CN1465529A - Method for preparing zirconium dioxide by electrically smelting zircon - Google Patents
Method for preparing zirconium dioxide by electrically smelting zircon Download PDFInfo
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- CN1465529A CN1465529A CNA021131325A CN02113132A CN1465529A CN 1465529 A CN1465529 A CN 1465529A CN A021131325 A CNA021131325 A CN A021131325A CN 02113132 A CN02113132 A CN 02113132A CN 1465529 A CN1465529 A CN 1465529A
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- zirconium dioxide
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- preparing zirconium
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Abstract
A process for preparing zirconium by means of electric melting zircon includes mixing zircon powder of 809-120 mesh which is used as the raw material with high pure graphite with a need for an exces coefficient of 13% and 4-14% of bonding material, feeding them into electric arc furnace and being smelt at voltage of 170-190 V, current of 3800-4300 A and temperature of 1700-2500 deg.C for 110-130 minutes, raising the temperature further to 2500-2700 deg.C, inclining the furnace and spraying out the liquid melt with mixed oxygen and air. The obtained zirconium is of monoclinic hollow micro-bead and have a purity of over 98%.
Description
Technical field
The present invention relates to a kind of method of preparing zirconium dioxide by electrically smelting zircon, refer to a kind of improved electric arc furnace electric smelting zircon that utilizes especially, produce the method for monoclinic form zirconium dioxide.
Background technology
Zirconium white is mainly used in aspects such as containing zirconium refractory product, zircite product, insulating refractory, cermet material and ceramic pigment as a kind of raw material.
In the prior art, newer production zirconium white method is Chinese patent ZL94115847 disclosed " a kind of electrofusion ball-blowing production method of zirconium dioxide ".This method is to adopt wet method to feed intake, promptly the water batch mixing, drop in the electric arc furnace, under low voltage 116V, with the low current 1800A starting the arc, about 2000 ℃, melting 1-2 hour, and in the time of 2430 ℃, inclination electric arc furnace, and with 8-10kg/cm
2Pressurized air is blown out hollow spherulite with fused solution.
There is following defective in this method:
1, the raw material after the wet laid furnishes when dropping in the stove, enters the high-temperature zone, does not have time of drying, and the temperature in the caking, and stove immediately is not a constant temperature, carbon-rich zone can occur, so that forms carburizing reagent, generates zirconium carbide, influences quality product;
2, under the low voltage 116V, with the low current 1800A starting the arc, be difficult to reach 2430 ℃, the electric smelting weak effect can't generate zirconium dioxide, influences quality product;
3,8-10kg/cm
2Pressurized air blows ball, and oxygen content is low in the air, can't make the further oxidation of zirconium in the fused solution, also influences quality product.
4, in view of the foregoing, this method is difficult to make purity and reaches 98% zirconium dioxide.
Summary of the invention
The object of the present invention is to provide that a kind of technology is easy, reliable, the method for fusion and the preparing zirconium dioxide by electrically smelting zircon that winding-up is once finished, purity height, quality product are good.
For reaching above-mentioned purpose, solution of the present invention is:
A kind of method of preparing zirconium dioxide by electrically smelting zircon, its step is as follows:
(1) be raw material with 80-120 purpose zircon, 13% as excessive adjustment coefficient adding 80-120 purpose high purity graphite powder, and adds the binding agent of 4%-10%, uniform mixing;
(2) mixed raw materials is dropped in the electric arc furnace, under the voltage of 170-190V, with the electric current starting the arc of 3800-4300A;
(3) in the time of 1700-2500 ℃, melting 110-130 minute;
(4) continue to heat, in the time of 2500-2700 ℃, the inclination electric arc furnace is with oxygen and Air mixing gas, with 6-8kg/cm again
2Pressure is jetted fused solution, promptly makes monoclinic crystal zirconium dioxide hollow spherulite.
Wherein, above-mentioned steps (1) may further be: mixed raw materials is extruded into strip, and 140 ℃ of dryings, so that reaction is more thorough, quality product is better.
Above-mentioned steps (3) may further be: adjust voltage to 120-140V, electric current is to 5300-5500A, in the time of 1700-2500 ℃, and melting 110-130 minute.
Above-mentioned steps (4) can increase a step before: continue to strengthen electric current to 5500-6200A, and voltage 110-130V, in the time of 2500-2700 ℃, refining 10-20 minute.
Oxygen and Air mixing ratio are 1: 1 in the above-mentioned steps (4).
After adopting aforesaid method, technology of the present invention is easy, reliable, fusion and winding-up are once finished, and the present invention compares with existing production technique, has the following advantages:
1, the raw material behind the dry mixing, when dropping in the stove, the temperature constant temperature in the arc stability, stove carbon-rich zone can not occur, and unlikely generation carburizing reagent does not have zirconium carbide extremely and generates, and furnace charge can not lump, and quality product is good, and power saving;
2, under the 170-190V voltage, with the starting the arc of 3800-4300A electric current, the high 1700-2500 of smelting temperature ℃, effective, easily generate zirconium dioxide, quality product is good;
3,6-8kg/cm
2Compressed oxygen and Air mixing gas blow ball, the oxygen content height, and the purity of further zirconium in the oxidation fusion liquid, and then raising zirconium dioxide can reach more than 98%, and quality product is good.
Embodiment
One, material choice:
Selecting for use of zircon: zirconium dioxide content is more than 65%, and dioxide-containing silica is more than 32%, the 80-120 order.
Selecting for use of high purity graphite powder: carbon content is more than 98%, the 80-120 order.
Selecting for use of binding agent: starch.
Two, raw material mixes:
In the zircon raw material, with 13% as excessive adjustment coefficient, add the high purity graphite powder, and add the binding agent of 4%-10%, with V-type mixer uniform mixing; Raw material behind the batch mixing is extruded into strip, and temperature is dry at 140 degree, becomes the strip shape body that certain anti-pressure ability is arranged.
Three, reinforced, desiliconization, refining:
Electric arc furnace liner diameters 1200-1400 millimeter, degree of depth 700-800 millimeter.
The 900-1300kg raw material is dropped in the stove electric arc.Select the submerged arc production method for use, striking current 3800-4300A, voltage 170-190V.According to physical change in the stove, adjust temperature in the stove, in the time of 1700-2500 ℃, carry out desiliconization, adjust electric current 5300-5500A, voltage 120-140V, melting 110-130 minute.Heat again, carry out refining according to the physical change in the stove (referring to desiliconization degree in the electric arc furnace), continue to strengthen electric current, to reach 5500-6200A, voltage 110-130V is greatly about 10-20 minute, when melt temperature reaches 2500-2700 ℃, when in stove, cannot see white fine silica, carry out discharging.
Four, discharging:
During discharging, electrode lifts, and the electric furnace 36-42 degree that tilts is inclined and liquation, and by the raw materials melt liquid of discharge port (being that the water-cooled stove is chewed), the mixed gas of handling through 1: 1 oxygen and air cooling-down is with 6-8kg/cm
2Pressure winding-up (flow velocity of 10 cubic metres of gas-holder stable airs is 12-14m/s), make 2500-2700 ℃ liquation reach rapid cooling, the zirconium that contains that promptly forms 1-5 mm dia, tawny, principal crystalline phase and be monoclinic crystal is 98% zirconium dioxide raw material product, it is the zirconium dioxide hollow ball, thereby solved carbonaceous particles problem in the zirconium ball, and improved the quality of product.
Claims (5)
1, a kind of method of preparing zirconium dioxide by electrically smelting zircon is characterized in that:
(1) be raw material with 80-120 purpose zircon, 13% as excessive adjustment coefficient adding 80-120 purpose high purity graphite powder, and adds the binding agent of 4%-10%, uniform mixing;
(2) mixed raw materials is dropped in the electric arc furnace, under the voltage of 170-190V, with the electric current starting the arc of 3800-4300A;
(3) in the time of 1700-2500 ℃, melting 110-130 minute;
(4) continue to heat, in the time of 2500-2700 ℃, the inclination electric arc furnace is with oxygen and Air mixing gas, with 6-8kg/cm again
2Pressure is jetted fused solution, promptly makes monoclinic crystal zirconium dioxide hollow spherulite.
2, the method for a kind of preparing zirconium dioxide by electrically smelting zircon as claimed in claim 1 is characterized in that:
Step (1) further is: mixed raw materials is extruded into strip, 140 ℃ of dryings.
3, the method for a kind of preparing zirconium dioxide by electrically smelting zircon as claimed in claim 1 is characterized in that:
Step (3) further is: adjust voltage to 120-140V, electric current is to 5300-5500A, in the time of 1700-2500 ℃, and melting 110-130 minute.
4, the method for a kind of preparing zirconium dioxide by electrically smelting zircon as claimed in claim 1 is characterized in that:
Step (4) increases a step before: continue to strengthen electric current to 5500-6200A, and voltage 110-130V, in the time of 2500-2700 ℃, refining 10-20 minute.
5, the method for a kind of preparing zirconium dioxide by electrically smelting zircon as claimed in claim 1 is characterized in that: oxygen and Air mixing ratio are 1: 1 in the step (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021131325A CN1193936C (en) | 2002-06-04 | 2002-06-04 | Method for preparing zirconium dioxide by electrically smelting zircon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021131325A CN1193936C (en) | 2002-06-04 | 2002-06-04 | Method for preparing zirconium dioxide by electrically smelting zircon |
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| CN1465529A true CN1465529A (en) | 2004-01-07 |
| CN1193936C CN1193936C (en) | 2005-03-23 |
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| CNB021131325A Expired - Lifetime CN1193936C (en) | 2002-06-04 | 2002-06-04 | Method for preparing zirconium dioxide by electrically smelting zircon |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328172C (en) * | 2004-06-25 | 2007-07-25 | 郑州振中电熔锆业有限公司 | Process for preparing high-purity zirconium dioxide |
| CN101108775B (en) * | 2007-08-27 | 2010-10-13 | 中钢集团洛阳耐火材料研究院有限公司 | Method for manufacturing zirconium oxide product |
| CN104445396A (en) * | 2014-12-05 | 2015-03-25 | 三祥新材股份有限公司 | Method for preparing high-purity fused zirconia |
| CN105905942A (en) * | 2014-12-05 | 2016-08-31 | 三祥新材股份有限公司 | High-purity electric smelting zirconium oxide |
| CN109773939A (en) * | 2019-01-17 | 2019-05-21 | 山东磊宝锆业科技股份有限公司 | It is the method for raw material blowing polycrystalline flint clay hollow sphere with flint clay |
-
2002
- 2002-06-04 CN CNB021131325A patent/CN1193936C/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328172C (en) * | 2004-06-25 | 2007-07-25 | 郑州振中电熔锆业有限公司 | Process for preparing high-purity zirconium dioxide |
| CN101108775B (en) * | 2007-08-27 | 2010-10-13 | 中钢集团洛阳耐火材料研究院有限公司 | Method for manufacturing zirconium oxide product |
| CN104445396A (en) * | 2014-12-05 | 2015-03-25 | 三祥新材股份有限公司 | Method for preparing high-purity fused zirconia |
| CN104445396B (en) * | 2014-12-05 | 2016-06-29 | 三祥新材股份有限公司 | A kind of zirconic preparation method of high-purity electro-melting |
| CN105905942A (en) * | 2014-12-05 | 2016-08-31 | 三祥新材股份有限公司 | High-purity electric smelting zirconium oxide |
| CN109773939A (en) * | 2019-01-17 | 2019-05-21 | 山东磊宝锆业科技股份有限公司 | It is the method for raw material blowing polycrystalline flint clay hollow sphere with flint clay |
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| Publication number | Publication date |
|---|---|
| CN1193936C (en) | 2005-03-23 |
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Denomination of invention: Method for preparing zirconium dioxide by electrically smelting zircon Effective date of registration: 20110624 Granted publication date: 20050323 Pledgee: Bank of China, Limited by Share Ltd, Zhangzhou, Huaan branch Pledgor: Zhangzhou Jinyuansheng Zirconium Industry Co., Ltd. Registration number: 2011990000239 |
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Granted publication date: 20050323 |
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