CN111302791A - Zirconia micro-bead and preparation method thereof - Google Patents
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Abstract
The invention discloses zirconia microspheres and a preparation method thereof, wherein zirconia high-solid-content slurry and titration emulsion are heated, titrated, settled and coagulated into zirconia spheres, and then subjected to low-temperature binder removal and sintering to obtain the zirconia microspheres, wherein the mass ratio of the zirconia high-solid-content slurry to the titration emulsion is 4-6:4-6, and the zirconia high-solid-content slurry is prepared from the following components in parts by weight: 80-100 parts of zirconium oxide powder, 16-20 parts of deionized water, 1-3 parts of ammonium polyacrylate dispersant, 2-3 parts of acrylamide and 0.2-0.4 part of N' N-methylene bisacrylamide; the titration emulsion is prepared from the following components in percentage by volume: 60-80% of dimethyl silicone oil, 19-39% of propylene glycol and 1% of span 80. The zirconia microspheres and the preparation method thereof solve the problems of poor quality and size stability, easy bead breaking and the like of the existing zirconia microspheres, have the advantages of simple process, zero pollution, good product size stability and the like, and are easy to screen and stable in quality.
Description
Technical Field
The invention relates to the technical field of inorganic materials, in particular to zirconia microspheres and a preparation method thereof.
Background
In recent years, with the development of the material industry and the advancement of the sand mill technology, the demand for the grinding medium for ultrafine grinding and nano grinding of the material has been increasing. The zirconia microspheres have outstanding excellent performances of high density, high strength, acid and alkali corrosion resistance, extremely low self-abrasion and the like, so that the zirconia microspheres stand out in various grinding medium materials, the grinding efficiency and the grinding fineness of the materials are greatly improved, the processing pollution of the ground materials is avoided due to zero pollution, and the application prospect is very wide.
Then, the rolling process is usually adopted in the processing and production of the zirconia micro beads at present, and the zirconia micro beads prepared by the rolling process have the defects of internal defects, wide size range and the like, and particularly the determination on the micro beads with the diameter of less than 0.5mm is more obvious, so that the defects of difficulty in screening, bead breaking risk and the like exist in the practical application of the micro beads and need to be solved urgently.
In view of the above, there is a need to develop a zirconia bead and a method for preparing the same, which can solve the above problems and has the advantages of good dimensional stability and consistency, basically no internal defects, wide size range, easy sieving, and the like.
Disclosure of Invention
The invention aims to provide zirconia microspheres and a preparation method thereof, which aim to solve the problems of poor quality and dimensional stability, easy bead breaking and the like of the existing zirconia microspheres, have the advantages of simple process, zero pollution, good product dimensional stability and the like, and are easy to screen and stable in quality.
The technical scheme adopted by the invention to achieve the aim is as follows:
the zirconia micro-bead is obtained by heating, titrating and settling zirconia high-solid slurry and titrating emulsion, condensing the slurry and the titrating emulsion into a zirconia sphere, and then performing low-temperature binder removal and sintering, wherein the mass ratio of the zirconia high-solid slurry to the titrating emulsion is 4-6: 4-6.
Preferably, the zirconia high-solid-content slurry is prepared from the following components in parts by weight: 80-100 parts of zirconia powder, 16-20 parts of deionized water, 1-3 parts of ammonium polyacrylate dispersant, 2-3 parts of acrylamide and 0.2-0.4 part of N, N-methylene bisacrylamide.
Preferably, the titration emulsion is prepared from the following components in percentage by volume: 60-80% of dimethyl silicone oil, 19-39% of propylene glycol and 1% of span 80.
Preferably, the zirconia powder is prepared from the following components in parts by weight: 100 parts of zirconia powder, 120 parts of deionized water, 240 parts of deionized water, 2-4 parts of ammonium polyacrylate, 4-6 parts of hexadecyl trimethyl ammonium bromide and 8-10 parts of silane coupling agent ethanol solution.
Preferably, the ammonium polyacrylate dispersant is low molecular weight ammonium polyacrylate synthesized by using acrylic acid as a monomer, ammonium persulfate as an initiator, isopropanol as a chain transfer agent and a heat transfer agent, and the viscosity-average molecular mass of the ammonium polyacrylate is (0.3-1.0) x 104.
The preparation method of the zirconia microspheres comprises the following steps:
s1: preparing high-solid zirconium oxide slurry and titration emulsion according to the raw material proportion set by claim 1; firstly heating the titration emulsion and maintaining the titration emulsion at a certain temperature, then titrating the zirconia high-solid slurry into the heated titration emulsion at normal pressure by a dropper, slowly settling, and evaporating and condensing water to form zirconia green body balls;
s2: taking out the zirconia sphere green body balls, draining, and discharging glue at low temperature in a glue discharging furnace to obtain a zirconia micro-bead green body;
s3: and (4) feeding the zirconia micro-bead blank into a sintering furnace for high-temperature sintering to obtain the zirconia micro-beads.
Preferably, the high-solid-content zirconia slurry is formed by mixing raw materials and grinding the raw materials in a roller ball mill, and the grinding time is 1.5 to 2.5 hours at normal temperature.
Preferably, the titration heating temperature in the step S1 is 110-130 ℃; the glue discharging temperature in the step S2 is 850-1050 ℃, and the glue discharging time is 1.5-2.5 hours.
Preferably, the sintering temperature in the step S3 is 1300-1500 ℃, and the sintering time is 3-5 hours.
Compared with the prior art, the invention has the following beneficial effects:
according to the zirconia microspheres and the preparation method thereof, the zirconia microspheres are obtained by preparing the zirconia high-solid slurry and the titration emulsion, then carrying out titration forming, low-temperature gel discharging and sintering, and the adopted technological method is simple in flow, and the obtained zirconia microspheres are good in size stability and stable in product quality. The adopted titration forming process solves the problem of internal defects in the production and preparation process of the zirconia beads, solves the risk of bead breaking, ensures that the prepared zirconia bead products have stable and consistent sizes, does not have the problem of size screening, basically has no internal defects and has wide size range, completely meets various use requirements, has the performance far superior to that of the existing zirconia bead products in the aspect of the beads with the diameter of less than 0.5mm, has wide application prospect, and can be popularized and applied in a large scale.
The foregoing is a summary of the technical solutions of the present invention, and the present invention is further described below with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments are described in detail. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1: the zirconia micro bead and the preparation method thereof provided by the embodiment of the invention are obtained by heating, titrating and then settling zirconia high-solid slurry and titrating emulsion and condensing the slurry and titrating emulsion into a zirconia sphere, and then performing low-temperature binder removal and sintering, wherein the mass ratio of the zirconia high-solid slurry to the titrating emulsion is 4-6: 4-6. The zirconia high-solid-content slurry is prepared from the following components in parts by weight: 80-100 parts of zirconium oxide powder, 16-20 parts of deionized water, 1-3 parts of ammonium polyacrylate dispersant, 2-3 parts of acrylamide and 0.2-0.4 part of N, N-methylene bisacrylamide; the titration emulsion is prepared from the following components in percentage by volume: 60% -80% of dimethyl silicone oil, 19% -39% of propylene glycol and 1% of span 80; the zirconia powder is prepared from the following components in parts by weight: 100 parts of zirconium oxide powder, 120 parts of deionized water, 240 parts of deionized water, 2-4 parts of ammonium polyacrylate, 4-6 parts of hexadecyl trimethyl ammonium bromide and 8-10 parts of silane coupling agent ethanol solution; the ammonium polyacrylate dispersant is low molecular weight ammonium polyacrylate synthesized by using acrylic acid as a monomer, ammonium persulfate as an initiator, isopropanol as a chain transfer agent and a heat transfer agent, and the viscosity-average molecular mass of the ammonium polyacrylate is (0.3-1.0) x 104.
The embodiment also provides a preparation method of the zirconia micro-bead, which comprises the following steps:
s1: preparing high-solid zirconium oxide slurry and titration emulsion according to the raw material proportion set by claim 1; firstly heating the titration emulsion at a certain temperature, wherein the titration heating temperature is 110-; s2: taking out the zirconia sphere green body balls, draining, and discharging glue at low temperature in a glue discharging furnace to obtain a zirconia micro-bead green body, wherein the glue discharging temperature is 850-; s3: and (3) delivering the zirconia micro-bead blank into a sintering furnace for high-temperature sintering to obtain the zirconia micro-beads, wherein the sintering temperature is 1300-1500 ℃, and the sintering time is 3-5 hours.
Preferably, the high-solid-content zirconia slurry is formed by mixing raw materials and grinding the raw materials in a roller ball mill, wherein the grinding time is 1.5 to 2.5 hours at normal temperature.
Example 2: the zirconia beads and the preparation method thereof provided in this example are substantially the same as those in example 1, except that:
s1, preparing zirconia high-solid-content slurry: the total amount of ingredients is 100kg, 80kg of zirconia powder, 16kg of deionized water, 2kg of ammonium polyacrylate dispersant, 1.8kg of acrylamide and 0.2kg of NN-methylene bisacrylamide are adopted, mixed and then placed in a roller ball mill for grinding, and the mixture is ground for 2 hours at normal temperature; the zirconia powder is prepared from the following components in parts by weight: 100 parts of zirconium oxide powder, 120 parts of deionized water, 2 parts of ammonium polyacrylate, 6 parts of hexadecyl trimethyl ammonium bromide and 8 parts of silane coupling agent ethanol solution;
s2, preparing titration emulsion: preparing a titration emulsion according to the volume ratio of 60 percent of simethicone, 39 percent of propylene glycol and 1 percent of span 80, and uniformly mixing to obtain the product; the mass ratio of the zirconia high-solid-content slurry to the titration emulsion is 4: 6.
S3, titration forming: heating the prepared titration emulsion to 120 +/-5 ℃, maintaining the temperature within the temperature range, titrating the prepared zirconia high-solid slurry into the heated titration emulsion through a dropper under normal pressure, slowly settling liquid drops, evaporating water in the settling process, and condensing into balls to obtain the zirconia ball green-forming balls.
S4, low-temperature rubber discharge: and taking out the zirconia ball green body balls at the bottom of the emulsion, draining, and then sending into a glue discharging furnace for glue discharging for 2 hours at the temperature of 900 ℃ to obtain a zirconia microbead green body.
S5, sintering: and (3) feeding the zirconium oxide microsphere green body after the binder removal into a sintering furnace, and sintering at the high temperature of 1400 ℃ for 4 hours to obtain the zirconium oxide microsphere.
Example 3: the zirconia beads and the preparation method thereof provided in this example are substantially the same as those in examples 1 and 2, except that: the zirconia microspheres are obtained by heating, titrating, settling and condensing zirconia high-solid slurry and titrating emulsion into zirconia spheres, and then carrying out low-temperature binder removal and sintering, wherein the mass ratio of the zirconia high-solid slurry to the titrating emulsion is 6: 4. The zirconia high-solid-content slurry is prepared from the following components in parts by weight: 80 parts of zirconium oxide powder, 20 parts of deionized water, 1 part of ammonium polyacrylate dispersant, 3 parts of acrylamide and 0.2 part of N, N-methylene bisacrylamide; the titration emulsion is prepared from the following components in percentage by volume: 80% of dimethyl silicone oil, 19% of propylene glycol and 1% of span 80; the zirconia powder is prepared from the following components in parts by weight: 100 parts of zirconium oxide powder, 240 parts of deionized water, 4 parts of ammonium polyacrylate, 4 parts of hexadecyl trimethyl ammonium bromide and 10 parts of silane coupling agent ethanol solution. The difference in the preparation method is that the high solid content zirconia slurry is formed by mixing raw materials and grinding the raw materials in a roller ball mill, and the grinding time is 2.5 hours at normal temperature. The titration heating temperature in the step S1 is 110 ℃; the glue discharging temperature in the step S2 is 1050 ℃, and the glue discharging time is 1.5 hours; in the step S3, the sintering temperature is 1500 ℃, and the sintering time is 3 hours.
Example 4: the zirconia beads and the preparation method thereof provided in this example are substantially the same as those in examples 1 and 2, except that: the zirconia microspheres are obtained by heating, titrating, settling and condensing zirconia high-solid slurry and titrating emulsion into zirconia spheres, and then carrying out low-temperature binder removal and sintering, wherein the mass ratio of the zirconia high-solid slurry to the titrating emulsion is 5: 6. The zirconia high-solid-content slurry is prepared from the following components in parts by weight: 95 parts of zirconium oxide powder, 16 parts of deionized water, 3 parts of ammonium polyacrylate dispersant, 2 parts of acrylamide and 0.2 part of N, N-methylene bisacrylamide; the titration emulsion is prepared from the following components in percentage by volume: 68% of simethicone, 31% of propylene glycol and 1% of span 80; the zirconia powder is prepared from the following components in parts by weight: 100 parts of zirconium oxide powder, 180 parts of deionized water, 2 parts of ammonium polyacrylate, 5 parts of hexadecyl trimethyl ammonium bromide and 8 parts of silane coupling agent ethanol solution. The difference in the preparation method is that the high solid content zirconia slurry is formed by mixing raw materials and grinding the raw materials in a roller ball mill, and the grinding time is 2 hours at normal temperature. The titration heating temperature in the step S1 is 120 ℃; the glue discharging temperature in the step S2 is 1000 ℃, and the glue discharging time is 2.5 hours; in the step S3, the sintering temperature is 1400 ℃ and the sintering time is 4 hours.
Example 5: the zirconia beads and the preparation method thereof provided in this example are substantially the same as those in examples 1 and 2, except that: the zirconia microspheres are obtained by heating, titrating, settling and condensing zirconia high-solid slurry and titrating emulsion into zirconia spheres, and then carrying out low-temperature binder removal and sintering, wherein the mass ratio of the zirconia high-solid slurry to the titrating emulsion is 6: 5. The zirconia high-solid-content slurry is prepared from the following components in parts by weight: 90 parts of zirconium oxide powder, 18 parts of deionized water, 3 parts of ammonium polyacrylate dispersant, 2 parts of acrylamide and 0.3 part of N, N-methylene bisacrylamide; the titration emulsion is prepared from the following components in percentage by volume: 70% of dimethyl silicone oil, 29% of propylene glycol and 1% of span 80; the zirconia powder is prepared from the following components in parts by weight: 100 parts of zirconium oxide powder, 200 parts of deionized water, 3 parts of ammonium polyacrylate, 5 parts of hexadecyl trimethyl ammonium bromide and 9 parts of silane coupling agent ethanol solution. The difference in the preparation method is that the high solid content zirconia slurry is formed by mixing raw materials and grinding the raw materials in a roller ball mill, and the grinding time is 1.5 hours at normal temperature. The titration heating temperature in the step S1 is 130 ℃; the glue discharging temperature in the step S2 is 850 ℃, and the glue discharging time is 2.5 hours; in the step S3, the sintering temperature is 1300 ℃ and the sintering time is 5 hours.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention.
Claims (9)
1. The zirconia microspheres are characterized by being prepared by heating, titrating, settling and condensing zirconia high-solid slurry and titrated emulsion into zirconia spheres, and then carrying out low-temperature binder removal and sintering, wherein the mass ratio of the zirconia high-solid slurry to the titrated emulsion is 4-6: 4-6.
2. The zirconia microbead according to claim 1, wherein the zirconia high-solids slurry is prepared from the following components in parts by weight: 80-100 parts of zirconia powder, 16-20 parts of deionized water, 1-3 parts of ammonium polyacrylate dispersant, 2-3 parts of acrylamide and 0.2-0.4 part of N' N-methylene bisacrylamide.
3. The zirconia microspheres of claim 1, wherein the titration emulsion is prepared from the following volume percent: 60-80% of dimethyl silicone oil, 19-39% of propylene glycol and 1% of span 80.
4. The zirconia microbead according to claim 1, wherein the zirconia powder is prepared from the following components in parts by weight: 100 parts of zirconia powder, 120 parts of deionized water, 240 parts of deionized water, 2-4 parts of ammonium polyacrylate, 4-6 parts of hexadecyl trimethyl ammonium bromide and 8-10 parts of silane coupling agent ethanol solution.
5. The zirconia microbead according to claim 1, wherein the ammonium polyacrylate dispersant is low molecular weight ammonium polyacrylate synthesized by using acrylic acid as a monomer, ammonium persulfate as an initiator, isopropanol as a chain transfer agent and a heat transfer agent, and the viscosity-average molecular mass of the ammonium polyacrylate is (0.3-1.0) x 104。
6. A method for preparing the zirconia micro beads according to any one of claims 1 to 5, comprising the steps of:
s1: preparing high-solid zirconium oxide slurry and titration emulsion according to the raw material proportion set by claim 1; firstly heating the titration emulsion and maintaining the titration emulsion at a certain temperature, then titrating the zirconia high-solid slurry into the heated titration emulsion at normal pressure by a dropper, slowly settling, and evaporating and condensing water to form zirconia green body balls;
s2: taking out the zirconia sphere green body balls, draining, and discharging glue at low temperature in a glue discharging furnace to obtain a zirconia micro-bead green body;
s3: and (4) feeding the zirconia micro-bead blank into a sintering furnace for high-temperature sintering to obtain the zirconia micro-beads.
7. The method for preparing zirconia micro beads according to claim 6, wherein the zirconia high solid content slurry is formed by mixing raw materials and grinding the raw materials in a roller ball mill, and the grinding time is 1.5 to 2.5 hours at normal temperature.
8. The method for preparing zirconia beads as claimed in claim 6, wherein the titration heating temperature in step S1 is 110-130 ℃; the glue discharging temperature in the step S2 is 850-1050 ℃, and the glue discharging time is 1.5-2.5 hours.
9. The method for preparing zirconia beads as claimed in claim 6, wherein the sintering temperature in step S3 is 1300-1500 ℃, and the sintering time is 3-5 hours.
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| CN115159981A (en) * | 2022-07-14 | 2022-10-11 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of ceramic granulation powder for plasma spraying |
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