CN112624729A - Metal and ceramic composite grinding medium and preparation method thereof - Google Patents

Metal and ceramic composite grinding medium and preparation method thereof Download PDF

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Publication number
CN112624729A
CN112624729A CN202011509818.8A CN202011509818A CN112624729A CN 112624729 A CN112624729 A CN 112624729A CN 202011509818 A CN202011509818 A CN 202011509818A CN 112624729 A CN112624729 A CN 112624729A
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ceramic
metal
putting
stirring
parts
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孟超
任永国
朱振宇
魏小威
范孝友
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Anhui Zhimo New Material Technology Co ltd
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Anhui Zhimo New Material Technology Co ltd
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Abstract

The invention discloses a metal and ceramic composite grinding medium and a preparation method thereof, wherein modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconium oxide and muscovite are added into a ball mill, and after ball milling, discharging is carried out to obtain ultramicro powder; the raw materials of the metal and ceramic composite grinding medium are connected closely, so that the metal and ceramic composite grinding medium has excellent hardness, and meanwhile, the metal is combined on the ceramic through the close compounding of the ceramic and the metal, so that the metal and ceramic composite grinding medium has excellent wear resistance.

Description

Metal and ceramic composite grinding medium and preparation method thereof
Technical Field
The invention relates to the field of grinding media, in particular to a metal and ceramic composite grinding media and a preparation method thereof.
Background
The ceramic grinding medium has 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, occupies a very important place in the field of grinding media, and is widely applied to the related fine processing fields of mineral products, chemical industry, paint, mechanical electronics and the like.
The existing ceramic microspheres mainly comprise aluminum oxide, zirconium oxide, silicon carbide, silicon nitride and the like, are expensive, high in manufacturing cost, free of market advantages, low in wear resistance and low in hardness, and are easy to crack in a grinding process.
Therefore, it is the key of the present invention to provide a low cost, high wear resistance, high hardness grinding media.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a metal and ceramic composite grinding medium and a preparation method thereof, wherein the metal and ceramic composite grinding medium comprises the following components: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconium oxide and muscovite into a ball mill, performing ball milling, discharging to obtain superfine powder, adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foamed microspheres into water, stirring and dispersing to obtain mixed slurry, adding the superfine powder into the mixed slurry while stirring, adding the mixed slurry, continuously stirring to obtain a mixed material after adding, putting the mixed material into a ball forming mill, adding water into the mixed material to mix uniformly, rolling to form a ball, polishing, then drying in a drying device to obtain a ceramic microsphere blank, putting the ceramic microsphere blank into a kiln, firing to obtain ceramic hollow microspheres, putting the hollow ceramic microspheres into a ceramic grinding machine to grind to obtain ceramic hollow microspheres with rough surfaces, putting the hollow microspheres with rough surfaces into a metal liquid to soak, taking out and naturally cooling to room temperature, the metal and ceramic composite grinding medium is put into a drying oven for drying to obtain a dried substance, and then is put into a polishing machine for polishing to obtain the metal and ceramic composite grinding medium, so that the problems that the existing ceramic micro-beads are expensive, high in manufacturing cost, low in wear resistance and hardness and easy to crack in the grinding process are solved.
The purpose of the invention can be realized by the following technical scheme:
a metal and ceramic composite grinding medium comprises the following components in parts by weight:
40-60 parts of modified kaolin, 8-12 parts of silicon carbide, 10-20 parts of feldspar, 6-8 parts of wollastonite, 5-7 parts of calcium oxide, 5-7 parts of zirconium oxide, 3-5 parts of muscovite mica, 2-4 parts of sodium dodecyl benzene sulfonate, 2-4 parts of binder, 1-2 parts of polyvinyl alcohol, 20-30 parts of foamed microspheres and 40-60 parts of water;
the metal and ceramic composite grinding medium is prepared by the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconia and muscovite into a ball mill, ball-milling to 2000-3000 meshes, and discharging to obtain ultrafine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foamed microspheres into water, and stirring and dispersing for 1-2 hours at the rotation speed of 500-;
step three: adding the superfine powder into the mixed slurry under stirring at the temperature of 90-100 ℃ and the rotating speed of 300-;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form a ball, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1400 ℃ at a heating rate of 1-3 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into the metal liquid to be soaked for 1-3s, taking out the hollow microspheres to be naturally cooled to room temperature, putting the hollow microspheres into an oven to be dried to obtain a dried substance, putting the dried substance into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
As a further scheme of the invention: the molten metal is a melt obtained by mixing and melting one or more of iron, copper, aluminum, manganese, zinc and chromium according to any proportion.
As a further scheme of the invention: the preparation method of the modified kaolin comprises the following steps:
s31: adding gamma-aminopropyltriethoxysilane into isopropanol, adjusting pH of the reaction system to 3-5 with citric acid-sodium dihydrogen phosphate buffer solution with pH of 2.2, heating in water bath at 35 deg.C and rotation speed of 50-100r/min, and stirring for 40-60min to obtain a transparent mixed solution A;
s32: adding calcined kaolin into the mixed solution A, stirring for 1-2h under the condition that the rotation speed is 300-500r/min, then adding absolute ethyl alcohol, continuously stirring for 1-2h in a water bath constant temperature bath at the temperature of 70-75 ℃, then heating to 85 ℃ until the solvent is completely evaporated, then carrying out suction filtration, placing the filter cake into a vacuum drying box, carrying out vacuum drying for 20-30h under the temperature of 70-75 ℃, and then grinding to obtain the modified kaolin.
As a further scheme of the invention: the dosage ratio of the gamma-aminopropyltriethoxysilane to the isopropanol in the step S31 is 1 g: 50 mL; in the step S32, the dosage ratio of the calcined kaolin to the mixed solution A to the absolute ethyl alcohol is 100 g: 100mL of: 10-20 mL.
As a further scheme of the invention: the preparation method of the adhesive comprises the following steps:
s51: ultrasonically dispersing water glass for 0.5-1h under the condition that the frequency is 80-120kHz to obtain a water glass dispersion;
s52: adding the water glass dispersion and sodium pyrophosphate into a three-neck flask provided with a thermometer, a reflux condenser and a stirrer, then moving the three-neck flask into a water bath thermostatic bath, stirring for 1-2h under the conditions that the temperature is 70-90 ℃, the rotating speed is 500 plus materials at 800r/min, and then removing the water bath thermostatic bath, continuing to perform condensation reflux and stirring until the temperature of a reaction system is reduced to the room temperature, thus obtaining the adhesive.
As a further scheme of the invention: the adding amount of the sodium pyrophosphate is 4.5-5.5% of the mass of the water glass.
As a further scheme of the invention: the preparation method of the foaming microsphere comprises the following steps:
s71: adding water, sodium thiosulfate and ammonium persulfate into a beaker, and carrying out ultrasonic treatment for 30-50min to obtain a mixed solution B;
s72: adding liquid paraffin oil, span 80, calcium stearate, acrylonitrile, methyl methacrylate, methacrylic acid and 1, 4-butanediol dimethacrylate into a flask, and stirring for 10-20min under the condition that the rotating speed is 1000r/min to obtain an oily substance;
s73: adding the mixed solution B into the oily substance while stirring, and continuously stirring and dispersing for 30-50min to obtain a mixed solution C;
s74: adding the mixed solution C into a flask, placing the flask into a water bath, firstly heating to 55 ℃ for reaction for 1h, then heating to 60 ℃ for reaction for 8h, then heating to 65 ℃ for reaction for 1h, cooling to room temperature after the reaction is finished, then carrying out vacuum filtration, respectively washing a filter cake for 2-3 times by using ethanol and distilled water, then placing the filter cake into a vacuum drying oven, and carrying out vacuum drying for 25-30h at the temperature of 50 ℃ to obtain the foamed microspheres.
As a further scheme of the invention: in the step S71, the mass ratio of the water to the sodium thiosulfate to the ammonium persulfate is 50:2: 5; in the step S72, the mass ratio of the liquid paraffin oil, the span 80, the calcium stearate, the acrylonitrile, the methyl methacrylate, the methacrylic acid and the 1, 4-butanediol dimethacrylate is 200:1.5:0.2:6:12:12: 1.
As a further scheme of the invention: a preparation method of a metal and ceramic composite grinding medium comprises the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconia and muscovite into a ball mill, ball-milling to 2000-3000 meshes, and discharging to obtain ultrafine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foamed microspheres into water, and stirring and dispersing for 1-2 hours at the rotation speed of 500-;
step three: adding the superfine powder into the mixed slurry under stirring at the temperature of 90-100 ℃ and the rotating speed of 300-;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form a ball, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1400 ℃ at a heating rate of 1-3 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into the metal liquid to be soaked for 1-3s, taking out the hollow microspheres to be naturally cooled to room temperature, putting the hollow microspheres into an oven to be dried to obtain a dried substance, putting the dried substance into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
The invention has the beneficial effects that:
the invention relates to a metal and ceramic composite grinding medium and a preparation method thereof, which comprises the steps of adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconium oxide and muscovite into a ball mill, carrying out ball milling, discharging to obtain ultramicro powder, adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foaming microspheres into water, stirring and dispersing to obtain mixed slurry, adding the ultramicro powder into the mixed slurry while stirring, continuously stirring after adding to obtain a mixed material, putting the mixed material into a ball forming machine, adding water to mix uniformly, rolling to form balls, polishing, then sending into a drying device for drying, drying to obtain ceramic microsphere blanks, putting the ceramic microsphere blanks into a kiln, firing to obtain ceramic hollow microspheres, putting the hollow ceramic microspheres into a ceramic polisher for polishing to obtain ceramic hollow microspheres with rough surfaces, soaking the hollow microspheres with rough surfaces in a metal liquid, taking out the hollow microspheres, naturally cooling the hollow microspheres to room temperature, then putting the hollow microspheres into an oven for drying to obtain a dried substance, then putting the dried substance into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium; the raw materials of the metal and ceramic composite grinding medium are connected closely, so that the metal and ceramic composite grinding medium has excellent hardness, and meanwhile, the metal is combined on the ceramic through the close compounding of the ceramic and the metal, so that the metal and ceramic composite grinding medium has excellent wear resistance, and has good grinding effect and long service life when used as a grinding medium;
the process for preparing the metal and ceramic composite grinding medium prepares modified kaolin, selects gamma-aminopropyl triethoxysilane as a modifier, isopropanol is taken as a modification auxiliary agent, gamma-aminopropyltriethoxysilane is hydrolyzed under the catalysis of the isopropanol and self-condensed into silanol (-Si-OH), the silanol and hydroxyl on the surface of calcined kaolin form hydrogen bonds, a covalent bond (-C-O-Si-structure) is formed after dehydration reaction, so that the gamma-aminopropyltriethoxysilane is connected on the kaolin in a chemical bond mode, meanwhile, condensation reaction is carried out between silanol groups to form film-coated kaolin particles with a net structure, so that the kaolin cannot agglomerate, thereby improving the dispersibility of the kaolin, and ensuring that the kaolin is uniformly dispersed and tightly connected with other raw materials;
the adhesive is prepared in the process of preparing the metal and ceramic composite grinding medium, the water glass is a green pollution-free adhesive, but the water glass is alkaline, silicon hydroxide molecules exist among the water glass, hydrogen bonds are formed among the silicon hydroxide molecules through-OH, colloidal particles can appear, so that the adhesive property of the water glass is reduced, sodium pyrophosphate can stably exist in an alkaline solution and cannot be decomposed by adding sodium pyrophosphate, and a P-O bond can be inserted into a Si-O bond to form a P-0-Si bond, so that a reticular structure is formed, the metal and ceramic composite grinding medium can be tightly connected with each component, and the mechanical property of the metal and ceramic composite grinding medium is improved;
the preparation method of the metal and ceramic composite grinding medium also comprises the step of preparing a foaming microsphere, wherein acrylonitrile, methyl methacrylate and methacrylic acid are melted and coated on water molecules to form a microsphere structure with a water-outer resin polymer as an inner layer, the curing speed of the resin polymer is higher than the steam pressure generated by water gasification in the heating process of the structure, and the wall breaking phenomenon is generated along with the increase of the steam pressure in a pore, so that the pore opening structure is formed, the mixture can be foamed due to the existence of the steam in the mixture, a subsequently prepared ceramic microsphere blank can form a hollow structure in the firing process, metal liquid can enter the ceramic microsphere, the metal and the ceramic are tightly compounded together, and the metal and ceramic composite grinding medium is endowed with excellent wear resistance.
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:
the embodiment is a metal and ceramic composite grinding medium, which comprises the following components in parts by weight:
40 parts of modified kaolin, 8 parts of silicon carbide, 10 parts of feldspar, 6 parts of wollastonite, 5 parts of calcium oxide, 5 parts of zirconium oxide, 3 parts of muscovite, 2 parts of sodium dodecyl benzene sulfonate, 2 parts of a binder, 1 part of polyvinyl alcohol, 20 parts of foamed microspheres and 40 parts of water;
the metal and ceramic composite grinding medium is prepared by the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconium oxide and muscovite into a ball mill, ball-milling to 2000 meshes, and discharging to obtain superfine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foaming microspheres into water, and stirring and dispersing for 1h at the rotating speed of 500r/min to obtain mixed slurry;
step three: adding the superfine powder into the mixed slurry under stirring at the temperature of 90 ℃ and the rotating speed of 300r/min, controlling the adding time of the mixed slurry to be 20min, and continuing stirring for 1h after the adding is finished to obtain a mixed material;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form a ball, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1400 ℃ at a heating rate of 1 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into a metal liquid for soaking for 1s, taking out, naturally cooling to room temperature, putting into an oven for drying to obtain a dried substance, putting into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
The molten metal is a melt obtained by mixing and melting iron, copper, aluminum, manganese, zinc and chromium according to any proportion.
The preparation method of the modified kaolin comprises the following steps:
s31: adding gamma-aminopropyltriethoxysilane into isopropanol, adjusting the pH of a reaction system to 3 by using a citric acid-sodium dihydrogen phosphate buffer solution with the pH of 2.2, heating in a water bath at the temperature of 35 ℃ and the rotating speed of 50r/min, and stirring for 40min to obtain a mixed solution A when the reaction system is uniform and transparent;
s32: adding calcined kaolin into the mixed solution A, stirring for 1h at the rotation speed of 300r/min, adding absolute ethyl alcohol, continuing stirring for 1h in a water bath thermostatic bath at the temperature of 70 ℃, heating to 85 ℃ until the solvent is completely evaporated, then carrying out suction filtration, placing the filter cake in a vacuum drying oven, carrying out vacuum drying for 20h at the temperature of 70 ℃, and then grinding to obtain the modified kaolin.
The dosage ratio of the gamma-aminopropyltriethoxysilane to the isopropanol in the step S31 is 1 g: 50 mL; in the step S32, the dosage ratio of the calcined kaolin to the mixed solution A to the absolute ethyl alcohol is 100 g: 100mL of: 10 mL.
The preparation method of the adhesive comprises the following steps:
s51: ultrasonically dispersing water glass for 0.5h under the condition that the frequency is 80kHz to obtain a water glass dispersion;
s52: adding the water glass dispersion and sodium pyrophosphate into a three-neck flask provided with a thermometer, a reflux condenser and a stirrer, then moving the three-neck flask into a water bath constant temperature tank, stirring for 1h under the conditions of 70 ℃ of temperature, 500r/min of rotating speed and condensation reflux, then removing the water bath constant temperature tank, continuing condensation reflux and stirring until the temperature of a reaction system is reduced to room temperature, and obtaining the adhesive.
The adding amount of the sodium pyrophosphate is 4.5 percent of the mass of the water glass.
The preparation method of the foaming microsphere comprises the following steps:
s71: adding water, sodium thiosulfate and ammonium persulfate into a beaker, and carrying out ultrasonic treatment for 30min to obtain a mixed solution B;
s72: adding liquid paraffin oil, span 80, calcium stearate, acrylonitrile, methyl methacrylate, methacrylic acid and 1, 4-butanediol dimethacrylate into a flask, and stirring for 10min under the condition that the rotating speed is 1000r/min to obtain an oily substance;
s73: adding the mixed solution B into the oily substance while stirring, and continuously stirring and dispersing for 30min to obtain a mixed solution C;
s74: adding the mixed solution C into a flask, placing the flask into a water bath, firstly heating to 55 ℃ for reaction for 1h, then heating to 60 ℃ for reaction for 8h, then heating to 65 ℃ for reaction for 1h, cooling to room temperature after the reaction is finished, then carrying out vacuum filtration, respectively washing a filter cake for 2 times by using ethanol and distilled water, then placing the filter cake into a vacuum drying oven, and carrying out vacuum drying for 25h at the temperature of 50 ℃ to obtain the foaming microspheres.
In the step S71, the mass ratio of the water to the sodium thiosulfate to the ammonium persulfate is 50:2: 5; in the step S72, the mass ratio of the liquid paraffin oil, the span 80, the calcium stearate, the acrylonitrile, the methyl methacrylate, the methacrylic acid and the 1, 4-butanediol dimethacrylate is 200:1.5:0.2:6:12:12: 1.
A preparation method of a metal and ceramic composite grinding medium comprises the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconium oxide and muscovite into a ball mill, ball-milling to 2000 meshes, and discharging to obtain superfine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foaming microspheres into water, and stirring and dispersing for 1h at the rotating speed of 500r/min to obtain mixed slurry;
step three: adding the superfine powder into the mixed slurry under stirring at the temperature of 90 ℃ and the rotating speed of 300r/min, controlling the adding time of the mixed slurry to be 20min, and continuing stirring for 1h after the adding is finished to obtain a mixed material;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form a ball, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1400 ℃ at a heating rate of 1 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into a metal liquid for soaking for 1s, taking out, naturally cooling to room temperature, putting into an oven for drying to obtain a dried substance, putting into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
Example 2:
the embodiment is a metal and ceramic composite grinding medium, which comprises the following components in parts by weight:
50 parts of modified kaolin, 10 parts of silicon carbide, 15 parts of feldspar, 7 parts of wollastonite, 6 parts of calcium oxide, 6 parts of zirconium oxide, 4 parts of muscovite, 3 parts of sodium dodecyl benzene sulfonate, 3 parts of a binder, 2 parts of polyvinyl alcohol, 25 parts of foamed microspheres and 50 parts of water;
the metal and ceramic composite grinding medium is prepared by the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconium oxide and muscovite into a ball mill, ball-milling to 2500 meshes, and discharging to obtain superfine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foaming microspheres into water, and stirring and dispersing for 2 hours at the rotating speed of 650r/min to obtain mixed slurry;
step three: adding the superfine powder into the mixed slurry under stirring at the temperature of 95 ℃ and the rotating speed of 400r/min, controlling the adding time of the mixed slurry to be 30min, and continuing stirring for 1h after the adding is finished to obtain a mixture;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form balls, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1450 ℃ at a heating rate of 2 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into a metal liquid for soaking for 2s, taking out, naturally cooling to room temperature, putting into an oven for drying to obtain a dried substance, putting into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
The molten metal is a melt obtained by mixing and melting iron, copper, aluminum, manganese, zinc and chromium according to any proportion.
The preparation method of the modified kaolin comprises the following steps:
s31: adding gamma-aminopropyltriethoxysilane into isopropanol, adjusting the pH of a reaction system to 4 by using a citric acid-sodium dihydrogen phosphate buffer solution with the pH of 2.2, heating in a water bath at the temperature of 35 ℃ and the rotating speed of 75r/min, and stirring for 50min to obtain a mixed solution A when the reaction system is uniform and transparent;
s32: adding calcined kaolin into the mixed solution A, stirring for 2 hours at the rotation speed of 400r/min, then adding absolute ethyl alcohol, continuing stirring for 1 hour in a water bath thermostatic bath at the temperature of 72 ℃, then heating to 85 ℃ until the solvent is completely evaporated, then carrying out suction filtration, placing the filter cake in a vacuum drying oven, carrying out vacuum drying for 25 hours at the temperature of 72 ℃, and then grinding to obtain the modified kaolin.
The dosage ratio of the gamma-aminopropyltriethoxysilane to the isopropanol in the step S31 is 1 g: 50 mL; in the step S32, the dosage ratio of the calcined kaolin to the mixed solution A to the absolute ethyl alcohol is 100 g: 100mL of: 15 mL.
The preparation method of the adhesive comprises the following steps:
s51: ultrasonically dispersing water glass for 0.8h under the condition that the frequency is 100kHz to obtain a water glass dispersion;
s52: adding the water glass dispersion and sodium pyrophosphate into a three-neck flask provided with a thermometer, a reflux condenser and a stirrer, then moving the three-neck flask into a water bath constant temperature tank, stirring for 2 hours under the conditions that the temperature is 80 ℃, the rotating speed is 650r/min, and carrying out condensation reflux, then removing the water bath constant temperature tank, continuing condensation reflux and stirring until the temperature of a reaction system is reduced to room temperature, and obtaining the adhesive.
The adding amount of the sodium pyrophosphate is 5.0 percent of the mass of the water glass.
The preparation method of the foaming microsphere comprises the following steps:
s71: adding water, sodium thiosulfate and ammonium persulfate into a beaker, and carrying out ultrasonic treatment for 30-50min to obtain a mixed solution B;
s72: adding liquid paraffin oil, span 80, calcium stearate, acrylonitrile, methyl methacrylate, methacrylic acid and 1, 4-butanediol dimethacrylate into a flask, and stirring for 15min under the condition that the rotating speed is 1000r/min to obtain an oily substance;
s73: adding the mixed solution B into the oily substance while stirring, and continuously stirring and dispersing for 40min to obtain a mixed solution C;
s74: adding the mixed solution C into a flask, placing the flask into a water bath, firstly heating to 55 ℃ for reaction for 1h, then heating to 60 ℃ for reaction for 8h, then heating to 65 ℃ for reaction for 1h, cooling to room temperature after the reaction is finished, then carrying out vacuum filtration, respectively washing a filter cake for 3 times by using ethanol and distilled water, then placing the filter cake into a vacuum drying oven, and carrying out vacuum drying for 28h at the temperature of 50 ℃ to obtain the foaming microsphere.
In the step S71, the mass ratio of the water to the sodium thiosulfate to the ammonium persulfate is 50:2: 5; in the step S72, the mass ratio of the liquid paraffin oil, the span 80, the calcium stearate, the acrylonitrile, the methyl methacrylate, the methacrylic acid and the 1, 4-butanediol dimethacrylate is 200:1.5:0.2:6:12:12: 1.
A preparation method of a metal and ceramic composite grinding medium comprises the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconium oxide and muscovite into a ball mill, ball-milling to 2500 meshes, and discharging to obtain superfine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foaming microspheres into water, and stirring and dispersing for 2 hours at the rotating speed of 650r/min to obtain mixed slurry;
step three: adding the superfine powder into the mixed slurry under stirring at the temperature of 95 ℃ and the rotating speed of 400r/min, controlling the adding time of the mixed slurry to be 30min, and continuing stirring for 1h after the adding is finished to obtain a mixture;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form balls, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1450 ℃ at a heating rate of 2 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into a metal liquid for soaking for 2s, taking out, naturally cooling to room temperature, putting into an oven for drying to obtain a dried substance, putting into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
Example 3:
the embodiment is a metal and ceramic composite grinding medium, which comprises the following components in parts by weight:
60 parts of modified kaolin, 12 parts of silicon carbide, 20 parts of feldspar, 8 parts of wollastonite, 7 parts of calcium oxide, 7 parts of zirconium oxide, 5 parts of muscovite, 4 parts of sodium dodecyl benzene sulfonate, 4 parts of binder, 2 parts of polyvinyl alcohol, 30 parts of foamed microspheres and 60 parts of water;
the metal and ceramic composite grinding medium is prepared by the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconia and muscovite into a ball mill, ball-milling to 3000 meshes, and discharging to obtain superfine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foaming microspheres into water, and stirring and dispersing for 2 hours at the rotating speed of 800r/min to obtain mixed slurry;
step three: adding the superfine powder into the mixed slurry under the conditions of 100 ℃ and 500r/min of rotating speed, controlling the adding time of the mixed slurry to be 40min, and continuing stirring for 2h after the adding is finished to obtain a mixture;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form a ball, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1500 ℃ at a heating rate of 3 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into a metal liquid for soaking for 3s, taking out, naturally cooling to room temperature, putting into an oven for drying to obtain a dried substance, putting into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
The molten metal is a melt obtained by mixing and melting iron, copper, aluminum, manganese, zinc and chromium according to any proportion.
The preparation method of the modified kaolin comprises the following steps:
s31: adding gamma-aminopropyltriethoxysilane into isopropanol, adjusting the pH of a reaction system to 5 by using a citric acid-sodium dihydrogen phosphate buffer solution with the pH of 2.2, heating in a water bath at the temperature of 35 ℃ and the rotating speed of 100r/min, and stirring for 60min to obtain a mixed solution A when the reaction system is uniform and transparent;
s32: adding calcined kaolin into the mixed solution A, stirring for 2h at the rotation speed of 500r/min, adding absolute ethyl alcohol, continuing stirring for 2h in a water bath thermostatic bath at the temperature of 75 ℃, heating to 85 ℃ until the solvent is completely evaporated, then carrying out suction filtration, placing the filter cake in a vacuum drying oven, carrying out vacuum drying for 30h at the temperature of 75 ℃, and then grinding to obtain the modified kaolin.
The dosage ratio of the gamma-aminopropyltriethoxysilane to the isopropanol in the step S31 is 1 g: 50 mL; in the step S32, the dosage ratio of the calcined kaolin to the mixed solution A to the absolute ethyl alcohol is 100 g: 100mL of: 20 mL.
The preparation method of the adhesive comprises the following steps:
s51: ultrasonically dispersing water glass for 1h under the condition that the frequency is 120kHz to obtain a water glass dispersion;
s52: adding the water glass dispersion and sodium pyrophosphate into a three-neck flask provided with a thermometer, a reflux condenser and a stirrer, then moving the three-neck flask into a water bath constant temperature tank, stirring for 2 hours under the conditions of the temperature of 90 ℃, the rotating speed of 800r/min and condensation reflux, then removing the water bath constant temperature tank, continuing condensation reflux and stirring until the temperature of a reaction system is reduced to room temperature, and obtaining the adhesive.
The adding amount of the sodium pyrophosphate is 5.5 percent of the mass of the water glass.
The preparation method of the foaming microsphere comprises the following steps:
s71: adding water, sodium thiosulfate and ammonium persulfate into a beaker, and carrying out ultrasonic treatment for 30-50min to obtain a mixed solution B;
s72: adding liquid paraffin oil, span 80, calcium stearate, acrylonitrile, methyl methacrylate, methacrylic acid and 1, 4-butanediol dimethacrylate into a flask, and stirring for 20min under the condition that the rotating speed is 1000r/min to obtain an oily substance;
s73: adding the mixed solution B into the oily substance while stirring, and continuously stirring and dispersing for 50min to obtain a mixed solution C;
s74: adding the mixed solution C into a flask, placing the flask into a water bath, firstly heating to 55 ℃ for reaction for 1h, then heating to 60 ℃ for reaction for 8h, then heating to 65 ℃ for reaction for 1h, cooling to room temperature after the reaction is finished, then carrying out vacuum filtration, respectively washing a filter cake for 3 times by using ethanol and distilled water, then placing the filter cake into a vacuum drying oven, and carrying out vacuum drying for 30h at the temperature of 50 ℃ to obtain the foaming microsphere.
In the step S71, the mass ratio of the water to the sodium thiosulfate to the ammonium persulfate is 50:2: 5; in the step S72, the mass ratio of the liquid paraffin oil, the span 80, the calcium stearate, the acrylonitrile, the methyl methacrylate, the methacrylic acid and the 1, 4-butanediol dimethacrylate is 200:1.5:0.2:6:12:12: 1.
A preparation method of a metal and ceramic composite grinding medium comprises the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconia and muscovite into a ball mill, ball-milling to 3000 meshes, and discharging to obtain superfine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foaming microspheres into water, and stirring and dispersing for 2 hours at the rotating speed of 800r/min to obtain mixed slurry;
step three: adding the superfine powder into the mixed slurry under the conditions of 100 ℃ and 500r/min of rotating speed, controlling the adding time of the mixed slurry to be 40min, and continuing stirring for 2h after the adding is finished to obtain a mixture;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form a ball, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1500 ℃ at a heating rate of 3 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into a metal liquid for soaking for 3s, taking out, naturally cooling to room temperature, putting into an oven for drying to obtain a dried substance, putting into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
Comparative example 1:
comparative example 1 is a commercially available ceramic grinding media;
the performances of examples 1 to 3 and comparative example 1 were examined, and the results were as follows:
sample (I) Wear rate (g/kg. h) Bulk Density (g/cm)3) Vickers hardness (HV10)
Example 1 0.28 3.02 1489
Example 2 0.26 3.08 1512
Example 3 0.25 3.15 1535
Comparative example 1 0.96 2.74 1310
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. The metal and ceramic composite grinding medium is characterized by comprising the following components in parts by weight:
40-60 parts of modified kaolin, 8-12 parts of silicon carbide, 10-20 parts of feldspar, 6-8 parts of wollastonite, 5-7 parts of calcium oxide, 5-7 parts of zirconium oxide, 3-5 parts of muscovite mica, 2-4 parts of sodium dodecyl benzene sulfonate, 2-4 parts of binder, 1-2 parts of polyvinyl alcohol, 20-30 parts of foamed microspheres and 40-60 parts of water;
the metal and ceramic composite grinding medium is prepared by the following steps:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconia and muscovite into a ball mill, ball-milling to 2000-3000 meshes, and discharging to obtain ultrafine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foamed microspheres into water, and stirring and dispersing for 1-2 hours at the rotation speed of 500-;
step three: adding the superfine powder into the mixed slurry under stirring at the temperature of 90-100 ℃ and the rotating speed of 300-;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form a ball, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1400 ℃ at a heating rate of 1-3 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into the metal liquid to be soaked for 1-3s, taking out the hollow microspheres to be naturally cooled to room temperature, putting the hollow microspheres into an oven to be dried to obtain a dried substance, putting the dried substance into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
2. The metal and ceramic composite grinding medium according to claim 1, wherein the molten metal is a melt obtained by mixing and melting one or more of iron, copper, aluminum, manganese, zinc and chromium in any proportion.
3. The metal and ceramic composite grinding medium of claim 1, wherein the modified kaolin is prepared by the following method:
s31: adding gamma-aminopropyltriethoxysilane into isopropanol, adjusting pH of the reaction system to 3-5 with citric acid-sodium dihydrogen phosphate buffer solution with pH of 2.2, heating in water bath at 35 deg.C and rotation speed of 50-100r/min, and stirring for 40-60min to obtain a transparent mixed solution A;
s32: adding calcined kaolin into the mixed solution A, stirring for 1-2h under the condition that the rotation speed is 300-500r/min, then adding absolute ethyl alcohol, continuously stirring for 1-2h in a water bath constant temperature bath at the temperature of 70-75 ℃, then heating to 85 ℃ until the solvent is completely evaporated, then carrying out suction filtration, placing the filter cake into a vacuum drying box, carrying out vacuum drying for 20-30h under the temperature of 70-75 ℃, and then grinding to obtain the modified kaolin.
4. The metal and ceramic composite grinding medium according to claim 3, wherein the amount ratio of the gamma-aminopropyltriethoxysilane to the isopropanol in step S31 is 1 g: 50 mL; in the step S32, the dosage ratio of the calcined kaolin to the mixed solution A to the absolute ethyl alcohol is 100 g: 100mL of: 10-20 mL.
5. The metal and ceramic composite grinding medium of claim 1, wherein the binder is prepared by the following method:
s51: ultrasonically dispersing water glass for 0.5-1h under the condition that the frequency is 80-120kHz to obtain a water glass dispersion;
s52: adding the water glass dispersion and sodium pyrophosphate into a three-neck flask provided with a thermometer, a reflux condenser and a stirrer, then moving the three-neck flask into a water bath thermostatic bath, stirring for 1-2h under the conditions that the temperature is 70-90 ℃, the rotating speed is 500 plus materials at 800r/min, and then removing the water bath thermostatic bath, continuing to perform condensation reflux and stirring until the temperature of a reaction system is reduced to the room temperature, thus obtaining the adhesive.
6. The metal and ceramic composite grinding medium according to claim 5, wherein the sodium pyrophosphate is added in an amount of 4.5 to 5.5% by mass based on the water glass.
7. The metal and ceramic composite grinding medium of claim 1, wherein the preparation method of the expanded microspheres is as follows:
s71: adding water, sodium thiosulfate and ammonium persulfate into a beaker, and carrying out ultrasonic treatment for 30-50min to obtain a mixed solution B;
s72: adding liquid paraffin oil, span 80, calcium stearate, acrylonitrile, methyl methacrylate, methacrylic acid and 1, 4-butanediol dimethacrylate into a flask, and stirring for 10-20min under the condition that the rotating speed is 1000r/min to obtain an oily substance;
s73: adding the mixed solution B into the oily substance while stirring, and continuously stirring and dispersing for 30-50min to obtain a mixed solution C;
s74: adding the mixed solution C into a flask, placing the flask into a water bath, firstly heating to 55 ℃ for reaction for 1h, then heating to 60 ℃ for reaction for 8h, then heating to 65 ℃ for reaction for 1h, cooling to room temperature after the reaction is finished, then carrying out vacuum filtration, respectively washing a filter cake for 2-3 times by using ethanol and distilled water, then placing the filter cake into a vacuum drying oven, and carrying out vacuum drying for 25-30h at the temperature of 50 ℃ to obtain the foamed microspheres.
8. The metal and ceramic composite grinding medium according to claim 7, wherein the mass ratio of the water to the sodium thiosulfate to the ammonium persulfate in the step S71 is 50:2: 5; in the step S72, the mass ratio of the liquid paraffin oil, the span 80, the calcium stearate, the acrylonitrile, the methyl methacrylate, the methacrylic acid and the 1, 4-butanediol dimethacrylate is 200:1.5:0.2:6:12:12: 1.
9. The method for preparing a metal and ceramic composite grinding medium according to claim 1, comprising the steps of:
the method comprises the following steps: adding modified kaolin, silicon carbide, feldspar, wollastonite, calcium oxide, zirconia and muscovite into a ball mill, ball-milling to 2000-3000 meshes, and discharging to obtain ultrafine powder;
step two: adding sodium dodecyl benzene sulfonate, a binder, polyvinyl alcohol and foamed microspheres into water, and stirring and dispersing for 1-2 hours at the rotation speed of 500-;
step three: adding the superfine powder into the mixed slurry under stirring at the temperature of 90-100 ℃ and the rotating speed of 300-;
step four: putting the mixture into a ball forming mill, adding water, uniformly mixing, rolling to form a ball, polishing, then drying in a drying device, drying to obtain a ceramic microbead blank, putting the ceramic microbead blank into a kiln, heating to 1400 ℃ at a heating rate of 1-3 ℃/min, firing to obtain ceramic hollow microbeads, and putting the hollow ceramic microbeads into a ceramic grinding machine for grinding to obtain ceramic hollow microspheres with rough surfaces;
step five: and (3) putting the hollow microspheres with rough surfaces into the metal liquid to be soaked for 1-3s, taking out the hollow microspheres to be naturally cooled to room temperature, putting the hollow microspheres into an oven to be dried to obtain a dried substance, putting the dried substance into a polishing machine, and polishing to obtain the metal and ceramic composite grinding medium.
CN202011509818.8A 2020-12-19 2020-12-19 Metal and ceramic composite grinding medium and preparation method thereof Pending CN112624729A (en)

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CN116283242A (en) * 2023-04-13 2023-06-23 安徽致磨新材料科技有限公司 Preparation method of metal-ceramic composite grinding medium with adjustable density

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CN113786821A (en) * 2021-10-20 2021-12-14 辽宁基伊能源科技有限公司 Desulfurizer containing high-density composite nano active calcium and preparation method and application thereof
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Application publication date: 20210409