CN103833392A - Preparation method for sintered corundum - Google Patents
Preparation method for sintered corundum Download PDFInfo
- Publication number
- CN103833392A CN103833392A CN201410005994.6A CN201410005994A CN103833392A CN 103833392 A CN103833392 A CN 103833392A CN 201410005994 A CN201410005994 A CN 201410005994A CN 103833392 A CN103833392 A CN 103833392A
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- alundum
- preparation
- balling
- corundum
- light
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Abstract
The invention discloses a preparation method for sintered corundum. The method comprises the following steps: (1) uniformly mixing gamma-Al2O3 and caustic-burned magnesia powder and carrying out crushing so as to obtain mixed powder, wherein a weight ratio of gamma-Al2O3 to caustic-burned magnesia powder is 94-96: 3-6; (2) subjecting the mixed powder prepared in the step (1) to balling twice so as to obtain a pre-sintered material; and (3) drying the pre-sintered material prepared in the step (2) and carrying out calcining and cooling molding so as to obtain sintered corundum. Preferably, the weight ratio of gamma-Al2O3 to caustic-burned magnesia powder is 95: 3-6. The method is energy saving and environment-friendly; the prepared sintered corundum has high volume density and low impurity content; a microstructure shows that crystal grain of the sintered corundum is of a sheet structure and has a size of 10 to 200 mu m, pores in the crystal exist in an enclosed form, and a crystal structure is compact; and the sintered corundum is widely applicable to production of high-grade shaped or shapeless refractory products.
Description
Technical field
The present invention relates to fire resisting material field, be specifically related to a kind of preparation method of alundum.
Background technology
Alundum belongs to high-purity refractory raw material, and it is widely used in produces high-grade setting or unsetting refractory product, has the features such as refractoriness is high, wear resistance good, resistance to fouling is good.It is raw material that alundum generally adopts Calcined polishing aluminum oxide or commercial alumina, add the appropriate short agent of burning, through dry grinding or wet-milling, make the weight percentage of the particle of granularity <10 μ m be greater than 95%, then through squeezing base or pelletizing, then drying and high temperature (1800～2000 DEG C) burn till.
Sintering plate corundum is to start development by Alcoa the thirties in 20th century, drops into a kind of high purity aluminium oxide raw material of suitability for industrialized production the seventies.Although the sintering plate corundum stable performance that Alcoa produces, production capacity is quite limited, and expensive, and the plate diamond spar that Alcoa produces exceeds 1200-2000 yuan/ton than domestic same quality plate diamond spar price.
Domestic have the company such as Hanzhong Qiyuan New Material Co., Ltd., Zibo Tai Beilier magnalium company limited to start development and production alundum at present, the plate diamond spar quality that wherein Hanzhong Qiyuan New Material Co., Ltd. produces is the most stable, but the non-energy of production capacity limited (10000 tons of left and right of annual production), cannot meet domestic market needs completely; The plate diamond spar production capacity that Zibo Tai Beilier magnalium company limited produces is large (producing 30000 tons of left and right per year) slightly, but quality is very unstable, often occurs quality problems in use procedure.
Along with the increase day by day to plate diamond spar demand, the supply of plate diamond spar and quality all cannot satisfy the demands, and therefore need to provide a kind of good product quality, and the high alundum of production capacity.
The disclosure of the invention that Granted publication number is CN101085706B a kind of processing method that adopts ultra-high temperature shaft kiln to produce sintering plate corundum, this patent is raw material because adopting low sodium high purity pre-burning aluminum oxide powder, firing temperature is higher, up to 1850～1920 DEG C, when this patent adopts pan-pelletizer and cylinder balling-up simultaneously, require intermittently to spray balling-up liquid, balling-up liquid is prepared by high-purity aluminium glue and phosphoric acid, rafifinal gum concentration is 0.3%, phosphoric acid concentration is 0.15%, balling-up liquid has in sharp balling-up, but introduces foreign matter of phosphor, causes product purity to decline.
Similarly, the disclosure of the invention that application publication number is CN102503448A a kind of preparation technology of sintering plate corundum, in this preparation technology, still used the balling-up liquid that comprises aluminium glue and phosphoric acid, cause the decline of product purity.
In prior art, in conventional corundum spinelle mould material, if while using plate diamond spar, all need to add magnesia or aluminum-spinel, make to form corundum spinelle system in mould material, to improve the slag resistance of mould material.
Summary of the invention
The invention provides a kind of preparation method of alundum, can under lower firing temperature, prepare corundum, at the crystals of corundum, aluminum-spinel crystal and corundum crystal are uniformly distributed mutually, in actual use, without adding again magnesia or other spinel raw materials, can ensure excellent slag resistance and thermal shock resistance, use convenient.
A preparation method for alundum, comprises the following steps:
(1) by γ-Al
2o
3after mixing with light-burning magnesium powder, pulverize, obtain powder mix, described γ-Al
2o
3with the weight ratio of light-burning magnesium powder be 94～96:3～6;
(2) step (1) gained powder mix, after twice balling-up, obtains Preburning material;
(3) after step (2) gained Preburning material is dried, through calcining and cooling forming, obtain described alundum.
Described γ-Al
2o
3for common industrial γ-Al
2o
3, γ-Al
2o
3in Al
2o
3content should be enough high, to meet the basic demand that forms corundum, described γ-Al
2o
3in each component weight percentage be respectively Al
2o
3>=98.5%, SiO
2≤ 0.04%.Also be described γ-Al
2o
3middle Al
2o
3weight percentage be 98.5%～100%, SiO
2weight percentage be 0～0.04%.
Described γ-Al
2o
3in residuals weight percentage ratio be foreign matter content, weight percentage≤0.55% of alkalimetal oxide in impurity.
In described light-burning magnesium powder, each component weight percentage is respectively MgO>=95%, SiO
2≤ 0.5%, CaO≤1.0%, Fe
2o
3≤ 0.7%.
Residuals weight percentage ratio in light-burning magnesium powder is foreign matter content, and owing to having added light-burning magnesium powder, sintering that can accelerating oxidation aluminium, has reduced sintering temperature, simultaneously light-burning magnesium powder and Al
2o
3can also form Spinel, improve the slag resistance of alundum.
Described γ-Al
2o
3within should being controlled at suitable scope with the weight ratio of light-burning magnesium powder, if the too high levels of light-burning magnesium powder may be destroyed the crystalline structure of corundum self, if the content of light-burning magnesium powder is too low, do not have the good burning effect that helps, and the change of slag resistance is also limited, preferably, described γ-Al
2o
3with the weight ratio of light-burning magnesium powder be 95:3～6.
As preferably, described γ-Al
2o
3in grain diameter≤60 order of 90wt% at least, grain diameter≤120 order of 90wt% at least in described light-burning magnesium powder.
Described γ-Al
2o
3in grain diameter≤60 order of 90wt% at least, for example, if γ-Al
2o
3weight be 100kg, γ-Al of 90kg at least wherein
2o
3grain diameter≤60 order (250um).
Grain diameter≤120 order of 90wt% at least in described light-burning magnesium powder, for example, if the weight of light-burning magnesium powder is 100kg, grain diameter≤120 order (125um) of the light-burning magnesium powder of 90kg at least wherein.
γ-Al
2o
3should there is suitable particle diameter proportioning with light-burning magnesium powder, be uniformly distributed to meet aluminum-spinel crystal and corundum crystal in the structure of final formation, crystalline structure densification, crystals pore all exists with closing form.
The raw material using in the present invention does not need in advance through processing, can directly use, when raw material is mixed, can adopt planetary or cone-type mixer, after mixing, put into tuber grinder dry grind (pulverize), by adjusting the proportioning of shredder in tuber grinder, the rotating speed of inlet amount and grading machine, makes the more than 95% granularity <325 order (44um) of weight fraction in discharging (powder mix).
Powder mix after dry grinding carries out balling-up, and preferably, described twice balling-up is followed successively by disk balling-up and cylinder balling-up.First adopt disk to carry out a balling-up, the diameter of a balling-up is 8～12mm, and then carry out secondary balling-up by cylinder, a balling-up gained pellet is further assembled, the diameter of secondary balling-up is 25～35mm, sprays continuously deionized water and (in deionized water, remove in advance Na in whole balling-up (comprising a balling-up and secondary balling-up) process
+and K
+), the moisture content in control ball is 18～22%.
After secondary balling-up, be dried, preferably, described dry comprise primary drying and redrying, the temperature of primary drying is 150～200 DEG C, the time of primary drying is 20～30h, and the temperature of redrying is 450～650 DEG C, and the time of redrying is 20～30h.
Hot blast when primary drying utilizes finished product (corundum after sintering completes) cooling is dried balling-up, the remaining <5% of moisture in the pellet after primary drying; Pellet after redrying utilizes shaft furnace smoke evacuation hot blast to primary drying further carries out redrying, the remaining <1.0% of moisture in the pellet after redrying.
Preferably, the temperature of described calcining is 1750～1850 DEG C, and the time of described calcining is 2～3h.
When calcining, use high temperature vertical kiln, adopt Sweet natural gas to burn till, by regulating the ratio of Sweet natural gas, combustion air and atomization wind, Sweet natural gas is fully burnt, calcining temperature decreases compared to existing technology, has effectively saved the energy.
After having calcined, carry out coolingly fast, pass into high pressure cold wind by the bottom of shaft furnace clinkering zone, make the ball after burning till cooling fast, cold high pressure is distinguished and admirable through burnt corundum just, and temperature can raise, become hot blast, utilize this hot blast to carry out the primary drying of pellet, realize the recycle of energy.
The inventive method energy-conserving and environment-protective, and the alundum preparing, volume density is high, foreign matter content is low, microstructure shows corundum crystal grain structure in the form of sheets, is of a size of 10～200 μ m, and crystals pore exists with closing form, crystalline structure is tight, can be widely used in and produce high-grade setting or unsetting refractory product.
Brief description of the drawings
Fig. 1 is the micro-structure diagram of the alundum for preparing of the present invention.
Embodiment
Embodiment 1
A preparation method for alundum, its technical process is:
(1) choose raw material
Choose general industry γ-Al
2o
3with light-burning magnesium powder be raw material, wherein general industry γ-Al
2o
3granularity requirements-60 order>=90.0%, Al
2o
3%>=98.5%, SiO
2%≤0.04%, R
2o%≤0.55%; Light-burning magnesium powder granularity requirements-120 order>=90.0%, MgO%>=95%, SiO
2%≤0.5%, CaO≤1.0%, Fe
2o
3≤ 0.7%.
In the present invention, if no special instructions, percentage ratio is weight percentage.
(2) mix
Take γ-Al of 950kg
2o
3mix in planetary-type mixer with the light-burning magnesium powder of 50kg, obtain mixture.
(3) grind
Mixture in step (2) is put into tuber grinder and dry grind, obtain powder mix.Mill ball mass ratio is large ball (diameter 50mm): bead (diameter 30mm)=1:4, inlet amount is 95kg/h, grading machine rotating speed is 900r/min, and powder mix granularity is controlled at the more than 95% median size <325 order (44um) of weight fraction.
(4) balling-up
Powder mix after dry grinding first adopts a balling-up of disk, and once becoming spherical diameter is 10mm, then by the balling-up of cylinder secondary, it is 25mm that secondary becomes spherical diameter.In whole balling-up process, spray continuously deionized water, this deionized water has been removed Na
+and K
+, control the moisture content <20% of ball simultaneously.
(5) dry
The pellet that the hot blast that utilizes the cooling generation of finished product obtains after to step (4) secondary balling-up carries out primary drying, and hot blast temperature is 170 DEG C of left and right, time of drying 24h, pellet residual water-content <5% after drying; Then utilize shaft furnace smoke evacuation hot blast further to carry out redrying to pellet, hot blast temperature is 550 DEG C of left and right, and time of drying, 24h, dried rear pellet residual water-content <1.0%.
(6) high temperature sintering
Dried pellet is placed in shaft furnace high-temperature calcination, and temperature is 1800 DEG C of left and right, calcination time 2 hours.
(7) cooling
Pass into high pressure cold wind by shaft furnace clinkering zone bottom, make the ball after burning till cooling fast.
(8) inspection
Ball to kiln discharge is tested, main test ball burn till quality, detect ball and whether have burning or raw burn phenomenon.
(9) processing, packaging
The corundum ball being up to the standards is carried out to fragmentation, the particle that fragmentation is good is tested, qualified product packaging warehouse-in.
The performance index of the prepared alundum of the present embodiment are as shown in table 1.
Table 1
The composition of plate diamond spar of the prior art is all aluminum oxide, and the alundum preparing in the application possesses the form of plate diamond spar, at the crystals of corundum, aluminum-spinel crystal and corundum crystal are uniformly distributed mutually, in actual use, without adding again magnesia or other spinel raw materials (as shown in table 1), and slag resistance excellence, be better than the refractory product making after plate diamond spar of the prior art mixes with magnesium oxide or spinel.
Claims (8)
1. a preparation method for alundum, is characterized in that, comprises the following steps:
(1) by γ-Al
2o
3after mixing with light-burning magnesium powder, pulverize, obtain powder mix, described γ-Al
2o
3with the weight ratio of light-burning magnesium powder be 94～96:3～6;
(2) step (1) gained powder mix, after twice balling-up, obtains Preburning material;
(3) after step (2) gained Preburning material is dried, through calcining and cooling forming, obtain described alundum.
2. the preparation method of alundum as claimed in claim 1, is characterized in that, described γ-Al
2o
3with the weight ratio of light-burning magnesium powder be 95:3～6.
3. the preparation method of alundum as claimed in claim 1 or 2, is characterized in that, described γ-Al
2o
3in each component weight percentage be respectively Al
2o
3>=98.5%, SiO
2≤ 0.04%.
4. the preparation method of alundum as claimed in claim 3, is characterized in that, in described light-burning magnesium powder, each component weight percentage is respectively MgO>=95%, SiO
2≤ 0.5%, CaO≤1.0%, Fe
2o
3≤ 0.7%.
5. the preparation method of alundum as claimed in claim 4, is characterized in that, described γ-Al
2o
3in grain diameter≤60 order of 90wt% at least, grain diameter≤120 order of 90wt% at least in described light-burning magnesium powder.
6. the preparation method of alundum as claimed in claim 5, is characterized in that, the temperature of described calcining is 1750～1850 DEG C, and the time of described calcining is 2～3h.
7. the preparation method of alundum as claimed in claim 6, is characterized in that, described twice balling-up is followed successively by disk balling-up and cylinder balling-up.
8. the preparation method of alundum as claimed in claim 7, it is characterized in that, described dry comprise primary drying and redrying, the temperature of primary drying is 150～200 DEG C, the time of primary drying is 20～30h, the temperature of redrying is 450～650 DEG C, and the time of redrying is 20～30h.
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|---|---|---|---|
| CN201410005994.6A CN103833392B (en) | 2014-01-03 | 2014-01-03 | A kind of preparation method of alundum |
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|---|---|---|---|
| CN201410005994.6A CN103833392B (en) | 2014-01-03 | 2014-01-03 | A kind of preparation method of alundum |
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| CN103833392B CN103833392B (en) | 2015-08-05 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072162A (en) * | 2014-06-19 | 2014-10-01 | 浙江自立氧化铝材料科技有限公司 | Preparation method of tabular corundum with high volume density |
| CN104496432A (en) * | 2014-12-29 | 2015-04-08 | 阳泉金隅通达高温材料有限公司 | Preparation method of modified sintered corundum |
| CN106631072A (en) * | 2016-12-29 | 2017-05-10 | 浙江自立新材料股份有限公司 | Gradient material for castable and preparation method thereof |
| CN107445595A (en) * | 2017-07-13 | 2017-12-08 | 河南建筑材料研究设计院有限责任公司 | The method that corundum abrasive is prepared using microwave sintering |
| CN111574205A (en) * | 2020-06-01 | 2020-08-25 | 江苏晶鑫新材料股份有限公司 | Production method of sintered corundum and production line for production and preparation |
| CN114394840A (en) * | 2021-12-31 | 2022-04-26 | 江苏新时高温材料股份有限公司 | Plate-shaped corundum ball for high-purity bulk density petrochemical filler |
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| US3905845A (en) * | 1969-08-27 | 1975-09-16 | Ngk Insulators Ltd | Translucent alumina containing magnesia yttria and lanthium oxide |
| CN1382658A (en) * | 2002-06-03 | 2002-12-04 | 江都市新晶辉特种耐火材料有限公司 | Process for sintering plate corundum from gamma-Al2O3 as raw material |
| CN101085706A (en) * | 2006-06-08 | 2007-12-12 | 汉中秦元新材料有限公司 | Method for producing sintering plate-like corundum by ultra-high temperature shaft kiln |
| CN102503448A (en) * | 2011-09-30 | 2012-06-20 | 汉中秦元新材料有限公司 | Preparation technology of sintered tabular corundum |
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2014
- 2014-01-03 CN CN201410005994.6A patent/CN103833392B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3905845A (en) * | 1969-08-27 | 1975-09-16 | Ngk Insulators Ltd | Translucent alumina containing magnesia yttria and lanthium oxide |
| CN1382658A (en) * | 2002-06-03 | 2002-12-04 | 江都市新晶辉特种耐火材料有限公司 | Process for sintering plate corundum from gamma-Al2O3 as raw material |
| CN101085706A (en) * | 2006-06-08 | 2007-12-12 | 汉中秦元新材料有限公司 | Method for producing sintering plate-like corundum by ultra-high temperature shaft kiln |
| CN102503448A (en) * | 2011-09-30 | 2012-06-20 | 汉中秦元新材料有限公司 | Preparation technology of sintered tabular corundum |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072162A (en) * | 2014-06-19 | 2014-10-01 | 浙江自立氧化铝材料科技有限公司 | Preparation method of tabular corundum with high volume density |
| CN104072162B (en) * | 2014-06-19 | 2016-01-13 | 浙江自立氧化铝材料科技有限公司 | The preparation method of the plate diamond spar that a kind of volume density is high |
| CN104496432A (en) * | 2014-12-29 | 2015-04-08 | 阳泉金隅通达高温材料有限公司 | Preparation method of modified sintered corundum |
| CN106631072A (en) * | 2016-12-29 | 2017-05-10 | 浙江自立新材料股份有限公司 | Gradient material for castable and preparation method thereof |
| CN106631072B (en) * | 2016-12-29 | 2019-05-28 | 浙江自立新材料股份有限公司 | A kind of functionally gradient material (FGM) and preparation method thereof for castable |
| CN107445595A (en) * | 2017-07-13 | 2017-12-08 | 河南建筑材料研究设计院有限责任公司 | The method that corundum abrasive is prepared using microwave sintering |
| CN111574205A (en) * | 2020-06-01 | 2020-08-25 | 江苏晶鑫新材料股份有限公司 | Production method of sintered corundum and production line for production and preparation |
| CN111574205B (en) * | 2020-06-01 | 2021-02-12 | 江苏晶鑫新材料股份有限公司 | Production line for preparing sintered corundum |
| CN114394840A (en) * | 2021-12-31 | 2022-04-26 | 江苏新时高温材料股份有限公司 | Plate-shaped corundum ball for high-purity bulk density petrochemical filler |
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|---|---|
| CN103833392B (en) | 2015-08-05 |
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Address after: 312369 Shangyu, Shaoxing, Hangzhou Bay Industrial Park, No., No. three East Road, No. 6 Patentee after: Zhejiang self-reliance new materials Limited by Share Ltd Address before: 312369 Shangyu, Shaoxing, Hangzhou Bay Industrial Park, No., No. three East Road, No. 6 Patentee before: ZHEJIANG ZILI ALUMINA MATERIAL TECHNOLOGY CO., LTD. |
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Application publication date: 20140604 Assignee: Zhejiang Zili High Temperature Technology Co.,Ltd. Assignor: ZHEJIANG ZILI ADVANCED MATERIALS Co.,Ltd. Contract record no.: X2021330000207 Denomination of invention: A preparation method of sintered corundum Granted publication date: 20150805 License type: Common License Record date: 20210831 Application publication date: 20140604 Assignee: Shaoxing Hongyi New Material Co.,Ltd. Assignor: ZHEJIANG ZILI ADVANCED MATERIALS Co.,Ltd. Contract record no.: X2021330000208 Denomination of invention: A preparation method of sintered corundum Granted publication date: 20150805 License type: Common License Record date: 20210831 |