, adding sodium bicarbonate, and stirring for reaction for 0.5 hour at room temperature to obtain an intermediate E;
s44: and (3) carrying out low-boiling-point substance removal pretreatment on the intermediate E, adding the intermediate D, a catalyst and an antioxidant into a round-bottom flask with an electric stirrer and a thermometer, uniformly mixing, heating to 40 ℃, dropwise adding the intermediate E, controlling the dropwise adding speed to be 2 drops/s, carrying out reaction heat release after an induction period of 15min, and controlling the system temperature to be 65 ℃ for heat preservation and reaction for 2.5h to obtain the dispersing agent.
Example 2:
this example is a ceramic composite grinding media prepared by the steps of:
s1: taking a metal grinding medium as a metal inner core, and grinding the outer surface of the metal grinding medium;
s2: coating the outer surface of the polished metal core with a composite ceramic layer, stirring and dispersing for 1h at the rotating speed of 800r/min, then putting into a ball forming mill, rolling to form a ball, polishing, and drying for 1h at 40 ℃;
s3: pressing into a blank by adopting isostatic pressing, placing the blank into a high-temperature kiln, firing at the heating rate of 5 ℃/min, keeping the temperature for 1h when the temperature is raised to 1000 ℃, then firing at the heating rate of 3 ℃/min, keeping the temperature for 0.1h when the temperature is raised to 1200 ℃, and naturally cooling and annealing to obtain the ceramic composite grinding medium;
the composite ceramic layer comprises the following components in parts by weight:
10 parts of kaolin, 20 parts of silicon carbide, 20 parts of feldspar, 5 parts of wollastonite, 7 parts of calcium oxide, 10 parts of zirconia, 3 parts of sodium dodecyl benzene sulfonate, 8 parts of a dispersing agent, 10 parts of a sintering aid, 5 parts of polyvinyl alcohol and 40 parts of water;
the sintering aid is prepared by the following steps:
s11: adding 2, 3-diaminotoluene into a three-neck flask, controlling the temperature at 10 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 5 hours to obtain an intermediate A;
s12: mixing SiO 2 And B 4 C, uniformly mixing, adding a silane coupling agent, adding a solvent ethanol, stirring for 1.5h, performing ultrasonic dispersion for 0.5h, and transferring to a drying oven at 85 ℃ for drying for 3h to obtain an intermediate B;
s13: and adding the intermediate B into the intermediate A, stirring for 1h, heating to 190 ℃ at the speed of 5 ℃/min, preserving heat for 1h, heating to 260 ℃ at the speed of 1 ℃/min, preserving heat for 1.5h, and naturally cooling to room temperature to obtain the sintering aid.
The dispersing agent is prepared by the following steps:
s41: adding a catalyst into a high-pressure reaction kettle, adding 3-methyl-3-butene-1-ol, pumping out the air in the kettle at room temperature, adding 1, 2-epoxybutane, reacting for 5 hours at 120 ℃, adding ethylene oxide, reacting for 3 hours at 110 ℃, cooling and discharging after complete reaction to obtain an intermediate C;
s42: adding acetic anhydride into the intermediate C, heating to 145 ℃, reacting for 3h, and reacting with N after the reaction is finished 2 Vacuum stripping, removing residual anhydride, adding an antioxidant, reacting at 95 ℃ for 3h, and performing antioxidant treatment to obtain an intermediate D;
s43: adding high hydrogen-containing silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane into a round-bottom flask, adding a catalyst, stirring for reaction for 5 hours, standing, separating out the catalyst at the lower layer, adding sodium bicarbonate, and stirring for reaction for 1.5 hours at room temperature to obtain an intermediate E;
s44: and (3) carrying out low-boiling-point substance removal pretreatment on the intermediate E, adding the intermediate D, a catalyst and an antioxidant into a round-bottom flask with an electric stirrer and a thermometer, uniformly mixing, heating to 50 ℃, dropwise adding the intermediate E, controlling the dropwise adding speed to be 2 drops/s, carrying out reaction heat release after an induction period of 15min, and controlling the system temperature to be 70 ℃ for carrying out heat preservation reaction for 2.5h to obtain the dispersing agent.
Example 3:
this example is a ceramic composite grinding media prepared by the steps of:
s1: taking a metal grinding medium as a metal inner core, and grinding the outer surface of the metal grinding medium;
s2: coating the outer surface of the polished metal core with a composite ceramic layer, stirring and dispersing for 2h at the rotation speed of 1000r/min, then putting into a ball forming mill, rolling to form a ball, polishing, and drying for 2h at 50 ℃;
s3: pressing into a blank by adopting isostatic pressing, placing the blank into a high-temperature kiln, firing at the heating rate of 10 ℃/min, keeping the temperature for 2h when the temperature is raised to 1000 ℃, firing at the heating rate of 5 ℃/min, keeping the temperature for 0.5h when the temperature is raised to 1250 ℃, and naturally cooling and annealing to obtain the ceramic composite grinding medium;
the composite ceramic layer comprises the following components in parts by weight:
20 parts of kaolin, 20 parts of silicon carbide, 20 parts of feldspar, 5 parts of wollastonite, 7 parts of calcium oxide, 15 parts of zirconium oxide, 3 parts of sodium dodecyl benzene sulfonate, 8 parts of a dispersing agent, 10 parts of a sintering aid, 5 parts of polyvinyl alcohol and 60 parts of water;
the sintering aid is prepared by the following steps:
s11: adding 2, 3-diaminotoluene into a three-neck flask, controlling the temperature at 11 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 6 hours to obtain an intermediate A;
s12: mixing SiO 2 And B 4 C, mixing evenly, adding a silane coupling agent, adding a solvent ethanol,stirring for 2.5h, performing ultrasonic dispersion for 2h, and transferring to a drying oven at 95 ℃ for drying for 4h to obtain an intermediate B;
s13: and adding the intermediate B into the intermediate A, stirring for 2h, heating to 190 ℃ at the speed of 5 ℃/min, preserving heat for 1.5h, heating to 270 ℃ at the speed of 3 ℃/min, preserving heat for 2.5h, and naturally cooling to room temperature to obtain the sintering aid.
The dispersing agent is prepared by the following steps:
s41: adding a catalyst into a high-pressure reaction kettle, adding 3-methyl-3-butene-1-ol, pumping out the air in the kettle at room temperature, adding 1, 2-epoxybutane, reacting for 5 hours at 120 ℃, adding ethylene oxide, reacting for 3 hours at 110 ℃, cooling and discharging after complete reaction to obtain an intermediate C;
s42: adding acetic anhydride into the intermediate C, heating to 145 ℃, reacting for 3h, and reacting with N after the reaction is finished 2 Vacuum stripping, removing residual anhydride, adding an antioxidant, reacting at 95 ℃ for 3h, and performing antioxidant treatment to obtain an intermediate D;
s43: adding high hydrogen-containing silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane into a round-bottom flask, adding a catalyst, stirring for reaction for 5 hours, standing, separating out the catalyst at the lower layer, adding sodium bicarbonate, and stirring for reaction for 1.5 hours at room temperature to obtain an intermediate E;
s44: and (3) carrying out low-boiling-point substance removal pretreatment on the intermediate E, adding the intermediate D, a catalyst and an antioxidant into a round-bottom flask with an electric stirrer and a thermometer, uniformly mixing, heating to 50 ℃, dropwise adding the intermediate E, controlling the dropwise adding speed to be 2 drops/s, after an induction period of 15min, carrying out reaction heat release, and controlling the system temperature to be 70 ℃ and carrying out heat preservation reaction for 2.5h to obtain the dispersing agent.
Comparative example 1:
comparative example 1 differs from example 1 in that no sintering aid is added.
Comparative example 2:
comparative example 2 differs from example 1 in that no dispersant is added.
Detecting the ceramic composite grinding media of the embodiments 1-3 and the comparative examples 1-2, weighing 500g of the grinding media, placing the grinding media into a 1000mL corundum grinding tank, adding 500g of water, rotating at 550r/min for 8h, taking out, drying, weighing, and calculating the wear rate;
the results are shown in the following table:
as can be seen from the above table, the density of the examples reached 3.8 to 3.9g/cm 3 While comparative example 1, in which no sintering aid was added, had a density of 3.1g/cm 3 While comparative example 2, in which no dispersant was added, had a density of 3.3g/cm 3 The Young's modulus of the examples reaches 89.9-90.0GPa, the Young's modulus of the comparative example 1 without adding the sintering aid is 78.5GPa, the Young's modulus of the comparative example 2 without adding the dispersing agent is 80.0GPa, the microhardness of the examples reaches 720-730, the microhardness of the comparative example 1 without adding the sintering aid is 655, the microhardness of the comparative example 2 without adding the dispersing agent is 675, the wear rate of the examples reaches 0.02-0.05%, the wear rate of the comparative example 1 without adding the sintering aid is 0.54%, the wear rate of the comparative example 2 without adding the dispersing agent is 0.48%, and the data of the examples are superior to those of the comparative examples, which shows that the dispersing agent and the sintering aid added to prepare the ceramic composite grinding medium can effectively improve the wear resistance and the hardness of the ceramic composite grinding medium.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (9)
1. A ceramic composite grinding medium, characterized in that it is prepared by the following steps:
s1: taking a metal grinding medium as a metal inner core, and grinding the outer surface of the metal grinding medium;
s2: coating the composite ceramic layer on the outer surface of the polished metal core, putting the metal core into a ball forming mill, rolling to form a ball, polishing and drying;
s3: pressing into a blank by isostatic pressing, and placing the blank into a high-temperature kiln to obtain the ceramic composite grinding medium;
the composite ceramic layer in the step S2 comprises the following components in parts by weight:
10-20 parts of kaolin, 10-20 parts of silicon carbide, 10-20 parts of feldspar, 3-5 parts of wollastonite, 5-7 parts of calcium oxide, 10-15 parts of zirconium oxide, 2-3 parts of sodium dodecyl benzene sulfonate, 5-8 parts of a dispersing agent, 5-10 parts of a sintering aid, 3-5 parts of polyvinyl alcohol and 40-60 parts of water;
the sintering aid is prepared by the following steps:
s11: adding 2, 3-diaminotoluene into a three-neck flask, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, and adding dried pyromellitic dianhydride to obtain an intermediate A;
s12: mixing SiO 2 And B 4 C, uniformly mixing, adding a silane coupling agent, and adding a solvent ethanol to obtain an intermediate B;
s13: and adding the intermediate B into the intermediate A, and sintering to obtain the sintering aid.
2. The ceramic composite grinding media of claim 1, wherein the molar ratio of 2, 3-diaminotoluene to pyromellitic dianhydride in step S11 is 1.2-1.3:1.
3. the ceramic composite grinding media of claim 1, wherein S is step S12iO 2 、B 4 The dosage ratio of C to the silane coupling agent is 10g:10g:1g, wherein the dosage ratio of the intermediate A to the intermediate B in the step S13 is 1g:1g of the total weight of the composition.
4. The ceramic composite grinding medium of claim 1, wherein the dispersant is prepared by the steps of:
s41: adding a catalyst into a high-pressure reaction kettle, adding 3-methyl-3-butylene-1-alcohol, adding 1, 2-epoxybutane, and adding ethylene oxide to obtain an intermediate C;
s42: adding acetic anhydride into the intermediate C, and adding an antioxidant to obtain an intermediate D;
s43: adding high hydrogen-containing silicone oil, octamethylcyclotetrasiloxane and hexamethyldisiloxane into a round-bottom flask, adding a catalyst, and adding sodium bicarbonate to obtain an intermediate E;
s44: and (3) carrying out low-boiling-point substance removal pretreatment on the intermediate E, adding the intermediate D, a catalyst and an antioxidant into a round-bottom flask, and dropwise adding the intermediate E to obtain the dispersing agent.
5. The ceramic composite grinding medium according to claim 4, wherein the catalyst in step S41 is potassium hydroxide, the catalyst is 0.3 to 0.4% of the total mass of 3-methyl-3-buten-1-ol, 1, 2-epoxybutane and ethylene oxide, and the molar ratio of the 4-penten-1-ol, 1, 2-epoxybutane and ethylene oxide is 1:1.5:1.
6. the ceramic composite grinding medium according to claim 4, wherein the antioxidant in step S42 is an aromatic amine antioxidant, the amount of the antioxidant is 0.3% of the total mass of the acetic anhydride and the intermediate E, and the molar ratio of the acetic anhydride to the intermediate C is 1:1.
7. the ceramic composite grinding medium according to claim 4, wherein the catalyst in step S43 is concentrated sulfuric acid with a mass fraction of 98%, the amount of the catalyst is 2% of the total mass of the high hydrogen-containing silicone oil, the octamethylcyclotetrasiloxane and the hexamethyldisiloxane, the amount of the sodium bicarbonate is 1% of the total mass of the high hydrogen-containing silicone oil, the octamethylcyclotetrasiloxane and the hexamethyldisiloxane, and the ratio of the amounts of the high hydrogen-containing silicone oil, the octamethylcyclotetrasiloxane and the hexamethyldisiloxane is 19.1g:78.4g:1.5g.
8. The ceramic composite grinding medium according to claim 4, wherein the catalyst in step S44 is chloroplatinic acid, the antioxidant is an aromatic amine antioxidant, the amount of the catalyst is 11% of the total mass of the intermediate D and the intermediate E, the amount of the antioxidant is 1% of the total mass of the intermediate D and the intermediate E, and the ratio of the amount of the intermediate D to the amount of the intermediate E is 25g:11g.
9. The method of any one of claims 1 to 8, comprising the steps of:
s1: taking a metal grinding medium as a metal inner core, and grinding the outer surface of the metal grinding medium;
s2: coating the outer surface of the polished metal core with a composite ceramic layer, stirring and dispersing for 1-2h at the rotation speed of 800-1000r/min, putting into a ball forming mill, rolling to form a ball, polishing, and drying for 1-2h at 40-50 ℃;
s3: pressing into a blank by isostatic pressing, placing the blank into a high-temperature kiln, firing at the heating rate of 5-10 ℃/min, keeping the temperature for 1-2h when the temperature is raised to 800-1000 ℃, firing at the heating rate of 3-5 ℃/min, keeping the temperature for 0.1-0.5h when the temperature is raised to 1200-1250 ℃, and naturally cooling and annealing to obtain the ceramic composite grinding medium.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107312499A (en) * | 2017-07-18 | 2017-11-03 | 洛阳理工学院 | A kind of ball mill metal and Ceramic Composite abrasive media and preparation method thereof |
| CN112624729A (en) * | 2020-12-19 | 2021-04-09 | 安徽致磨新材料科技有限公司 | Metal and ceramic composite grinding medium and preparation method thereof |
| CN113477926A (en) * | 2021-07-20 | 2021-10-08 | 扬州金鑫管业有限公司 | Production process of high-performance ceramic lining composite steel pipe |
| CN113831840A (en) * | 2021-10-27 | 2021-12-24 | 江苏拜富科技股份有限公司 | Preparation process of high-performance antireflection film |
| CN114836172A (en) * | 2022-06-06 | 2022-08-02 | 安徽致磨新材料科技有限公司 | Composite grinding medium for grinder and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107312499A (en) * | 2017-07-18 | 2017-11-03 | 洛阳理工学院 | A kind of ball mill metal and Ceramic Composite abrasive media and preparation method thereof |
| CN112624729A (en) * | 2020-12-19 | 2021-04-09 | 安徽致磨新材料科技有限公司 | Metal and ceramic composite grinding medium and preparation method thereof |
| CN113477926A (en) * | 2021-07-20 | 2021-10-08 | 扬州金鑫管业有限公司 | Production process of high-performance ceramic lining composite steel pipe |
| CN113831840A (en) * | 2021-10-27 | 2021-12-24 | 江苏拜富科技股份有限公司 | Preparation process of high-performance antireflection film |
| CN114836172A (en) * | 2022-06-06 | 2022-08-02 | 安徽致磨新材料科技有限公司 | Composite grinding medium for grinder and preparation method thereof |
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