CN101786867A - Preparation method for zirconium silicate ball - Google Patents
Preparation method for zirconium silicate ball Download PDFInfo
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- CN101786867A CN101786867A CN201010122895A CN201010122895A CN101786867A CN 101786867 A CN101786867 A CN 101786867A CN 201010122895 A CN201010122895 A CN 201010122895A CN 201010122895 A CN201010122895 A CN 201010122895A CN 101786867 A CN101786867 A CN 101786867A
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Abstract
The invention discloses a preparation method for zirconium silicate balls, which relates to a grinding medium and provides a preparation method for zirconium silicate balls by spray granulation, isopressing and high-temperature sintering. The method comprises the following steps: adding grinding disperant, additive and dispersion medium into zircon sand, and grinding to obtain sizing agent; granulating the sizing agent to obtain zirconium silicate particles; forming the zirconium silicate particles to obtain bisuits of the zirconium silicate balls; and sintering the zirconium silicate ball bisuits to obtain the zirconium silicate balls. The prepared zirconium silicate balls have the advantages of high density, high strength, high sphericity degree, high abrasion performance and the like. By experiments, the prepared zirconium silicate balls are characterized in that the volume density thereof are larger than 4.0g/cm<3>, the sphericity degree is above 90%, the mohs hardness is more than 7.4 and the compression strength is more than 750N. The ball consists of the compact zirconium silicate particles, is free from capillary tips and cavities; and compared with the other similar balls, the balls of the invention have larger density and compression strength.
Description
Technical field
The present invention relates to a kind of grinding medium, especially relate to a kind of preparation method of zirconium silicate ball.
Background technology
Ball mill is widely used in fields such as metallurgy, mineral products, electric power, building materials, chemical industry, is a kind of use disintegrating apparatus very widely.Grinding medium is the key of ball mill comminuting matter, and its shape is generally spheroid or right cylinder, relies on the motion of various complexity such as the rolling of grinding medium in ball mill, bump, extruding, friction, and material is pulverized.The quality of grinding medium not only directly has influence on the height of production efficiency, but also can have influence on the quality of quality product.
Developing rapidly of superfine powder processing industry driven the research and development and the production of grinding medium.Develop the high-quality grinding medium of high quality and high mill efficiency, to the powder processing industry is had positive contribution, and create great economic benefit.At present, various mill balls (pearl) are arranged on the grinding medium market, its performance is different, price does not wait.How the user uses suitable and best medium, effectively reduces cost, and improves processing benefit, has become the very important problem of industry of grinding.Need the diversity of abrasive product and the complicacy of production technique, determined the diversity of grinding medium.Multiple grinding ball as granulated glass sphere, alumina balls, zirconium silicate pearl, pure zirconium pearl and chromium steel ball etc., according to different converted productss and field of employment, will occupy different status on market.
It is grinding medium that the coml measure of grinding is adopted usually as quartz sand, granulated glass sphere, ceramic dielectic or steel ball.Wherein, the density of quartz sand and granulated glass sphere is very low, has only 2.6g/cm
3, the hardness of granulated glass sphere is very low again, and this has just limited the material that can grind with quartz sand and granulated glass sphere.The use of small ball can only be limited in the situation that the iron pollution that is produced by the abrasion of small ball in the process of lapping can allow.
Usually the zirconium ball is meant zirconium silicate (ZrSiO
4) ball and zirconium white (ZrO
2) ball.The theoretical density of zirconium silicate is 4.6g/cm
3, 7～8 grades of Mohs' hardness, fusing point is 2430 ℃, but it begins to be decomposed into ZrO in the time of 1540 ℃
2And SiO
2The zirconium silicate pearl is made up of the zirconium silicate crystal grain of all even densifications, and crystal boundary has low-melting SiO
2Glassy phase.Wherein zirconic content is generally 64%～70%, excellent ball-type degree and intermediate density have increased mill efficiency and have reduced the abrasion of equipment, are fit to the dispersion and the grinding of viscosity higher and medium-hard material (as titanium dioxide, lime carbonate, zircon powder, kaolin etc.).
The production technique of existing zirconium silicate pearl as grinding medium is essentially two kinds of high-temperature melting method and sintering processs.The shortcoming of scorification is to form defective easily.Pearl is at the high temperature fused state compacted under, if a certain critical technical parameter is not controlled well, formed product will form defective easy broken pearl: bubble pearl, tail pearl and flat (ellipse) pearl.Above pearl is because of having region of stress concentration, and is broken easily in the middle of grinding, so should avoid having in the product too much this type of pearl when using as far as possible.The ball diameter that this kind method is made is difficult to do greatly, generally below 2mm.And adopt sintering process to prepare zirconium silicate ball, and the moulding of normally rolling of ball base substrate, its shortcoming is to be difficult to prepare than ball great, that hardness is high and wear(ing)value is low.At present, domestic have a nine divisions of China in remote antiquity grinding medium company limited with what high-temperature melting method was produced zirconium silicate ball, its product main exit, and particle size range 0.2～2.5mm, deviation is 0.2～0.4mm.And domestic enterprise uses mainly is the zirconium silicate ball of import Germany Nai Nuo company, particle size range 0.4～2.8mm, and deviation is 0.2mm.
At present, external method of producing zirconium silicate ball, for example the zirconium silicate of anti-promise pearl NanorZr-64 adopts titration moulding in the electrolytic solution, the advanced technologies of high temperature sintering phasing, pearl is made up of the zirconium silicate particulate of densification, refused capillary and cavity, than other similar pearl bigger density and crushing strength have been arranged, its rate of wear is 1/2 of " melting " method pearl.The zirconium silicate of anti-promise pearl NanorZr-70 adopts moulding in the electrolytic solution, and the technology of high-temperature roasting is made.Pearl is made up of the zirconium silicate crystal grain of all even densifications, has refused cavity pearl, tail pearl and snowman pearl etc.
Application number is that 99118965.5 Chinese patent discloses a kind of Zirconite ball making technology, and this patent adopts a kind of fusion zircon to make the method for silicon zirconium microballoon.This method is that the raw material that will add solubility promoter places the DC-ore-heating furnace melting, produces high number airflow with air compressor machine and jets, and makes the zirconite ball microballon.The shortcoming of this method is that zirconium silicate ball size is little, and particle size uniformity is poor.
Up to now, use sintering process to prepare diameter and be the zirconium silicate ball more than the 5mm, but, also not have the product of being satisfied with on the market because technical that is that all right is ripe.Therefore, the high-quality zirconium silicate ball of developing serial diameter will have huge market outlook.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who adopts the zirconium silicate ball of mist projection granulating, isostatic pressing and high temperature sintering.
Technical scheme of the present invention is that zircon sand is prepared burden, mix dispersion agent and admixture, with the deionized water is dispersion medium, ball milling mixes and obtains stable slurry, then with slurry spray-drier granulation, and moulding in the isostatic pressing machine of then particulate material being packed into, the demoulding, obtain the zirconium silicate ball biscuit, with zirconium silicate ball biscuit high temperature sintering in air atmosphere, promptly obtain zirconium silicate ball at last.
The present invention includes following steps:
1) in zircon sand, adds grinding dispersion agent, admixture and dispersion medium, get slurry after the grinding;
2) the slurry granulation that step 1) is made gets zirconium silicate particles;
3) with step 2) the zirconium silicate particles moulding that obtains, the zirconium silicate ball biscuit;
4) with the zirconium silicate ball biscuit sintering of step 3) gained, get the product zirconium silicate ball.
In step 1), by mass percentage, the consumption of described grinding dispersion agent can be 0.1%～2% of total slurry, and the consumption of admixture can be 3%～10% of zircon sand, and the consumption of dispersion medium can be 15%～50% of zircon sand; Described grinding dispersion agent is optional from polypropylene phthalein amine or ammonium citrate etc., and described admixture can be commercial alumina powder etc., and described dispersion medium can be deionized water etc.
In step 2) in, described granulation can be adopted the spray-drier granulation, and the processing parameter of granulation can be 250～300 ℃ of inlet temperatures, 110～150 ℃ of temperature outs; The water ratio of described zirconium silicate particles can be 0.2%～2% by mass percentage, and the granularity of zirconium silicate particles can be the particulate material of 100～280 mesh sieves.
In step 3), described moulding can be adopted the isostatic pressing machine moulding, and pressure can be 120～200MPa, and the dwell time can be 150～200s.
In step 4), described sintering can adopt sintering in air atmosphere, the agglomerating temperature: the speed with 250～300 ℃/h is heated to 1450～1550 ℃ of temperature, and preferably isothermal is incubated 1h, and sample cools off with stove then.
Outstanding advantage of the present invention is: prepared zirconium silicate ball has density height, intensity height, ball-type degree height and wear resistance advantages of higher, and its preparation technology is easy, reliable and stable, production efficiency is high, and the large-sized product of energy moulding is convenient to realize industrialization.Through test, the volume density that makes zirconium silicate ball is 4.0g/cm
3More than, the ball-type degree is more than 90%, and Mohs' hardness is more than 7.4, more than the ultimate compression strength 750N.Ball is made up of the zirconium silicate particulate of densification, has refused capillary and cavity, than other similar pearl bigger density and crushing strength is arranged.Product has competitive power, is convenient to Industry Promotion, has very considerable market outlook.
Embodiment
It is raw material that the present invention adopts zircon sand, and the zircon sand main component is zirconium silicate (ZrSiO
4), ZrO
2Content is 62.38%～67.02%, SiO
2Content also has other association oxide compounds greater than 1% 31.74%～33.17%, and granularity is all less than 0.18mm.
Embodiment 1
1, be example with Australian import zircon sand and commercially available commercial alumina powder.The zircon sand main component is zirconium silicate (ZrSiO
4), ZrO
2Content is 65.16%, SiO
2Content is 32.64%, Al
2O
3Content is 1.84%, and CaO content is 1.01%, also has other a spot of Fe
2O
3, TiO
2, granularity is all less than 0.18mm.Commercially available commercial alumina powder purity＞99.5%, median size are 1 μ m.
2, polypropylene phthalein amine dispersion agent in the ball mill is accounted for 2% of slurry, the aluminum oxide powder admixture accounts for 8% of zircon sand, and the dispersion medium deionized water accounts for 45% of zircon sand, and the ball milling uniform mixing makes stable slurry.
3, with step 2) slurry of gained sends into the spray-drier granulation, 280～290 ℃ of inlet temperatures, 130～140 ℃ of temperature outs make water ratio and are 1% zirconium silicate particles, choose the particulate material that granularity is 100～280 mesh sieves.
4, the particulate material of step 3) gained is loaded mould, isostatic pressing, pressure 150MPa, pressurize 180s, the demoulding then obtains the zirconium silicate ball biscuit.
5, with zirconium silicate ball work in-process sintering in air atmosphere of step 4) gained, be heated to 1500 ℃ of the temperature of isothermal insulation with the speed of 280 ℃/h, isothermal insulation 1h, sample cools off with stove then, promptly obtains final zirconium silicate ball.
6, the volume density of present embodiment mesosilicic acid zirconium ball is 4.4g/cm
3, diameter is 2.0mm (diameter of spherical die cavity is 2.0mm in the mould), ball-type degree 98%, Mohs' hardness 7.7, ultimate compression strength 960N.
Embodiment 2
Raw material and technological process are similar to Example 1.Polypropylene phthalein amine dispersion agent in the ball mill is accounted for 1.5% of slurry, the aluminum oxide powder admixture accounts for 5% of zircon sand, the dispersion medium deionized water accounts for 30% of zircon sand, make stable slurry, the slurry mist projection granulating of gained, 280～290 ℃ of inlet temperatures, 125～135 ℃ of temperature outs, make water ratio and be 1.2% zirconium silicate particles, choosing granularity is the filling mould of the particulate material of 100～280 mesh sieves, isostatic pressing, pressure 150MPa, pressurize 180s is heated to 1500 ℃ of the temperature of isothermal insulation, isothermal insulation 1h with the speed of 280 ℃/h.The volume density of present embodiment mesosilicic acid zirconium ball is 4.2g/cm
3, diameter is 5mm (diameter of spherical die cavity is 5mm in the mould), ball-type degree 98%, Mohs' hardness 7.5, ultimate compression strength 900N.
Embodiment 3
Raw material and technological process are similar to Example 1.Polypropylene phthalein amine dispersion agent in the ball mill is accounted for 1.0% of slurry, the aluminum oxide powder admixture accounts for 8% of zircon sand, the dispersion medium deionized water accounts for 30% of zircon sand, make stable slurry, the slurry mist projection granulating of gained, 280～290 ℃ of inlet temperatures, 130～140 ℃ of temperature outs, make water ratio and be 1.1% zirconium silicate particles, choosing granularity is the filling mould of the particulate material of 100～280 mesh sieves, isostatic pressing, pressure 150MPa, pressurize 180s is heated to 1500 ℃ of the temperature of isothermal insulation, isothermal insulation 1h with the speed of 270 ℃/h.The volume density 4.4g/cm of present embodiment mesosilicic acid zirconium ball
3, diameter is 9.9mm (diameter of spherical die cavity is 10mm in the mould), ball-type degree 95%, Mohs' hardness 7.6, ultimate compression strength 940N.
Embodiment 4
Raw material and technological process are similar to Example 1.Polypropylene phthalein amine dispersion agent in the ball mill is accounted for 1.0% of slurry, the aluminum oxide powder admixture accounts for 4% of zircon sand, the dispersion medium deionized water accounts for 45% of zircon sand, make stable slurry, the slurry mist projection granulating of gained, 275～285 ℃ of inlet temperatures, 120～130 ℃ of temperature outs, make water ratio and be 1.4% zirconium silicate particles, choosing granularity is the filling mould of the particulate material of 100～280 mesh sieves, isostatic pressing, pressure 180MPa, pressurize 200s is heated to 1530 ℃ of the temperature of isothermal insulation, isothermal insulation 1h with the speed of 260 ℃/h.The volume density 4.1g/cm of present embodiment mesosilicic acid zirconium ball
3, diameter is 14.5mm (diameter of spherical die cavity is 15mm in the mould), ball-type degree 95%, Mohs' hardness 7.4, ultimate compression strength 800N.
Embodiment 5
Raw material and technological process are similar to Example 1.Polypropylene phthalein amine dispersion agent in the ball mill is accounted for 2% of slurry, the aluminum oxide powder admixture accounts for 5% of zircon sand, the dispersion medium deionized water accounts for 25% of zircon sand, make stable slurry, the slurry mist projection granulating of gained, 280～290 ℃ of inlet temperatures, 130～140 ℃ of temperature outs, make water ratio and be 0.9% zirconium silicate particles, choosing granularity is the filling mould of the particulate material of 100～280 mesh sieves, isostatic pressing, pressure 130MPa, pressurize 150s is heated to 1500 ℃ of the temperature of isothermal insulation, isothermal insulation 1h with the speed of 280 ℃/h.The volume density 4.0g/cm of present embodiment mesosilicic acid zirconium ball
3, diameter is 19.5mm (diameter of spherical die cavity is 20mm in the mould), ball-type degree 95%, Mohs' hardness 7.4, ultimate compression strength 760N.
Embodiment 6
Raw material and technological process are similar to Example 1.Polypropylene phthalein amine dispersion agent in the ball mill is accounted for 0.5% of slurry, the aluminum oxide powder admixture accounts for 8% of zircon sand, the dispersion medium deionized water accounts for 50% of zircon sand, make stable slurry, the slurry mist projection granulating of gained, 280～290 ℃ of inlet temperatures, 125～135 ℃ of temperature outs, make water ratio and be 1.5% zirconium silicate particles, choosing granularity is the filling mould of the particulate material of 100～280 mesh sieves, isostatic pressing, pressure 200MPa, pressurize 200s is heated to 1530 ℃ of the temperature of isothermal insulation, isothermal insulation 1h with the speed of 250 ℃/h.The volume density 4.3g/cm of present embodiment mesosilicic acid zirconium ball
3, diameter is 24mm (diameter of spherical die cavity is 25mm in the mould), ball-type degree 90%, Mohs' hardness 7.6, ultimate compression strength 920N.
Embodiment 7
Raw material and technological process are similar to Example 1.Polypropylene phthalein amine dispersion agent in the ball mill is accounted for 1.5% of slurry, the aluminum oxide powder admixture accounts for 6% of zircon sand, the dispersion medium deionized water accounts for 35% of zircon sand, make stable slurry, the slurry mist projection granulating of gained, 280～285 ℃ of inlet temperatures, 130～140 ℃ of temperature outs, make water ratio and be 0.8% zirconium silicate particles, choosing granularity is the filling mould of the particulate material of 100～280 mesh sieves, isostatic pressing, pressure 130MPa, pressurize 150s is heated to 1480 ℃ of the temperature of isothermal insulation, isothermal insulation 1h with the speed of 300 ℃/h.The volume density 4.2g/cm of present embodiment mesosilicic acid zirconium ball
3, diameter is 28mm (diameter of spherical die cavity is 30mm in the mould), ball-type degree 90%, Mohs' hardness 7.5, ultimate compression strength 860N.
Claims (10)
1. the preparation method of a zirconium silicate ball is characterized in that may further comprise the steps:
1) in zircon sand, adds grinding dispersion agent, admixture and dispersion medium, get slurry after the grinding;
2) the slurry granulation that step 1) is made gets zirconium silicate particles;
3) with step 2) the zirconium silicate particles moulding that obtains, the zirconium silicate ball biscuit;
4) with the zirconium silicate ball biscuit sintering of step 3) gained, get the product zirconium silicate ball.
2. the preparation method of a kind of zirconium silicate ball as claimed in claim 1, it is characterized in that in step 1), by mass percentage, the consumption of described grinding dispersion agent is 0.1%～2% of total slurry, the consumption of admixture is 3%～10% of a zircon sand, and the consumption of dispersion medium is 15%～50% of a zircon sand.
3. the preparation method of a kind of zirconium silicate ball as claimed in claim 1 is characterized in that in step 1), and described grinding dispersion agent is selected from polypropylene phthalein amine or ammonium citrate.
4. the preparation method of a kind of zirconium silicate ball as claimed in claim 1 is characterized in that in step 1), and described admixture is the commercial alumina powder.
5. the preparation method of a kind of zirconium silicate ball as claimed in claim 1 is characterized in that in step 1), and described dispersion medium is a deionized water.
6. the preparation method of a kind of zirconium silicate ball as claimed in claim 1 is characterized in that in step 2) in, the spray-drier granulation is adopted in described granulation, and the processing parameter of granulation is 250～300 ℃ of inlet temperatures, 110～150 ℃ of temperature outs.
7. the preparation method of a kind of zirconium silicate ball as claimed in claim 1 is characterized in that in step 2) in, the water ratio of described zirconium silicate particles is 0.2%～2% by mass percentage.
8. as the preparation method of claim 1 or 7 described a kind of zirconium silicate balls, it is characterized in that in step 2) in, the granularity of described zirconium silicate particles is the particulate material of 100～280 mesh sieves.
9. the preparation method of a kind of zirconium silicate ball as claimed in claim 1 is characterized in that in step 3), and the isostatic pressing machine moulding is adopted in described moulding, and pressure is 120～200MPa, and the dwell time is 150～200s.
10. the preparation method of a kind of zirconium silicate ball as claimed in claim 1, it is characterized in that in step 4), described sintering adopts sintering in air atmosphere, the agglomerating temperature: the speed with 250～300 ℃/h is heated to 1450～1550 ℃ of temperature, isothermal insulation 1h, sample cools off with stove then.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795848A (en) * | 2012-08-02 | 2012-11-28 | 江苏锡阳研磨科技有限公司 | Low-temperature sintered zirconium silicate grinding ball and preparation method thereof |
| WO2013011436A1 (en) | 2011-07-20 | 2013-01-24 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Sintered zircon particle |
| CN103011787A (en) * | 2012-12-20 | 2013-04-03 | 淄博和润研磨材料科技有限公司 | Zirconium silicate ceramic grinding medium and preparation method thereof |
| CN104609868A (en) * | 2015-01-13 | 2015-05-13 | 江苏金石研磨有限公司 | Dispersant for wet grinding of zirconium-silicate-based composite ceramic raw materials and preparation method of dispersant |
| CN105855000A (en) * | 2016-05-26 | 2016-08-17 | 景德镇百特威尔新材料有限公司 | Ore grinding method adopting ceramic dielectric applied to tower mill |
| CN106000566A (en) * | 2016-05-26 | 2016-10-12 | 景德镇百特威尔新材料有限公司 | Novel ball-milling method used for magnetic material industry |
| CN109678499A (en) * | 2018-12-30 | 2019-04-26 | 郑州可塑金新材料有限公司 | A method of using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads |
| CN112457006A (en) * | 2020-12-20 | 2021-03-09 | 长沙县新光特种陶瓷有限公司 | Preparation process of zirconium silicate ball filler |
| CN114260067A (en) * | 2021-12-22 | 2022-04-01 | 北矿机电科技有限责任公司 | Grinding method for slurry difficult to grind |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013011436A1 (en) | 2011-07-20 | 2013-01-24 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Sintered zircon particle |
| CN102795848A (en) * | 2012-08-02 | 2012-11-28 | 江苏锡阳研磨科技有限公司 | Low-temperature sintered zirconium silicate grinding ball and preparation method thereof |
| CN102795848B (en) * | 2012-08-02 | 2013-10-23 | 江苏锡阳研磨科技有限公司 | Low-temperature sintered zirconium silicate grinding ball and preparation method thereof |
| CN103011787A (en) * | 2012-12-20 | 2013-04-03 | 淄博和润研磨材料科技有限公司 | Zirconium silicate ceramic grinding medium and preparation method thereof |
| CN104609868A (en) * | 2015-01-13 | 2015-05-13 | 江苏金石研磨有限公司 | Dispersant for wet grinding of zirconium-silicate-based composite ceramic raw materials and preparation method of dispersant |
| CN105855000A (en) * | 2016-05-26 | 2016-08-17 | 景德镇百特威尔新材料有限公司 | Ore grinding method adopting ceramic dielectric applied to tower mill |
| CN106000566A (en) * | 2016-05-26 | 2016-10-12 | 景德镇百特威尔新材料有限公司 | Novel ball-milling method used for magnetic material industry |
| CN105855000B (en) * | 2016-05-26 | 2018-05-22 | 景德镇百特威尔新材料有限公司 | The milling method that ceramic dielectric is applied in tower grinding machine |
| CN109678499A (en) * | 2018-12-30 | 2019-04-26 | 郑州可塑金新材料有限公司 | A method of using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads |
| CN112457006A (en) * | 2020-12-20 | 2021-03-09 | 长沙县新光特种陶瓷有限公司 | Preparation process of zirconium silicate ball filler |
| CN114260067A (en) * | 2021-12-22 | 2022-04-01 | 北矿机电科技有限责任公司 | Grinding method for slurry difficult to grind |
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Application publication date: 20100728 |