CN1193958C - 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 PDF

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Publication number
CN1193958C
CN1193958C CNB021130981A CN02113098A CN1193958C CN 1193958 C CN1193958 C CN 1193958C CN B021130981 A CNB021130981 A CN B021130981A CN 02113098 A CN02113098 A CN 02113098A CN 1193958 C CN1193958 C CN 1193958C
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raw material
add
gamma
sintering
batching
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CN1382658A (en
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李正坤
张家勤
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Xinjinghua Special Refractory Co ltd Jiangdu City
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Xinjinghua Special Refractory Co ltd Jiangdu City
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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. The method comprises the following steps: the ingredients are gamma-Al2O3Adding additives into the main raw materials; adding water for superfine grinding; performing filter pressing and dehydration; performing vacuum extrusion blank making; drying; sintering at high temperature; crushing, screening and removing iron; and (6) packaging. The prepared product has high particle strength and good grain boundary bonding; few intercrystalline pores are distributed uniformly, and the product has high density and good wear resistance and erosion resistance; the content of alkali metal oxide is extremely low and reaches less than 0.2 percent; uniform crystal size, few abnormally grown crystal grains and good thermal shock property.

Description

With γ-Al 2O 3Processing method for the raw material production sintering plate corundum
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, the additive add-on is 0.1~0.8% of total batching;
B, add the entry extra-fine grinding, water accounts for 40~60% of total batching and water gross weight;
C, filter-press dehydration;
D, vacuum extrusion base;
E, oven dry;
F, adopt tunnel kiln, through 1790~1860 ℃ of high temperature sinterings, firing period is more than 50 hours, and wherein, base substrate stops more than 10 hours in being higher than 1600 ℃ zone;
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 surface energy again, and crush efficiency is improved.The adding of grinding aid simultaneously 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, are base under the 0.095Mpa condition 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 (4)

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, the additive add-on is 0.1~0.8% of total batching;
B, add the entry extra-fine grinding, water accounts for 40~60% of total batching and water gross weight;
C, filter-press dehydration;
D, vacuum extrusion base;
E, oven dry;
F, adopt tunnel kiln, through 1790~1860 ℃ of high temperature sinterings, firing period is more than 50 hours, and wherein, base substrate stops more than 10 hours in being higher than 1600 ℃ zone;
G, fragmentation, screening, deironing;
H, packing.
2, according to the described technology of claim 1, 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.
3, according to the described technology of claim 1, it is characterized in that, adopt vacuum deairing machine in steps d, is base under the 0.095Mpa condition in vacuum tightness.
According to the described technology of claim 1, it is characterized in that 4, tunnel kiln is small cross-section, many burners tunnel kiln in step f.
CNB021130981A 2002-06-03 2002-06-03 With gamma-Al2O3Process for producing sintered tabular corundum from raw material Expired - Fee Related CN1193958C (en)

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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

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Application Number Priority Date Filing Date Title
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CN1193958C true CN1193958C (en) 2005-03-23

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Families Citing this family (11)

* Cited by examiner, † Cited by third party
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
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
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
CN107074574B (en) * 2015-09-30 2020-09-22 日本碍子株式会社 Method for producing plate-like alumina 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
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
CN111136589B (en) * 2019-12-30 2022-10-21 宁波大学 Preparation method of abrasive grain boundary bonding and fixing grinding tool

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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

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

C17 Cessation of patent right
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Granted publication date: 20050323

Termination date: 20120603