CN101722085B - Grinding technology of high purity sub-nano level superfine zirconium silicate powder - Google Patents

Grinding technology of high purity sub-nano level superfine zirconium silicate powder Download PDF

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CN101722085B
CN101722085B CN2008101955048A CN200810195504A CN101722085B CN 101722085 B CN101722085 B CN 101722085B CN 2008101955048 A CN2008101955048 A CN 2008101955048A CN 200810195504 A CN200810195504 A CN 200810195504A CN 101722085 B CN101722085 B CN 101722085B
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grinding
zirconium silicate
mill
ball
zircon sand
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CN101722085A (en
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许兴康
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Abstract

The invention provides a grinding technology of high purity sub-nano level superfine zirconium silicate powder, which comprises the following steps: first adopting wet process ball-milling method and selecting homogenous silicic acid zirconium balls with a diameter ranging from phi 10mm to phi 15mm as grinding balls, grinding zircon sand to have a diameter of 3-5 mum; then selecting homogenous silicic acid zirconium balls with a diameter ranging from phi 1mm to phi 3mm as grinding balls; grinding the zircon sand twice in a stirring mill at a rotating speed standing at 100-300rmp and grinding the zircon sand to have a diameter ranging from 0.8mum to 1.0mum; then selecting homogenous silicic acid zirconium balls with a diameter ranging from phi 0.5mm to phi 1mm as grinding balls and grinding the zircon sand twice in a stirring mill at a rotating speed standing at 100-300rmp and grinding the zircon sand to have a diameter ranging from 0.45mum to 0.55mum.The grinding efficiency is relatively high, product energy consumption is low, and use level of the obtained high purity sub-nano level superfine zirconium silicate powder is reduced by 20-40% compared with the use level of ordinary pulverulent bodies of the same type, thus deserving promotion in the industry.

Description

The grinding technics of high purity sub-nano level superfine zirconium silicate powder
Technical field
The present invention relates to the ultra-fine wet grinding method of high hardness mineral material, relate in particular to a kind of grinding technics of high purity sub-nano level superfine zirconium silicate powder.
Background technology
Superfine zirconium silicate powder is widely used in building, sanitary ceramics industry, plays milkiness and base substrate whitening effect.The equal import of the high-grade raw materials used zircon sand of superfine zirconium silicate powder, domestic exploitation zircon sand does not all become scale, and recovery process is very big to environmental disruption, and country is to the also strict restriction of the exploitation of zircon sand; And because zircon sand and radioactive substance such as thorium, uranium symbiosis on a small quantity exceed standard the radioactive indicator of zircon sand through regular meeting.So satisfying under the ceramic industry instructions for use prerequisite, reduce use amount, will make ceramic product more green, environmental protection.
The grinding technics of zirconium silicate powder mainly contains at present:
1. the traditional wet ball-milling technology is made mill ball with alumina balls or cobblestone, and specification is generally Φ 8-13mm, and device therefor is common ball mill at a slow speed, and rotating speed is generally 10-20 rev/min, and one is ground to the end until reaching the requirement fineness.This technology General Spherical time consuming is 50-70 hour, and the fineness of zirconium silicate powder product can reach 1.4-1.6 μ.As rethink and improve product fineness then milling time will be above more than 100 hours, and fineness improves limitedly, causes that slurry temperature rises to 100 ℃ in the ball mill, will greatly damage grinding machine, causes in the grinding machine pottery to serve as a contrast and comes off, energy consumption is high.And to cause in the products obtained therefrom oxidation of impurities aluminium to be sneaked into many because of alumina balls wear rate height, product ZrO 2Content drops to 60-63%.
2. dry pulverization process, micro-powder graded technology can be saved dry materials workshop section, but can't be milled to very low fineness, have only through classification, and meal returns mill and reaches the requirement fineness.But cause efficient low, classification is not thorough.In addition, because of zircon sand hardness is high, to the equipment part well damage, replacing, maintenance cost costliness.
3. adopt steel ball to carry out wet ball grinding as mill ball, sour again blanking iron, grinding efficiency is high, and material is levigate easily, but environmental pollution is serious.
4. wet ball grinding, wet classification technology to certain fineness, propose with the wet classification machine zircon sand wet ball grinding with the classification of fine powder slurry, meal slurry recirculation ball milling, so repeatedly.When powdery pulp is milled to 2 μ m when following, the grader classification efficiency is extremely low, and classification misses by a mile; During the slurry classification, must reduce slurry viscosity greatly, increase moisture content and could effectively reach the classification purpose, but after solid content significantly reduced, the coarse particles that needs back to grind was also wanted thickening, greatly influences production efficiency.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of grinding technics of high purity sub-nano level superfine zirconium silicate powder is provided.
The object of the invention is realized through following technical scheme:
The grinding technics of high purity sub-nano level superfine zirconium silicate powder (remarks: zircon sand is exactly a zirconium silicate powder after grinding) may further comprise the steps---
1. roughly grind: adopt the wet ball grinding method, select for use Φ 10~Φ 15mm homogeneity zirconium silicate ball to make abrading-ball, zircon sand is milled to 3~5 μ m;
2. mill in: select for use the homogeneity zirconium silicate ball of Φ 1~3mm to make abrading-ball, in the stirring mill of rotating speed 100~300rpm, above-mentioned zircon sand is carried out twice grinding, be ground to 0.8~1.0 μ m;
3. ultra-fine mill: select for use the homogeneity zirconium silicate ball of Φ 0.5~1mm to make abrading-ball, in the stirring mill of rotating speed 500~1000rpm, above-mentioned zircon sand is carried out twice grinding again, be ground to 0.45~0.55 μ m.
Further, the grinding technics of above-mentioned high purity sub-nano level superfine zirconium silicate powder all adds composite polyacrylic acid dipersant in the process of corase grind, middle mill, ultra-fine mill.
Further, the grinding technics of above-mentioned high purity sub-nano level superfine zirconium silicate powder, the addition of composite polyacrylic acid dipersant is 0.5% in said corase grind, middle mill, each process of ultra-fine mill.
Substantive distinguishing features and obvious improvement that technical scheme of the present invention is outstanding are mainly reflected in:
1. carry out carse, medium and small mill respectively, greatly improve grinding efficiency, product energy consumption is significantly reduced;
2. all grinding stages all adopt homogeneity zirconium silicate ball to make abrading-ball, and cost is not high, guarantee that impurity is sneaked into few in the process of lapping;
3. adopt composite polypropylene hydrochlorate to make dispersant, prevent particle agglomeration, improve wet-milling material solid content, effectively improve grinding efficiency, reduce energy consumption for drying;
4. this product can reduce by 20~40% use amounts in the ceramic industry use amount than similar meal product (survey at same granularity instrument: imported product is 1.2~1.3 μ m, and homemade goods is 1.5~1.8 μ m).
The specific embodiment:
The grinding technics of high purity sub-nano level superfine zirconium silicate powder of the present invention is made first section corase grind with traditional ball mill and homogeneity zirconium silicate ball, is milled to fineness 2~3 μ m; (rotating speed 100~300rpm) stirs mill in the mill work, through second and third section material is milled to 0.8~1.0 μ m with middling speed; With (rotating speed 500~1000rpm) stirs mill and makes ultra-fine mill, through fourth, fifth section material is milled to 0.45~0.55 μ m fast.
Its corase grind adopts big specification (Φ 10~Φ 15) homogeneity zirconium silicate ball, in traditional ball mill, zircon sand is milled to 3~5 μ m; First section is adopted large ball games, mainly plays pulverization.Different sphere diameter zirconium silicate pearls are then adopted in middle mill, fine grinding, in the different rotating speeds grinding machine, carry out respectively, play best grinding effect.In each process of lapping, add composite polyacrylic acid dipersant (amount is about 0.5%), prevent particle agglomeration, improve wet-milling material solid content, effectively improve grinding efficiency, reduce energy consumption for drying.
Embodiment 1
With zircon, Φ 10~Φ 15mm zirconium silicate ball, water, in the ratio of the 1:2.5:0.8 corundum lining ball mill of packing into.Roughly ground 12~15 hours, and made its fineness reach 3~5 μ m, slurry is emitted.
In the 1000L grinder that Φ 2~3mm zirconium silicate pearl is housed, (rotating speed 100~300rpm), fineness reach 1.5~2.0 μ m to carry out once middle mill.
In the 1000L grinder that Φ 1~2mm zirconium silicate pearl is housed, (fineness reaches 0.8~1.0 μ m for rotating speed 100~300rpm), middling speed rotating speed 100~300rpm to carry out in the secondary mill.
In the 1000L grinder that Φ 0.8~1.0mm zirconium silicate pearl is housed, (rotating speed 500~1000rpm), fineness reach 0.6~0.7 μ m to carry out once ultra-fine mill.
In the 1000L grinder that Φ 0.5~0.8mm zirconium silicate pearl is housed, (rotating speed 500~1000rpm), fineness reach 0.45~0.55 μ m to carry out the ultra-fine mill of secondary.
All add composite polyacrylic acid dipersant in above-mentioned each process of lapping.
At last, levigate slurry spray-drying is made fine powder, pack get product (high purity sub-nano level superfine zirconium silicate powder).
Embodiment 2
With zircon, Φ 10~Φ 15mm zirconium silicate ball, water, in the ratio of the 1:2.5:1.0 corundum lining ball mill of packing into.Roughly ground 10~12 hours, and made its fineness reach 3~5 μ m, slurry is emitted.
In the 1000L grinder that Φ 2~3mm zirconium silicate pearl is housed, (rotating speed 100~300rpm), fineness reach 1.5~2.0 μ m to carry out once middle mill.
In the 1000L grinder that Φ 1~2mm zirconium silicate pearl is housed, (rotating speed 100~300rpm), fineness reach 0.8~1.0 μ m to carry out in the secondary mill.
In the 1000L grinder that Φ 0.8~1.0mm zirconium silicate pearl is housed, (rotating speed 500~1000rpm), fineness reach 0.6~0.7 μ m to carry out once ultra-fine mill.
In the 1000L grinder that Φ 0.5~0.8mm zirconium silicate pearl is housed, (rotating speed 500~1000rpm), fineness reach 0.45~0.55 μ m to carry out the ultra-fine mill of secondary.
All add composite polyacrylic acid dipersant (amount is 0.5%) in above-mentioned each process of lapping.
At last, levigate slurry spray-drying is made fine powder, pack get product (high purity sub-nano level superfine zirconium silicate powder).
Embodiment 3
With zircon, Φ 10~Φ 15mm zirconium silicate ball, water, in the ratio of the 1:2:0.8 corundum lining ball mill of packing into.Roughly ground 12~14 hours, and made its fineness reach 3~5 μ m, slurry is emitted.
In the 1000L grinder that Φ 2~3mm zirconium silicate pearl is housed, carry out once middle mill, fineness reaches 1.5~2.0 μ m.
In the 1000L grinder that Φ 1~2mm zirconium silicate pearl is housed, to carry out grinding in the secondary, fineness reaches 0.8~1.0 μ m.
In the 1000L grinder that Φ 0.8~1.0mm zirconium silicate pearl is housed, carry out once ultra-fine mill, fineness reaches 0.6~0.7 μ m.
In the 1000L grinder that Φ 0.5~0.8mm zirconium silicate pearl is housed, carry out the ultra-fine mill of secondary, fineness reaches 0.45~0.55 μ m.
All add composite polyacrylic acid dipersant in above-mentioned each process of lapping.
At last, levigate slurry spray-drying is made fine powder, pack get product (high purity sub-nano level superfine zirconium silicate powder).
Technical scheme of the present invention is carried out carse, medium and small mill respectively, greatly improves grinding efficiency, and product energy consumption is significantly reduced; All grinding stages all adopt homogeneity zirconium silicate ball to make abrading-ball, and cost is not high, guarantee that impurity is sneaked into few in the process of lapping; Adopt composite polypropylene hydrochlorate to make dispersant, prevent particle agglomeration, improve wet-milling material solid content, effectively improve grinding efficiency, reduce energy consumption for drying; This product can reduce by 20~40% use amounts in the ceramic industry use amount than similar meal product (survey at same granularity instrument: imported product is 1.2~1.3 μ m, and homemade goods is 1.5~1.8 μ m), and prospect is very good.
Below only be concrete exemplary applications of the present invention, protection scope of the present invention is not constituted any limitation.All employing equivalents or equivalence are replaced and the technical scheme of formation, all drop within the rights protection scope of the present invention.

Claims (2)

1. the grinding technics of high purity sub-nano level superfine zirconium silicate powder is characterized in that: may further comprise the steps---
1. roughly grind: adopt the wet ball grinding method, select for use Φ 10~Φ 15mm homogeneity zirconium silicate ball to make abrading-ball, zircon sand is milled to 3~5 μ m; In pass, add composite polyacrylic acid dipersant;
2. mill in: select for use the homogeneity zirconium silicate ball of Φ 1~3mm to make abrading-ball, in the stirring mill of rotating speed 100~300rpm, above-mentioned zircon sand is carried out twice grinding, be ground to 0.8~1.0 μ m; In middle mill process, add composite polyacrylic acid dipersant;
3. ultra-fine mill: select for use the homogeneity zirconium silicate ball of Φ 0.5~1mm to make abrading-ball, in the stirring mill of rotating speed 500~1000rpm, above-mentioned zircon sand is carried out twice grinding again, be ground to 0.45~0.55 μ m; In the process of ultra-fine mill, add composite polyacrylic acid dipersant.
2. the grinding technics of high purity sub-nano level superfine zirconium silicate powder according to claim 1, it is characterized in that: the addition of composite polyacrylic acid dipersant is 0.5% in said corase grind, middle mill, each process of ultra-fine mill.
CN2008101955048A 2008-10-15 2008-10-15 Grinding technology of high purity sub-nano level superfine zirconium silicate powder Expired - Fee Related CN101722085B (en)

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CN102442838A (en) * 2011-08-28 2012-05-09 内蒙古科技大学 Preparation method of superfine zirconium silicate powder
CN102765729B (en) * 2012-08-22 2014-05-28 山东神州锆业有限公司 Method for homogenizing super-fine powder of zirconium silicate
CN103170393B (en) * 2012-12-28 2015-04-29 北京新航建材集团有限公司 Preparation method of superfine slag powder
CN103316742B (en) * 2013-05-31 2015-04-08 尚越光电科技有限公司 High-energy vibration ball milling technology for binary selenide nano-powder
CN104353521A (en) * 2014-08-14 2015-02-18 佛山市阳光陶瓷有限公司 Ball-milling process for superfine ceramic powder
CN104475213A (en) * 2014-11-10 2015-04-01 张藜泷 Method for preparing ultra-fine Hetian jade powder
CN104609868B (en) * 2015-01-13 2016-06-15 江苏金石研磨有限公司 A kind of zirconium silicate-based composite ceramics raw material dispersant for wet grinding and preparation method thereof
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CN109133893A (en) * 2018-10-31 2019-01-04 江苏脒诺甫纳米材料有限公司 A method of preparing superfine zirconium silicate
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