CN1176875C - Hydration-resisting refractory MgO-CaO material series and its prepn - Google Patents
Hydration-resisting refractory MgO-CaO material series and its prepnInfo
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- CN1176875C CN1176875C CNB01128336XA CN01128336A CN1176875C CN 1176875 C CN1176875 C CN 1176875C CN B01128336X A CNB01128336X A CN B01128336XA CN 01128336 A CN01128336 A CN 01128336A CN 1176875 C CN1176875 C CN 1176875C
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- cao
- mgo
- hydration
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Abstract
The present invention relates to hydration-resisting refractory MgO-CaO materials used for metallurgy industry, and a preparing method thereof. Granular refractory MgO-CaO materials are used as raw materials, the material surfaces are treated in a light hydration mode and a carbonization mode by mixed gas of CO2 water vapor, and thus, a dense CaCO3 hydration-resisting film is formed at the refractory material surfaces; the film can effectively isolate CaO at the inner part to come into contact with external moisture, and thus, the hydration-resisting performance of the refractory MgO-CaO materials is obviously improved. Because the surface of CaO is treated, the present invention reserve the activity at the inner part of CaO, and thereby, the steel liquid cleaning performance of the refractory MgO-CaO materials is not damaged; simultaneously, CaCO3 at the material surfaces can be re-decomposed into CaO and CO2 in using, and the CaO which is obtained by re-decomposing the CaCO3 has high activity, and is favorable to decontaminating impurities in molten steel. The present invention has the advantages of high generating speed rate, short treating time and low production cost.
Description
The present invention relates to a kind of hydration-resisting refractory MgO-CaO material series that is used for metallurgy industry and preparation method thereof, this refractory materials can be made into the good various refractory products of hydration resistance.
Because the MgO-CaO series refractory material has characteristics such as fusing point height, reserves are big, alkali-resistivity scouring ability is strong, as far back as 16th century MgO-CaO series refractory material just be applied in the metallurgy industry.Especially in recent years, development along with steel-smelting technology, therefore specification of quality to iron and steel improves constantly, and requires Iron And Steel Industry should reduce the steel impurity component as much as possible, but does not adsorb the ability of impurity such as Si, S in the molten steel, P usually for most of refractory materials.The MgO-CaO series refractory material has the effect of unique cleaning molten steel by force owing to absorption impurity ability, and good high-temperature use properties, thermodynamic stability preferably, and be considered to a kind of comparatively ideal steel-making refractory materials, can be widely used as ladle and middle cylinder-packing material, and the external refining refractory materials.But this material causes the destruction of goods because the free CaO that contains very easily reacts with water.Therefore, for the unsetting refractory product that extensively in the steel-making industry, uses owing to need to add the moisture of higher proportion in process of production, make the MgO-CaO series refractory material be difficult to be applied to unsetting refractory product, thereby limited its use in Iron And Steel Industry greatly.
For improving MgO-CaO series refractory material hydration resistance problem, mainly contain following approach:
(a) by adding various additives, the CaO crystal grain in the MgO-CaO series refractory material is coated;
(b) be that the inorganic salt coating is carried out on the refractory raw material surface to MgO-CaO;
(c) be that the organism coating is carried out on the refractory raw material surface to MgO-CaO;
More for (a) method people research, Chinese patent 1156710 are to adopt by at ZrO
2Add 0-3%CeO, 0-2%Fe in the-CaO material
2O
3, 1-8%SiO
2Deng additive and by heat-treating methods the hydration resistance of material is increased; " silicate journal " 1991 (2) once reported interpolation Al
2O
3To MgO-CaO is the influence of the coking property and the hydration resistance of grog refractory, and the result thinks and adds 3%Al
2O
3To MgO-CaO is that the hydration resistance of grog refractory has tangible raising effect.But this method can make the goods high-temperature behavior be subjected to a certain extent infringement usually, and some material that exists in the additive is easy to diffuse in the molten steel simultaneously, can cause to a certain degree pollution to molten steel.
For (b) method, people such as the white department of " external refractory materials " 1996 (3) report mortar wells are that refractory raw material is immersed in the phosphoric acid solution of 5% concentration and carries out surface treatment with MgO-CaO.Find that the grog surface of handling generally covers phosphorus, particularly where, generated phosphate compounds, make the hydration resistance degree of grog that the raising of going up largely be arranged based on calcium phosphate at CaO.But, this MgO-CaO of improvement is that the method for grog refractory hydration resistance tends to bring certain detrimental impurity, as P, S etc., molten steel is caused to a certain degree pollution, and integument comes off easily in construction process, causes the hydration resistance of grog to reduce.The clear 61-256961 of Japanese Patent is by using CO
2Gas is handled pure CaO material surface, but because of
Speed of response is slower, and is difficult to reach the ideal effect, the refractory product that makes based on this, and hydration resistance improves not fairly obvious.
For (c) method, Chinese patent 1245479 adopts a kind of three liquid type surface treatment agents that contain the matrix treatment agent of water slurry shape, liquid matrix strengthening agent and tinting material, order is coated with said mixture etc., can form on the calcium-base inorganic members surface at short notice do not have be full of cracks, level and smooth, high strength and high resistivity against fire, glossiness painted filming.Anhydrous organism carries out the surface-treated method, though help improving the water-fast voltinism of CaO, also there is the organic composition instability in this method, coats uneven shortcoming, thereby has influenced anti-aquation effect.
Problem to be solved by this invention be the deficiency that exists at above-mentioned prior art and provide a kind of simple for production, hydration resistance is good and the hydration-resisting refractory MgO-CaO material series of favourable purification of molten steel and preparation method thereof.
Refractory materials of the present invention is realized by following technical scheme: with particulate state MgO-CaO series refractory material is raw material, and its difference is to coat on MgO-CaO series refractory material surface the CaCO of one deck densification
3Anti-aquation rete.
The preparation method of refractory materials of the present invention is: with granular MgO-CaO series refractory material is raw material, places 300-800 ℃ temperature to handle, and charges into CO
2With the mixed gas of water vapor, the temperature of water vapor is 40-90 ℃, handles 0.5-3 hour.
It is that raw material is at CO that characteristics of the present invention are with the MgO-CaO series refractory material
2With in the mixed gas of water vapor through certain temperature and the processing of time, make this raw material existing free CaO elder generation in surface and H
2Chemical reaction takes place in O:
The Ca (OH) that generates
2Again with CO
2React:
Thereby look unfamiliar into the CaCO of one deck densification at stock chart
3Anti-aquation rete.Because surface compact CaCO
3Formation can effectively completely cut off CaCO
3The inner CaO of layer contacts with extraneous moisture, and therefore having improved MgO-CaO significantly is the hydration resistance of refractory raw material.The advantage of this treatment process is just surperficial CaO has been carried out handling and well kept the active CaO of calcium magnesia sand inside, thereby the performance of the clean molten steel that the MgO-CaO series refractory material is had can not cause damage; Simultaneously, surperficial formed CaCO in the process that this material uses
3Can be decomposed into CaO and CO again
2, therefore can not cause any pollution, and the CaO that decomposites again will have higher activity to molten steel, more help the impurity in the purify hot metal; In addition, this method has changed CaCO owing to introduced water vapor
3The formation mechanism of layer makes its generating rate than adopting CaO directly and CO
2Reaction generates CaCO
3Speed faster, therefore shortened the treatment time greatly, reduced production cost.MgO-CaO series refractory material of the present invention can be used to make various unsetting refractory products, has good hydration resistance.
Fig. 1 analyzes through electron scanning micrograph and this zone composition profiles of the MgO-CaO series refractory material surface tomography that the inventive method was handled, can find out from the distribution of C element, edge C element at the particle tomography is dense distribution, shows that really there is the CaCO of one deck densification in particle surface
3
Fig. 2 is scanned photograph and the composition analysis without the MgO-CaO series refractory material surface electronic probe of the inventive method processing.
Fig. 3 is the scanned photograph and the composition analysis of the MgO-CaO series refractory material surface electronic probe handled through the inventive method.
As can be seen, the carbon content of the sample after the processing increases substantially from composition analysis, and untreated samples does not then almost have to find to have the existence of C element, and there is CaCO in also provable thus MgO-CaO series refractory material surface of handling through the inventive method
3
Below further describe embodiments of the invention.
The MgO-CaO series refractory material that the present invention adopts is the sintering calcium magnesia sand that contains 10-59%CaO, and its component concentration is by weight:
MgO 40-89％ CaO 10-59％ Fe
2O
3 ＜0.6％
Al
2O
3 ＜0.4％ SiO
2 ＜0.1％。
The granularity of sintering calcium magnesia sand is 1-12mm, is good with 2-5mm, and its surface is formed with CaCO
3Anti-aquation rete, CaCO
3The thickness of anti-aquation rete is 2-20um.Thickness is too small, is subjected to the effect of external force such as machinery easily and suffers damage the hydration resistance of the goods of reduction; Thickness is excessive, causes on the one hand the increase of cost, on the other hand CaCO in use
3Decomposition makes residual more pore in the goods, has reduced the high temperature working strength of goods.Therefore, the present invention is through implementing surface C aCO
3Layer thickness is good at 4-10um, and crossing thin and blocked up hydration resistance and high temperature use properties to calcium magnesia sand all has disadvantageous effect.
Preparation process of the present invention mainly is subject to processing the influence of temperature, steam temperature and this Several Factors of treatment time.Handling required temperature range should be good at 600-700 ℃ especially between 300-800 ℃, and this is because the speed of carrying out in reaction below 300 ℃ is slower, and more than 800 ℃ because near CaCO
3Decomposition temperature and cause the formed CaCO of part
3Decompose, therefore under this temperature, will expect thicker CaCO
3Layer is difficulty comparatively.Because the dividing potential drop of water vapor and the temperature of water vapor have metastable one-to-one relationship, so CO in the mixed gas
2Can mainly control by the temperature of regulating water vapor with the component proportions of water vapor, the ratio of water vapor in mixed gas is 4-50% usually.The temperature of water vapor generally in the time of 40-90 ℃ result more excellent, best results between 70 ℃-80 ℃ especially.This is because of CO under this temperature
2The Ca (OH) comparatively suitable with the ratio of water vapor, that CaO and steam reaction are generated
2Just and CO
2Fully react completely, thereby obtain certain thickness CaCO
3Film.Steam temperature is low excessively, and the ratio that it is occupied in mixed gas is little, thus cause the calcium magnesia sand surface CaO can not with H
2O fully reacts, therefore formed CaCO
3Layer is thinner.Steam temperature is too high, the H that contains in the mixed gas
2O is too much, thus the Ca (OH) that causes reaction earlier to generate
2Can not with CO
2Fully reaction, thus the generation skin is fine and close CaCO
3And internal layer is loose Ca (OH)
2Bilayer structure, and make CaCO easily
3In use produce and come off.The treatment time of this method be it is generally acknowledged about 1 hour, enough makes the calcium magnesia sand surface form the CaCO of desired thickness
3Layer, though with the prolongation of handling the time, the anti-aquation effect of raw material is still improving, amplitude is very little.Because certain thickness CaCO
3After the formation, extraneous moisture and CO
2Want and CaCO
3CaO in the layer continues reaction again, then needs by diffusing into and by established CaCO
3Layer.Obviously this process is very slowly, therefore generally speaking, handles and can reach the purpose that increases substantially the anti-hydratability of raw material in 1 hour.
The quality contrast of the hydration resistance of embodiments of the invention and comparative example, adopt following anti-aquation detection method: with granular MgO-CaO series refractory material, in the steam autoclave of 0.15Mpa, force aquation 2 hours, weigh up its aquation weightening finish then, by formula:
In the formula: the W1-sample is done smoked;
W2-experiment back sample and beaker gross weight;
The W0-beaker is heavy;
Calculate rate of body weight gain.
Shown in following each table of a plurality of embodiment of the present invention and hydration resistance thereof:
Granularity shown in the table 1 is that the calcium magnesia sand of 2-3mm is distinguished the light-water carbonizing treatment after 1 hour, the rate of body weight gain of gained after anti-aquation detects when steam temperature is 70 ℃ under 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃ different treatment temperature.Comparative example 1 is the result after the anti-aquation of untreated calcium magnesia sand detects.
Table 1
| Treatment temp | Aquation increment rate (weight %) | |
| Comparative example 1 | - | 1.650 |
| Comparative example 1 | 300 | 1.077 |
| 400 | 1.383 | |
| 500 | 1.074 | |
| 600 | 0.330 | |
| 700 | 0.287 | |
| 800 | 1.580 |
Embodiment 2
Granularity shown in the table 2 is that the calcium magnesia sand of 2-3mm is under 700 ℃ the treatment temp at steam temperature, steam temperature was respectively under 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ the condition respectively the light-water carbonizing treatment after 1 hour, the rate of body weight gain of gained after anti-aquation detects.
Table 2
| Steam temperature | Aquation increment rate (weight %) |
| 40 | 0.428 |
| 50 | 0.401 |
| 60 | 0.456 |
| 70 | 0.221 |
| 80 | 0.261 |
| 90 | 0.375 |
Embodiment 3
Granularity shown in the table 3 is that the calcium magnesia sand of 2-3mm is under 700 ℃ the treatment temp at steam temperature, steam temperature is under 70 ℃ the condition, distinguish the light-water carbonizing treatment after 0.5 hour, 1 hour, 2 hours, 3 hours, the rate of body weight gain of gained after anti-aquation detects.
Table 3
| Treatment time | Aquation increment rate (weight %) |
| 0.5 | 0.351 |
| 1 | 0.221 |
| 2 | 0.215 |
| 3 | 0.209 |
Claims (8)
1, a kind of hydration-resisting refractory MgO-CaO material series is a raw material with particulate state MgO-CaO series refractory material, it is characterized in that coating on MgO-CaO series refractory material surface the CaCO of one deck densification
3Anti-aquation rete, described MgO-CaO series refractory material are the sintering calcium magnesia sand that contains 10-59%CaO.
2, by the described hydration-resisting refractory MgO-CaO material series of claim 1, it is characterized in that the sintering calcium magnesia sand of the described 10-59%CaO of containing, its component concentration is by weight:
MgO 40-89％ CaO 10-59％ Fe
2O
3＜0.6％
Al
2O
3＜0.4％ SiO
2＜0.1％。
3, by the described hydration-resisting refractory MgO-CaO material series of claim 1, it is characterized in that described CaCO
3The thickness of anti-aquation rete is 2-20um.
4, by the described hydration-resisting refractory MgO-CaO material series of claim 1, the granularity that it is characterized in that described sintering calcium magnesia sand is 1-12mm.
5, a kind of preparation method by the described hydration-resisting refractory MgO-CaO material series of claim 1 is characterized in that placing 300-800 ℃ temperature to handle described raw material, charges into CO
2With the mixed gas of water vapor, the temperature of water vapor is 40-90 ℃, handles 0.5-3 hour, and the ratio of water vapor in mixed gas is 4-50%.
6, by the preparation method of the described a kind of hydration-resisting refractory MgO-CaO material series of claim 5, it is characterized in that handling temperature required at 600-700 ℃.
7, by the preparation method of claim 5 or 6 described a kind of hydration-resisting refractory MgO-CaO material series, it is characterized in that steam temperature is 70-80 ℃ in the mixed gas.
8, by the preparation method of claim 5 or 6 described a kind of hydration-resisting refractory MgO-CaO material series, it is characterized in that the treatment time is 1 hour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01128336XA CN1176875C (en) | 2001-08-13 | 2001-08-13 | Hydration-resisting refractory MgO-CaO material series and its prepn |
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|---|---|---|---|
| CNB01128336XA CN1176875C (en) | 2001-08-13 | 2001-08-13 | Hydration-resisting refractory MgO-CaO material series and its prepn |
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|---|---|
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| CN1176875C true CN1176875C (en) | 2004-11-24 |
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Families Citing this family (16)
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| JP4261841B2 (en) * | 2002-08-20 | 2009-04-30 | 黒崎播磨株式会社 | Casting nozzle |
| JP4272856B2 (en) * | 2002-08-20 | 2009-06-03 | 黒崎播磨株式会社 | Manufacturing method of immersion nozzle for continuous casting with difficulty alumina adhesion |
| CN100348536C (en) * | 2002-08-30 | 2007-11-14 | 武汉科技大学 | Antihydration MgO-CaO clinker and its preparation method |
| TW200925135A (en) * | 2007-08-17 | 2009-06-16 | Specialty Minerals Michigan | Calcium enriched refractory material by the addition of calcium carbonate |
| CN101602602B (en) * | 2009-07-06 | 2011-12-28 | 西安建筑科技大学 | Hydration-resistant MgO-CaO series fireproofing material and preparation method thereof |
| CN101921123B (en) * | 2010-08-17 | 2011-10-26 | 浙江金磊高温材料股份有限公司 | Production process of high-purity calcium magnesite |
| CN104177100B (en) * | 2014-08-18 | 2015-11-11 | 武汉科技大学 | A kind of Clean Steel is smelted with calcium oxide material and preparation method thereof |
| CN105777186B (en) * | 2016-03-24 | 2018-05-18 | 西安建筑科技大学 | A kind of MgO-CaO systems light weight refractory material and preparation method thereof |
| CN107285781A (en) * | 2017-06-30 | 2017-10-24 | 长兴泓矿炉料有限公司 | A kind of hydration-resisting magnesite-dolomite refractories and preparation method thereof |
| CN107235739A (en) * | 2017-06-30 | 2017-10-10 | 长兴泓矿炉料有限公司 | A kind of high CaO content low-loss magnesia-calica refractory castable and preparation method thereof |
| CN107352975A (en) * | 2017-06-30 | 2017-11-17 | 长兴泓矿炉料有限公司 | A kind of heat-insulated magnesite-dolomite refractories of light weight and preparation method thereof |
| CN107686340A (en) * | 2017-08-29 | 2018-02-13 | 浙江攀盛冶金材料有限公司 | A kind of calcareous dry materials of magnesium and preparation method thereof |
| ES2928477T3 (en) * | 2019-08-05 | 2022-11-18 | Refractory Intellectual Property Gmbh & Co Kg | Procedure for the treatment of magnesia-carbon products |
| CN110668833A (en) * | 2019-10-28 | 2020-01-10 | 刘晓慧 | Preparation method of magnesium-calcium-carbon composite material |
| CN111217613A (en) * | 2020-02-17 | 2020-06-02 | 武汉科技大学 | Magnesium-calcium material and preparation method thereof |
| CN112830799B (en) * | 2021-01-21 | 2022-08-09 | 西安建筑科技大学 | CaCO (calcium carbonate) 3 Coated corundum aggregate and preparation method and application thereof |
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2001
- 2001-08-13 CN CNB01128336XA patent/CN1176875C/en not_active Expired - Lifetime
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