CN1382658A - With gamma-AL2O3Process for producing sintered tabular corundum from raw material - Google Patents
With gamma-AL2O3Process for producing sintered tabular corundum from raw material Download PDFInfo
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- CN1382658A CN1382658A CN 02113098 CN02113098A CN1382658A CN 1382658 A CN1382658 A CN 1382658A CN 02113098 CN02113098 CN 02113098 CN 02113098 A CN02113098 A CN 02113098A CN 1382658 A CN1382658 A CN 1382658A
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- Prior art keywords
- raw material
- sintering
- described technology
- add
- gamma
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- 239000002994 raw material Substances 0.000 title claims abstract description 18
- 229910052593 corundum Inorganic materials 0.000 title claims abstract description 10
- 239000010431 corundum Substances 0.000 title claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000012856 packing Methods 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000005516 engineering process Methods 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 229910016569 AlF 3 Inorganic materials 0.000 claims description 5
- 238000013467 fragmentation Methods 0.000 claims description 5
- 238000006062 fragmentation reaction Methods 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 5
- 239000011822 basic refractory Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 229910000272 alkali metal oxide Inorganic materials 0.000 abstract description 2
- 230000003628 erosive effect Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000035939 shock Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 abstract 1
- 239000002585 base Substances 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 239000004902 Softening Agent Substances 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008398 formation water Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000001778 solid-state sintering Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 206010020843 Hyperthermia Diseases 0.000 description 1
- 235000019013 Viburnum opulus Nutrition 0.000 description 1
- 244000071378 Viburnum opulus Species 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036031 hyperthermia Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a preparation process of a basic refractory raw material, which is prepared from gamma-Al2O3Producing sintered plate-shaped corundum as raw material. Comprises the following process steps of selecting gamma-Al as the raw material2O3Adding additive into main material, adding water, grinding, press filtering, dewatering, vacuum extruding, baking, high-temp sintering, crushing, sieving, removing iron and packing. The prepared product has high particle strength, good grain boundary bonding, less intercrystalline pores, uniform distribution, high product density, good wear resistance and erosion resistance, and low content of alkali metal oxide<0.2 percent, even crystal size, extremely few abnormally grown crystal grains and good thermal shock property.
Description
Affiliated field
The present invention relates to a kind of preparation technology of basic refractory raw material.
Background technology
Sintering plate corundum is a kind of high-purity sintering refractory raw material, is widely used in industries such as metallurgy, pottery, chemical industry, glass, is the metallurgical industry slide plate, the basic refractory raw material of refractory products such as submerged nozzle, casting house amorphous refractory, blast furnace lining.
Domestic certain factory once used two-step process, promptly earlier with γ-Al
2O
3Calcining is converted into α-Al
2O
3, then with α-Al
2O
3In small, broken bits, balling-up, burn till, produce sintering plate corundum, finally too high and be difficult to development and promote with production cost.
The step of external production technique is:
Gamma-alumina, mineralizer → ball milling → balling-up (similar snowball) → drying → sintering → pick (underburnt, burning) → fragmentation, screening, deironing → check → packing.
There is defective:
What (1) processing of raw material was adopted is the ball milling dry process, and the distribution of various raw materials and grain diameter homogeneity are undesirable in the batching.
(2) nodulizer is used in the work in-process moulding, and power consumption is big, the noise height, and green strength and density are low, and easily broken in the transportation, easily stop up kiln during sintering.
(3) burn till employing shaft furnace, firing temperature at 1815--1925 ℃, material to kiln requires high, owing to adopt in conjunction with balling technique, ball base intensity is not high, and is easily broken in the sintering process, easily makes kiln inwall ring formation, it is the major cause that causes frequent obstruction kiln, so it is difficult to burn till control, fault is got rid of difficult, the maintenance cost height.
(4) because of adopting ultrahigh-temperature to burn till fast, base substrate is short at kiln residence time, so the crystal development of product is undesirable, the crystalline size size differs greatly, and it is more that unusual grown crystal reaches 400--600 μ m intergranular pore, and it is very inhomogeneous to distribute.Therefore its granule strength of sintering plate corundum of this kind explained hereafter is not high, and corrosion-resistant property is not in perfect condition.
Technical scheme
The object of the invention is to invent that a kind of technology is simple, yield is high, cost is low with γ-Al
2O
3The processing method of directly synthesizing sintering plate corundum for starting material.
The present invention includes following steps:
A, batching are selected γ-Al for use
2O
3Be main raw material, add additive, additive is MgO, AlF
3At least a
B, add the entry extra-fine grinding
C, filter-press dehydration
D, vacuum extrusion base
E, oven dry
F, high temperature sintering
G, fragmentation, screening, deironing
H, packing.
Superiority of the present invention is embodied in:
1, adopt wet grinding: the main raw material of sintering plate corundum is a commercial alumina, with regard to its internal crystal structure, it is by many porous spherical aggregates of forming less than the small crystal of 0.1 μ m, its equal average crystalline particle diameter is 40--70 μ m, void content reaches 50%, is difficult to destroy this vesicular structure during dry ground.The particle of this structure is difficult to obtain the high goods of density on the other hand, and owing to dispersion expansion, the slabbing action of water, than the vesicular structure of destructible aggregate, crush efficiency, effect are all comparatively desirable during wet-milling.
2, half-finished forming method difference, all adopting in conjunction with nodulizer both at home and abroad, is vacuum deairing machine and the present invention adopts, and the cost of equipment is low, half-finished density is higher than the base substrate that nodulizer forms far away, and highdensity base substrate is to promoting burning till of product very favourable.
What 3, calcination equipment of the present invention adopted is hyperthermia tunnel Kiln, and operation control is simple, firing period is long, the product crystal zoon, and the cost of kiln is relatively low, and generic failure can be got rid of in normal productive process.And, make oxious component Na in the finished product owing to adopt the slow firing technique of high temperature
2O content≤0.2% (U.S.'s product is normally 0.3～0.4%), volume density height (＞3.60g/cm
3), intergranular gas is empty few, and grain size is more even, normally between 30-70cm.
4, owing to add MgO, AlF
3Densification additive makes sintering plate corundum near just obtaining the high-density finished product under the melt temperature.
After material is crushed to certain fineness; particle can produce cohesion; influence crush efficiency; therefore, the present invention has added grinding aid ethylene glycol in fine grinding technology, and add-on is 0.1-0.8%; after this active substance is adsorbed on particle surface; both can separate and coagulate, can reduce the particulate table again and energy, and crush efficiency is improved.The adding of grinding aid during department can reduce the consumption of water, improves the flowability of dispersed and mud.
By above several raw material technical finesse schemes, the fine mill size d50 that makes raw material below 2 μ m, thereby reduced the difficulty of solid state sintering, the firing temperature of product is compared with similar products at home and abroad is reduced nearly 100 ℃.
In addition, work in-process of the present invention adopt the stainless-steel vacuum pug mill, equal base under the 0.095Mpa condition greatly in vacuum tightness, and the base substrate section pore-free after the moulding shows compact shape, certain intensity is arranged, to satisfy the requirement of loading of kiln piling after the drying.
The present invention adopts small cross-section, many burners tunnel kiln, carry out combustion-supporting sintering with high temperature preheating wind, sintering temperature is 1790～1860 ℃, firing period is more than 50 hours, and wherein, base substrate stops more than 10 hours in being higher than 1600 ℃ zone, because firing temperature height, long in the high-temperature area residence time, the solid state sintering effect of base substrate is more complete, has guaranteed that every technical indicator of the finished product reaches higher level.
Embodiment one:
Step 1: batching
Take by weighing homemade one-level commercial alumina γ-Al
2O
3995 kilograms, MgO2.5 kilogram, AlF
32.5 kilogram.
Step 2: grind
Above-mentioned raw materials and 1000 kilograms in water, ethylene glycol are dropped in the grinding plant for 5 kilograms and grinds, make slip.
Step 3: filter-press dehydration
Above-mentioned slip is sent into pressure filter, by high-pressure filteration, slough the part moisture content in the slurry, the formation water content is 28% mud cake.
Step 4: base
Above-mentioned mud cake being dropped in the stainless-steel vacuum pug mill, add softening agent, is base under the 0.095Mpa condition in vacuum tightness.
Step 5: oven dry
Step 6: sintering
Small cross-section, many burners tunnel kiln carry out combustion-supporting sintering with high temperature preheating wind, and sintering temperature is 1800 ℃, and firing period is more than 70 hours, and wherein, base substrate stopped 11 hours in 1600 ℃ zone.
Step 7: fragmentation, screening, deironing
Step 8: packing
Embodiment two:
Step 1: batching
Take by weighing import commercial alumina γ-Al
2O
3994 kilograms, AlF
36 kilograms.
Step 2: grind
Above-mentioned raw materials and 1000 kilograms in water, ethylene glycol are dropped in the grinding plant for 5 kilograms and grinds, make slip.
Step 3: filter-press dehydration
Above-mentioned slip is sent into pressure filter, by high-pressure filteration, slough the part moisture content in the slurry, the formation water content is 33% mud cake.
Step 4: base
Above-mentioned mud cake being dropped in the stainless-steel vacuum pug mill, add softening agent, is base under the 0.095Mpa condition in vacuum tightness.
Step 5: oven dry
Step 6: sintering
Small cross-section, many burners tunnel kiln carry out combustion-supporting sintering with high temperature preheating wind, and sintering temperature is 1800 ℃, and firing period is more than 60 hours, and wherein, base substrate stopped 12 hours in 1600 ℃ zone.
Step 7: fragmentation, screening, deironing
Step 8: packing
Through above-mentioned technology, the product of making has following characteristic:
1, granule strength height, crystal boundary is in conjunction with fine;
2, the intergranular pore is few, and be evenly distributed, close higher, the wear resistance of product body, erosion resistance be good;
3, alkali metal oxide content is extremely low, reach＜0.2%;
4, crystallographic dimension is even, and the crystal grain of growing up unusually is few, and thermal shock resistance is good.
Claims (6)
1, with γ-Al
2O
3Be the processing method of raw material production sintering plate corundum, be characterised in that by following processing step and finish:
A, batching are selected γ-Al for use
2O
3Be main raw material, add additive, additive is MgO, AlF
3At least a
B, add the entry extra-fine grinding
C, filter-press dehydration
D, vacuum extrusion base
E, oven dry
F, high temperature sintering
G, fragmentation, screening, deironing
H, packing.
2,, it is characterized in that the additive add-on is 0.1～0.8% of total batching among the step a according to the described technology of claim 1.
3,, it is characterized in that water accounts for 40～60% of total batching and water gross weight among the step b according to the described technology of claim 1.
4, according to the described technology of claim 3, it is characterized in that also adding among the step b grinding aid, grinding aid is an ethylene glycol, add-on accounts for 0.1～0.8% of total batching.
5, according to the described technology of claim 1, it is characterized in that, in steps d, adopt vacuum deairing machine, equal base under the 0.095Mpa condition greatly in vacuum tightness.
6, according to the described technology of claim 1, it is characterized in that, in step f, adopt small cross-section, many burners tunnel kiln, carry out combustion-supporting sintering with high temperature preheating wind, sintering temperature is 1790～1860 ℃, firing period is more than 50 hours, and wherein, base substrate stops more than 10 hours in being higher than 1600 ℃ zone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021130981A CN1193958C (en) | 2002-06-03 | 2002-06-03 | With gamma-Al2O3Process for producing sintered tabular corundum from raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021130981A CN1193958C (en) | 2002-06-03 | 2002-06-03 | With gamma-Al2O3Process for producing sintered tabular corundum from raw material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1382658A true CN1382658A (en) | 2002-12-04 |
| CN1193958C CN1193958C (en) | 2005-03-23 |
Family
ID=4742438
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021130981A Expired - Fee Related CN1193958C (en) | 2002-06-03 | 2002-06-03 | With gamma-Al2O3Process for producing sintered tabular corundum from raw material |
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| Country | Link |
|---|---|
| CN (1) | CN1193958C (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439289C (en) * | 2006-06-08 | 2008-12-03 | 汉中秦元新材料有限公司 | Method for producing sintering plate-like corundum by ultra-high temperature shaft kiln |
| CN101209928B (en) * | 2006-12-29 | 2010-07-14 | 李正坤 | Technique for processing corundum |
| CN103833392A (en) * | 2014-01-03 | 2014-06-04 | 浙江自立氧化铝材料科技有限公司 | Preparation method for sintered corundum |
| CN103936440A (en) * | 2014-03-28 | 2014-07-23 | 浙江自立氧化铝材料科技有限公司 | Preparation method of sintered corundum with good wear resistance |
| CN104108922A (en) * | 2014-05-19 | 2014-10-22 | 江苏新时高温材料有限公司 | Processing technology of active corundum |
| CN104108942A (en) * | 2014-05-16 | 2014-10-22 | 江苏新时高温材料有限公司 | Processing technology of high-density sintered tabular corundum |
| CN107032764A (en) * | 2017-04-05 | 2017-08-11 | 淄博泰贝利尔铝镁有限公司 | A kind of dense ceramic material sintering method of high volume density |
| CN107074574A (en) * | 2015-09-30 | 2017-08-18 | 日本碍子株式会社 | The preparation method of plate-like aluminum oxide powder |
| CN108059447A (en) * | 2018-01-08 | 2018-05-22 | 浙江自立新材料股份有限公司 | A kind of big crystallization sintering plate corundum and preparation method thereof |
| CN109277518A (en) * | 2017-07-21 | 2019-01-29 | 中国科学院金属研究所 | A kind of preparation method of TiAl alloy hot investment casting refractory material |
| CN111136589A (en) * | 2019-12-30 | 2020-05-12 | 宁波大学 | Abrasive grain boundary bonding and fixing grinding tool and preparation method thereof |
-
2002
- 2002-06-03 CN CNB021130981A patent/CN1193958C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439289C (en) * | 2006-06-08 | 2008-12-03 | 汉中秦元新材料有限公司 | Method for producing sintering plate-like corundum by ultra-high temperature shaft kiln |
| CN101209928B (en) * | 2006-12-29 | 2010-07-14 | 李正坤 | Technique for processing corundum |
| CN103833392A (en) * | 2014-01-03 | 2014-06-04 | 浙江自立氧化铝材料科技有限公司 | Preparation method for sintered corundum |
| CN103833392B (en) * | 2014-01-03 | 2015-08-05 | 浙江自立氧化铝材料科技有限公司 | A kind of preparation method of alundum |
| CN103936440B (en) * | 2014-03-28 | 2015-04-01 | 浙江自立氧化铝材料科技有限公司 | Preparation method of sintered corundum with good wear resistance |
| CN103936440A (en) * | 2014-03-28 | 2014-07-23 | 浙江自立氧化铝材料科技有限公司 | Preparation method of sintered corundum with good wear resistance |
| CN104108942A (en) * | 2014-05-16 | 2014-10-22 | 江苏新时高温材料有限公司 | Processing technology of high-density sintered tabular corundum |
| CN104108922A (en) * | 2014-05-19 | 2014-10-22 | 江苏新时高温材料有限公司 | Processing technology of active corundum |
| CN107074574A (en) * | 2015-09-30 | 2017-08-18 | 日本碍子株式会社 | The preparation method of plate-like aluminum oxide powder |
| CN107032764A (en) * | 2017-04-05 | 2017-08-11 | 淄博泰贝利尔铝镁有限公司 | A kind of dense ceramic material sintering method of high volume density |
| CN109277518A (en) * | 2017-07-21 | 2019-01-29 | 中国科学院金属研究所 | A kind of preparation method of TiAl alloy hot investment casting refractory material |
| CN109277518B (en) * | 2017-07-21 | 2020-09-18 | 中国科学院金属研究所 | Preparation method of refractory material for TiAl alloy precision casting |
| CN108059447A (en) * | 2018-01-08 | 2018-05-22 | 浙江自立新材料股份有限公司 | A kind of big crystallization sintering plate corundum and preparation method thereof |
| CN111136589A (en) * | 2019-12-30 | 2020-05-12 | 宁波大学 | Abrasive grain boundary bonding and fixing grinding tool and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1193958C (en) | 2005-03-23 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Jiangsu Jingxin High-temperature Materials Co.,Ltd. Assignor: Xinjinghua Special Refractory Co Ltd, Jiangdu City Contract fulfillment period: 2008.12.18 to 2022.6.3 contract change Contract record no.: 2009320000204 Denomination of invention: Process for producing sintered tabular corundum by using gamma -AL#-[2]O#-[3] as raw material Granted publication date: 20050323 License type: Exclusive license Record date: 2009.3.3 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.12.18 TO 2022.6.3; CHANGE OF CONTRACT Name of requester: JIANGSU JINGXIN HIGH-TEMPERATURE MATERIALS CO., LT Effective date: 20090303 |
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Granted publication date: 20050323 Termination date: 20120603 |