CN104150883B - A kind of preparation method of aluminum oxide pelletizing - Google Patents

A kind of preparation method of aluminum oxide pelletizing Download PDF

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CN104150883B
CN104150883B CN201410308502.0A CN201410308502A CN104150883B CN 104150883 B CN104150883 B CN 104150883B CN 201410308502 A CN201410308502 A CN 201410308502A CN 104150883 B CN104150883 B CN 104150883B
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pelletizing
aluminum oxide
powder
preparation
ball
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CN104150883A (en
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赵友谊
曾华生
王�琦
王晋槐
宋友杰
马晓兵
刘菲菲
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JINGANG NEW MATERIALS CO Ltd
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Abstract

The invention discloses a kind of preparation method of aluminum oxide pelletizing, belong to ceramic technology field.The method adopts preferably special aluminum oxide powder to be main raw material, adopts unique ball-milling technology to control mud grain size distribution; Adopt composite additive in use can arrive the effect of similar dry grinding pelletizing (micro mist) by the particulate state pelletizing that surface modification pelletizing reaches wet spray.The aluminum oxide pelletizing of preparation is applicable to each producer hot die-casting molding equipment in the market, and the Product Precision fired is high, indeformable, polishing effect is good.

Description

A kind of preparation method of aluminum oxide pelletizing
Technical field
The present invention relates to a kind of aluminum oxide pelletizing and preparation method thereof, belong to ceramic technology field.
Background technology
Alumina-ceramic physical strength is high, hardness is large, corrosion-resistant, and raw material sources are wide, low price is widely used in fields such as filler, grinding medium, wear-resistant liner, corrosion-resistant finishess.
Aluminum oxide pelletizing is an industry of extending along with the development of alumina-ceramic industry, and its market demand is very huge.Except for except alumina-ceramic, be also applicable to high-grade sealing member, electron trade, textile industry, military industry, Abrasive Industry etc.Wherein for the molded aluminum oxide pelletizing market demand of Rapid dry at about 50000 tons/year.And manufacturer is more scattered, output is little, industry standard disunity.
At present centrifugal or press spray drying process is mainly adopted to obtain for the aluminum oxide pelletizing that Rapid dry is molded.In use there is following problem in aluminum oxide pelletizing obtained like this: full particle prepared by centrifugal granulating tower is too thin, molded for Rapid dry, and easily produce cracking, demixing phenomenon, reclaimed materials causes pelletizing qualification rate too low too much simultaneously; And adopt pelletizing prepared by pressure type drying tower, having certain hollow bead exists, and causes produced alumina article to there will be pin hole in later stage polishing process.
The pelletizing being applicable to 20 times/min Rapid dry press forming device is different from common pelletizing, its pelletizing be necessary for spherical, full particle, unit weight are large, grain composition is suitable, so that because pelletizing good fluidity, tap density are large in Rapid Prototyping Process, clearance air is few and shaping smoothly, facilitates later stage retrofit, polishing yield rate.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, provide a kind of dry-pressing aluminum oxide pelletizing and preparation method thereof fast.
Principal feature of the present invention adopts special raw material and formula system for relying on, and adopts constant temperature ball-milling technology to improve grinding efficiency and Control granularity grating; Centrifugal-drying plant combined of spraying is adopted to reach control pelletizing pattern and grain composition object.The aluminum oxide pelletizing of preparation is applicable to 20 times/min Rapid dry press forming device in the market, and the product fired is easy to the complete processings such as polishing.
Technical scheme of the present invention is as follows:
A preparation method for aluminum oxide pelletizing, is characterized in that,
(1) raw material and weight part
Major ingredient: aluminum oxide powder 80-92 part, kaolin 3-15 part;
Complex sintering aids: magnesium oxide 0.5-5 part, calcium carbonate 0.5-5 part, silicon powder 0.5-5 part;
(2) put into intermittent ball mill constant temperature ball milling together with after aluminum oxide powder, kaolin, silicon powder being weighed respectively with complex sintering aids, qualified rear mistake 180 mesh sieve of fineness, obtains ceramic mud after electromagnetism deironing;
(3), after adopting surge pump to squeeze into and stir half an hour in transferring cylinder step (2) ceramic mud, add 1-5% composite additive, carry out strong stirring;
(4) the mist projection granulating tower that ceramic mud step (3) obtained adopts centrifugal-pressure to combine is dried to ceramic prilling powder, crosses 40 mesh sieves and removes the larger agglomerating particles that on tower wall, caking is formed;
(5) ceramic prilling powder step (4) obtained is by after feed bin homogenizing, and pelletizing is mixed 0.3-1 ‰ releasing agent in blender, is packaged to be a kind of dry-pressing aluminum oxide pelletizing fast.
Above-mentioned steps (5) is main to be loaded feed bin and adds micro-releasing agent by pelletizing.The object of feeding warehouse carries out batch pelletizing homogenizing and old; The releasing agent object of mixed trace is that less friction improves alloy mold access times.
Preferably, the preparation method of described aluminum oxide powder is: by moisture be 2-3% aluminium hydroxide and industrial alumina powder in high temperature rotary kiln 1380-1400 DEG C fire and form;
Described moisture is the weight ratio of 2-3% aluminium hydroxide and industrial alumina powder is 1:3.
Above-mentioned aluminum oxide powder has larger activity, detects former footpath centralized particle diameter, about D90=5 μm after ball milling, and aluminium powder remains without mineralizer.The AL-Si-Mg-Ca quaternary formula system adopted, adopts pure solid state sintering, ensure that intensity and the toughness of product, facilitates later stage polishing to use.
Preferably, in described step (2), when adopting intermittent ball mill ball milling, alumina balls masonry is adopted to be grinding medium, material: ball: water=1:2-3:1; Ball mill physical dimension 3000*4500mm, rotating speed 13r/min, Ball-milling Time 25-35 hour, slurry fineness D90 < 7 μm, slurry water sub-control is built in 35-55%.
Described ball-milling technology is: add 60-70 DEG C of hot water in early stage and directly to score grinding machine, at ball milling after two hours, opens ball milling cover and pass into hot steam second-heating to 70-80 DEG C, until ball milling terminates after formulation material and water form mud.Best, the easy ball milling of material of slip fluidity at high operating temperatures, improves grinding efficiency clearly.
Preferably, described in described step (3), composite additive is water-soluble polyvinyl alcohol: dispersion agent: starch=3:1:1.
Preferably, the rotating speed of the strong stirring described in described step (3) is 60 turns/min.
Ceramic mud carries out strong stirring (reaching 60 turns/min) and adds composite additive (water-soluble polyvinyl alcohol: dispersion agent: starch=3:1:1) after half an hour in transferring cylinder, directly adds dispersion agent and polyvinyl alcohol and avoid and cause dispersion agent, polyvinyl alcohol and starch to lose efficacy at ball mill ball milling and high temperature in transferring cylinder.Stir formation circulation whirlpool fast and reach the object mixing, prevent mud sediment and froth breaking, do not add the additive such as glycerine, emulsifying wax at needs.
Preferably, described in described step (4) centrifugal-mist projection granulating tower that pressure combines is: increased by the cylindrical shell of atomizer tower, 1/3 place's setting pressure formula spray gun below cylindrical shell, spray tower is equipped with and two overlaps independently pulp feeding system; Described centrifugal-processing condition of mist projection granulating tower that pressure combines are: spray gun pressure is 2-3MPa, adopts aperture 1.8mm to spray sheet; Centrifugal rotational speed 2000 turns/min; Spray tower temperature suitable for reading controls at 350-380 DEG C, and end opening temperature controls at 80-100 DEG C, and powder moisture controlled is at 0.5-5%.
Adopt pelletizing medium particle diameter that transformed mist projection granulating tower is collected about 140 orders, slurry is fully removed moisture in the process of cylindrical shell inner drying through the hot blast stirred and mixes, wherein centrifugal pellet is thinner full particle, be equipped with the pressure coarse particles of trace, only needed 40 mesh sieves to remove sticky wall caking, minus mesh is all qualified pelletizing.By regulating Spray Gun Of The Pressure or centrifugal atomizing dish stock volume, adjustment pelletizing pattern, solid degree and grain composition, fundamentally solve centrifugal or pressure-type spray tower granulation separately and produce shaping, product later stage polishing problem.
Step of the present invention (5) is main to be loaded feed bin and adds micro-releasing agent by pelletizing.The object of feeding warehouse carries out batch pelletizing homogenizing and old; The releasing agent object of mixed trace is that less friction improves alloy mold access times.
Preferably, described releasing agent is hard magnesium and calcium stearate mixture.
Preferably, the weight ratio of described hard magnesium and calcium stearate is 1:2.
The present invention compared with prior art, has following outstanding feature:
(1) the present invention with the raw material of mixing when without being fired into noresidue mineralizer, oxide of high activity aluminium powder when mineralizer for main raw material in rotary kiln, adopt quaternary formula system and solid-phase sintering process, product has higher-strength and toughness, and in later stage polishing etc., the deep processing stage not easily collapses limit, yield rate is high, wear-resisting and sealing property is better.
(2) the present invention adopts the constant temperature ball-milling technology of original creation to be add hot water in early stage directly to score grinding machine, at ball milling after two hours, formulation material and water are formed after mud opens ball milling cover and pass into hot steam second-heating, until slurry keeps continuous high temperature in last blowing ball mill, best, the easy ball milling of material of slip fluidity at high operating temperatures, improves grinding efficiency clearly.
(3) the present invention adds various composite additive in transferring cylinder, the object mixing, prevent mud sediment and froth breaking is reached by strong stirring, avoid various additive to lose efficacy after ball milling in ball mill, finally less or can not add some additive and reach obvious effect.
(4) the present invention adopts originality thinking to carry out the combination transformation of pressure and Centrafugal spray drying tower, thus by many kinds of parameters regulation and control pelletizing exterior appearance and pelletizing performance, fundamentally solve centrifugal or pressure-type spray tower granulation separately and produce shaping, product later stage polishing problem.Do not need the powder of below removal 200 order to improve powder qualification rate, spherical, determine that it has better mobility without the granule-morphology of adhesion, applicable Rapid dry is molded, and later stage polishing there will not be needle pore defect.
(5) features such as it is high that the aluminum oxide pelletizing that the present invention produces has yield rate, and granule-morphology is good, and applicable Rapid dry is molded; The product fired shrinks easy to control, and post-production is not turned black, do not collapse limit, yield rate high.
Accompanying drawing explanation
Fig. 1 process flow sheet of the present invention.
Embodiment
Embodiment is only described further the present invention, but is not limited only to this, and those skilled in the art obtains other embodiments under the prerequisite not paying creative work, all belongs to the scope of protection of the invention.
Aluminum oxide powder fires form by be 2-3% aluminium hydroxide and industrial alumina powder at moisture to be blended in high temperature rotary kiln 1380-1400 DEG C with 1:3 ratio.Its aluminum oxide powder has larger activity, detects former footpath centralized particle diameter, about D90=5 μm after ball milling, and aluminium powder remains without mineralizer.The chemical composition of other raw materials sees the above table 1.Adopt the high quality raw material that the alkali metal content of high-quality is few.
The chemical constitution of other raw materials of table 1 and weight part
Embodiment 1:
(1) raw material and weight part
Major ingredient: aluminum oxide powder 92 parts, kaolin 3 parts;
Complex sintering aids: 3 parts, magnesium oxide, 1 part, calcium carbonate, silicon powder 1 part;
(2) putting into intermittent ball mill constant temperature ball milling together with after aluminum oxide powder, kaolin, silicon powder being weighed respectively with complex sintering aids (adopts alumina balls masonry to be grinding medium, material: ball: water=1:2.3:1), qualified rear mistake 180 mesh sieve of fineness, ceramic mud is obtained after electromagnetism deironing, ball mill physical dimension 3000*4500mm, rotating speed 13r/min, Ball-milling Time 25 hours, slurry fineness D90 < 6.8 μm; Add 60 DEG C of hot water in early stage directly to score grinding machine, at ball milling after two hours, after formulation material and water form mud, pass into hot steam second-heating to 70 DEG C, until slurry keeps continuous high temperature in last blowing ball mill.
(3), after adopting surge pump to squeeze into and stir half an hour in transferring cylinder step (2) ceramic mud, add 1% composite additive (water-soluble polyvinyl alcohol: dispersion agent=3:1), carry out strong stirring.
(4) the mist projection granulating tower that ceramic mud step (3) obtained adopts centrifugal-pressure to combine is dried to ceramic prilling powder, crosses on 40 mesh sieves removal tower walls and lumps.Its technique is: spray gun pressure is 2MPa, adopts aperture 1.8mm to spray sheet; Centrifugal rotational speed 2000 turns/min; Spray tower temperature suitable for reading controls at 350 DEG C, and end opening temperature controls at 80 DEG C, and powder moisture controlled is 5%.
(5) ceramic prilling powder step (4) obtained is by after feed bin homogenizing, and mixed 0.3 ‰ releasing agents (weight ratio of hard magnesium and calcium stearate is 1:2) are packaged to be a kind of dry-pressing aluminum oxide pelletizing fast.
Product performance detect and see the following form 2.
Embodiment 2:
(1) raw material and weight part
Major ingredient: aluminum oxide powder 90 parts, kaolin 3 parts;
Complex sintering aids: 3 parts, magnesium oxide, 2 parts, calcium carbonate, silicon powder 2 parts;
(2) putting into intermittent ball mill constant temperature ball milling together with after aluminum oxide powder, kaolin, silicon powder being weighed respectively with complex sintering aids (adopts alumina balls masonry to be grinding medium, material: ball: water=1:2.6:1), qualified rear mistake 180 mesh sieve of fineness, ceramic mud is obtained after electromagnetism deironing, ball mill physical dimension 3000*4500mm, rotating speed 13r/min, Ball-milling Time 26 hours, slurry fineness D90 < 6.5 μm; Add 70 DEG C of hot water in early stage directly to score grinding machine, at ball milling after two hours, after formulation material and water form mud, pass into hot steam second-heating to 72 DEG C, until slurry keeps continuous high temperature in last blowing ball mill.
(3), after adopting surge pump to squeeze into and stir half an hour in transferring cylinder step (2) ceramic mud, add 2% composite additive (water-soluble polyvinyl alcohol: dispersion agent=3:1), carry out strong stirring.
(4) the mist projection granulating tower that ceramic mud step (3) obtained adopts centrifugal-pressure to combine is dried to ceramic prilling powder, crosses on 40 mesh sieves removal tower walls and lumps.Its technique is: spray gun pressure is 2.2MPa, adopts aperture 1.8mm to spray sheet; Centrifugal rotational speed 2000 turns/min; Spray tower temperature suitable for reading controls at 370 DEG C, and end opening temperature controls at 95 DEG C, and powder moisture controlled is 0.5%.
(5) ceramic prilling powder step (4) obtained is by after feed bin homogenizing, and mixed 0.8 ‰ releasing agents (weight ratio of hard magnesium and calcium stearate is 1:2) are packaged to be a kind of dry-pressing aluminum oxide pelletizing fast.
Product performance detect and see the following form 2.
Embodiment 3:
(1) raw material and weight part
Major ingredient: aluminum oxide powder 85 parts, kaolin 8 parts;
Complex sintering aids: 1 part, magnesium oxide, 3 parts, calcium carbonate, silicon powder 3 parts;
(2) putting into intermittent ball mill constant temperature ball milling together with after aluminum oxide powder, kaolin, silicon powder being weighed respectively with complex sintering aids (adopts alumina balls masonry to be grinding medium, material: ball: water=1:2.9:1), qualified rear mistake 180 mesh sieve of fineness, ceramic mud is obtained after electromagnetism deironing, ball mill physical dimension 3000*4500mm, rotating speed 13r/min, Ball-milling Time 26 hours, slurry fineness D90 < 6.5 μm; Add 65 DEG C of hot water in early stage directly to score grinding machine, at ball milling after two hours, after formulation material and water form mud, pass into hot steam second-heating to 80 DEG C, until slurry keeps continuous high temperature in last blowing ball mill.
(3), after adopting surge pump to squeeze into and stir half an hour in transferring cylinder step (2) ceramic mud, add 3.2% composite additive (water-soluble polyvinyl alcohol: dispersion agent=3:1), carry out strong stirring.
(4) the mist projection granulating tower that ceramic mud step (3) obtained adopts centrifugal-pressure to combine is dried to ceramic prilling powder, crosses on 40 mesh sieves removal tower walls and lumps.Its technique is: spray gun pressure is 3MPa, adopts aperture 1.8mm to spray sheet; Centrifugal rotational speed 2000 turns/min; Spray tower temperature suitable for reading controls at 368 DEG C, and end opening temperature controls at 95 DEG C, and powder moisture controlled is 1.2%.
(5) ceramic prilling powder step (4) obtained is by after feed bin homogenizing, and mixed 0.8 ‰ releasing agents (weight ratio of hard magnesium and calcium stearate is 1:2) are packaged to be a kind of dry-pressing aluminum oxide pelletizing fast.
Product performance detect and see the following form 2.
In table 2 embodiment 1-3, product performance detect data
Pelletizing unit weight Molding effect Become porcelain density g/cm 3 Contraction ratio Polishing effect
Embodiment 1 1.16 Without cracking, layering 3.73 1.16 Without stain, do not collapse limit
Embodiment 2 1.20 Without cracking, layering 3.68 1.16 Without stain, do not collapse limit
Embodiment 3 1.18 Without cracking, layering 3.60 1.16 Without stain, do not collapse limit

Claims (5)

1. a preparation method for aluminum oxide pelletizing, is characterized in that,
(1) raw material and weight part
Major ingredient: aluminum oxide powder 80-92 part, kaolin 3-15 part;
Complex sintering aids: magnesium oxide 0.5-5 part, calcium carbonate 0.5-5 part, silicon powder 0.5-5 part;
(2) put into intermittent ball mill constant temperature ball milling after aluminum oxide powder, kaolin, complex sintering aids being weighed respectively together, qualified rear mistake 180 mesh sieve of fineness, obtains ceramic mud after electromagnetism deironing;
Described ball-milling technology is: add 60-70 DEG C of hot water in early stage and directly to score grinding machine, at ball milling after two hours, opens ball milling cover and pass into hot steam second-heating to 70-80 DEG C, until ball milling terminates after formulation material and water form mud;
(3), after adopting surge pump to squeeze into and stir half an hour in transferring cylinder step (2) ceramic mud, add 1-5% composite additive, carry out strong stirring;
(4) the mist projection granulating tower that ceramic mud step (3) obtained adopts centrifugal-pressure to combine is dried to ceramic prilling powder, crosses 40 mesh sieves and removes the larger agglomerating particles that on tower wall, caking is formed;
(5) ceramic prilling powder step (4) obtained is by after feed bin homogenizing, and pelletizing is mixed 0.3-1 ‰ releasing agent in blender, is packaged to be a kind of dry-pressing aluminum oxide pelletizing fast;
The preparation method of aluminum oxide powder is: by moisture be 2-3% aluminium hydroxide and industrial alumina powder in high temperature rotary kiln 1380-1400 DEG C fire and form;
Moisture is the weight ratio of 2-3% aluminium hydroxide and industrial alumina powder is 1:3;
Described in step (3), composite additive is water-soluble polyvinyl alcohol: dispersion agent: starch=3:1:1;
Described in step (4) centrifugal-mist projection granulating tower that pressure combines is: increased by the cylindrical shell of atomizer tower, 1/3 place's setting pressure formula spray gun below cylindrical shell, spray tower is equipped with and two overlaps independently pulp feeding system; Described centrifugal-processing condition of mist projection granulating tower that pressure combines are: spray gun pressure is 2-3MPa, adopts aperture 1.8mm to spray sheet; Centrifugal rotational speed 2000 turns/min; Spray tower temperature suitable for reading controls at 350-380 DEG C, and end opening temperature controls at 80-100 DEG C, and powder moisture controlled is at 0.5-5%.
2. preparation method according to claim 1, is characterized in that, in described step (2), when adopting intermittent ball mill ball milling, adopts alumina balls masonry to be grinding medium, material: ball: water=1:2-3:1; Ball mill physical dimension 3000*4500mm, rotating speed 13r/min, Ball-milling Time 25-35 hour, slurry fineness D90 < 7 μm, slurry water sub-control is built in 35-55%.
3. preparation method according to claim 1, is characterized in that, the rotating speed of the strong stirring described in described step (3) is 60 turns/min.
4. preparation method according to claim 1, is characterized in that, described releasing agent is hard magnesium and calcium stearate mixture.
5. preparation method according to claim 4, is characterized in that, the weight ratio of described hard magnesium and calcium stearate is 1:2.
CN201410308502.0A 2014-06-30 2014-06-30 A kind of preparation method of aluminum oxide pelletizing Active CN104150883B (en)

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